Sheet preparation method and device

Abstract

The present invention discloses a method of making a sheet, comprising: a) providing a liquid feedstock comprising at least one solid material dissolved or dispersed in a liquid; b) applying the liquid raw material to a first movable surface to form a layer of liquid raw material film thereon; c) cyclically i) evaporating at least a portion of the liquid from the film to increase the concentration of the solid particles; and ii) passing the film through at least one nip formed by pressing opposite surfaces against each other, thereby applying pressure to the film to gradually form a layer of relatively dry flakes consisting of agglomerated and / or compacted solid particles. The invention also discloses the sheet prepared by the method, production equipment of the sheet, and application and advantages of the sheet.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority under the Paris Convention based on UK patent application numbers GB 2302788.1 (filing date: February 27, 2023) and GB 2316241.5 (filing date: October 24, 2023), the entire contents of which are incorporated herein by reference as if fully disclosed in this application. Technical Field

[0003] The present disclosure relates to a method for preparing a sheet from a liquid, and an apparatus for carrying out the method. Background Art

[0004] Modifying a material's morphology has long been known to influence its properties or behavior in numerous ways. By altering a material's size and shape, as well as, but not limited to, its specific surface area (SSA), one of the properties that can be influenced is its solubility in a particular liquid. Increasing a material's surface area and its dissolution rate has numerous applications in agriculture, cosmetics, manufacturing, water treatment, fire protection, pharmaceuticals, and food, to name a few.

[0005] Since the above fields ultimately involve products being ingested by organisms, their advantages are more intuitive, and the present invention will be explained using the ingredients of such products as an example.

[0006] Taste perception is a complex process that involves smell, taste, and chemical sensations (e.g., pungency, astringency, irritation, etc.). In terms of taste, it is perceived through specialized taste receptors in taste buds on the tongue, on the sides of the mouth, on the soft palate, in the cheeks, at the back of the throat, and even in the esophagus. The five main tastes that can be perceived are sweet, sour, salty, bitter, and umami, which can be perceived when consuming sugar, vinegar, salt, caffeine, and monosodium glutamate, respectively. Compounds or mixtures that can induce or trigger one or more taste categories or other taste perceptions are called tastants. Tastants can be added to foods to enhance the overall taste. Taste stimulants need to be dissolved in a solution to be perceived as flavor, which is one of the reasons why animals secrete saliva. Once the taste stimulant molecules dissolve in the saliva, they can properly contact the taste receptor nerves in the taste buds, stimulating them to transmit the corresponding taste perception to the brain.

[0007] While the importance of taste extends beyond human consumption and can also influence compliance with medications in other animals, the current discussion of this issue may be more relevant in the context of human food. For example, table salt (sodium chloride, often referred to as salt) and sugars (such as glucose, fructose, sucrose, and lactose) are common ingredients in our daily diets. Their relatively high levels are even labeled as health risks on packaging due to the potential health risks associated with long-term consumption. Excessive salt in the diet, through its sodium content, can lead to conditions such as high blood pressure, heart disease, and stroke. Excessive sugar intake can lead to weight gain, eye, kidney, or nerve damage, and diabetes, particularly if the body's insulin production is insufficient to clear the excess sugar. On the other hand, insufficient intake of either substance can also have adverse consequences: insufficient salt can cause fatigue, nausea, or muscle cramps; insufficient sugar (e.g., hypoglycemia) can cause headaches, dizziness, or confusion. Chronic low or high levels of salt or sugar, if left untreated, can lead to worsening medical consequences or even death. For some people, access to foods that are low in certain taste substances is a medical necessity.

[0008] In recent years, the food industry has taken steps to reduce the salt and sugar content of its products, sometimes compensating for this reduction by adding substances that enhance their taste. Other approaches include replacing these key flavorings with substances that provide similar flavors but are considered less harmful to health; or forming them into hollow structures (such as spheres, cubes, or pyramids) or coating them with thin layers on edible cores. These methods increase surface area and enhance flavor perception. Simply grinding flavorings into smaller particles to increase surface area, improve adhesion to dry foods to some extent, and enhance flavor perception has been ruled out as a viable option. This approach can introduce new flowability issues. Small particles are more likely to stick together to form lumps. Blockage and clumping can cause difficulties in handling, transportation, and storage, or lead to undesirable dusting issues. Small particles can become airborne during processing. Small particles may also be more easily encapsulated by oil, slowing dissolution and reducing the intensity of the flavor they provide.

[0009] Consumer welfare, consumer acceptance of materials in favorable morphologies, and the potential for these morphologies to enhance material performance during the manufacture of products containing them, or to improve the performance of these products after use, are not the only improvements sought. Moderately improved materials can further reduce their relative content in target products, thereby reducing costs.

[0010] There remains a need to modify the morphology of materials to improve at least one of their properties in order to meet the requirements of their future intended use. In the context of edible products (e.g., foods or pharmaceuticals), such morphological modifications can be manifested in maintaining desirable sensory properties associated with flavoring substances or achieving the desired solubility of active ingredients while advantageously reducing their content in the corresponding manufactured product. Summary of the Invention

[0011] The present disclosure aims to address some of the above needs and provide a material with significant morphological advantages to overcome the limitations observed in the current field, such as reducing the content of such materials and / or improving their performance in their respective intended uses.

[0012] In a first aspect, the present disclosure provides a method of manufacturing a sheet as set forth in the following detailed description and as claimed in the appended claim 1 and claims derived therefrom.

[0013] In a second aspect, the present disclosure provides an apparatus for producing a sheet as shown in the following detailed description and as claimed in appended claim 15 and claims derived therefrom.

[0014] Further aspects of the disclosure are set forth in detail in the following clauses, which follow the description of the embodiments.

[0015] These aspects, as well as additional advantages and features of the present disclosure, will be better understood by reference to the following detailed description taken in conjunction with the accompanying drawings and non-limiting examples. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Some embodiments of the present disclosure will be further described with reference to the accompanying drawings, in which the same reference numerals or characters (or their last digits) represent corresponding or identical components. In conjunction with the accompanying drawings, those skilled in the art can understand how some embodiments of the present disclosure are put into practice. The figures are only used to illustrate the discussion and do not attempt to show the structural details of the embodiments in details beyond the basic necessary level for understanding the present disclosure. For clarity and convenience, some objects in the figures are not drawn to scale.

[0017] In the figure:

[0018] Figure 1 A flow chart for preparing a tablet (eg, a taste agent) according to an embodiment of the present disclosure is shown.

[0019] Figure 2-7 A pressure roller or a pressure roller series which can be used according to an exemplary embodiment of the method or device according to the invention is shown schematically.

[0020] Figure 8A and 8B The images were taken with a scanning electron microscope (SEM) that also has focused ion beam (FIB) capabilities. Figure 8Ashows the state of the tastant before being processed by the method or apparatus according to an embodiment of the present invention; and Figure 8B The same tastant after the treatment is shown. In this particular case, the tastant is fed into the rollers as a dry powder.

[0021] Figure 9A and 9B A similar image was taken by SEM-FIB microscopy. Figure 9A shows a sample to be tested before being processed by a method or device according to another embodiment of the present invention; and Figure 9B The same test sample after being processed by the method or apparatus is shown. In this particular case, the test sample is fed into the nip in the form of a paste of dry powder dispersed in a viscous medium.

[0022] Figure 10A and 10B A similar image was taken by SEM-FIB microscopy. Figure 10A shows a sample before being processed by a method or apparatus according to another embodiment of the present invention; and Figure 10B The same sample is shown after this treatment. In this particular case, the sample was fed into the nip as a solution.

[0023] Figure 11A and 11B A similar image was taken by SEM-FIB microscopy. Figure 11A and Figure 10A Similarly, a sample before being processed by a method or apparatus according to another further embodiment of the present invention is shown; and Figure 11B The same sample is shown after this treatment. In this particular case, the sample was fed into the nip as a dispersion soluble in a low concentration of liquid.

[0024] Figure 12A and 12B A similar image was taken by SEM-FIB microscopy. Figure 12A and Figure 10A and 11A Similarly, a sample before being processed by a method or apparatus according to another embodiment of the present invention is shown; and Figure 12B The same sample is shown after this treatment. In this particular case, the material is fed into the nip in dispersed form in a liquid in which it is insoluble.

[0025] Figure 13A and 13B A similar image was taken by SEM-FIB microscopy. Figure 13A shows a water-soluble material before being treated by a method or apparatus according to another embodiment of the present invention; and Figure 13B The same material after this treatment is shown. In this particular case, the water-soluble material (which can be the active ingredient in various products) is fed into the nip in solution.

[0026] Figure 14A and 14B A similar image was taken by SEM-FIB microscopy. Figure 14A shows a water-insoluble material before being treated by a method or apparatus according to another embodiment of the present invention; and Figure 14B The same material after this treatment is shown. In this particular case, the water-insoluble material (which can be the active ingredient in various products) is fed into the nip as a dispersion.

[0027] Figure 15A and 15B A similar image was taken by SEM-FIB microscopy. Figure 15A shows a water-insoluble material before being treated with a method or apparatus according to the teachings of the present invention; and Figure 15B The same material is shown after this treatment. In this particular case, the material is fed into the nip as a solution in a non-aqueous solvent.

[0028] Figures 16A to 16F A similar picture is taken by SEM-FIB microscopy. Figures 16A to 16E Different commercially available sodium chloride granules prepared conventionally are shown; Figure 16F A sheet of the same material prepared according to the invention is shown. DETAILED DESCRIPTION

[0029] To address some of the shortcomings of the prior art, the present invention aims to modify the morphology of materials (whether inert ingredients or active ingredients, such as taste enhancers) to obtain a sheet-like structure. The method and apparatus designed for this purpose may accordingly be referred to as a "sheeting" process and apparatus.

[0030] While the present invention is not limited to taste enhancers and is similarly applicable to other water-soluble or water-insoluble materials (e.g., detergents or any other active ingredients), these materials, when formed into sheets in the manner described herein, may yield different morphologically derived advantages. However, for the sake of simplicity, the present technology will primarily be described using these specific types of materials as examples, including but not limited to materials that can improve the taste of food products. Therefore, for the sake of simplicity, references to "taste enhancers" below should be understood to refer generally to any material that can be similarly treated in the manner described herein, and are not intended to be limiting.

[0031] Before describing at least some embodiments in detail, some general introduction is provided.

[0032] Water-soluble materials are soluble in water (e.g., forming a clear solution). Water-soluble materials are soluble in water at a concentration of at least 10 g / l (i.e., 1 wt.% or more), and in certain embodiments, the water-soluble materials used to prepare the flaked materials in the compositions of the present invention are soluble in water at 2 wt.% or more, 4 wt.% or more, 6 wt.% or more, 8 wt.% or more, or 10 wt.% or more. Water solubility is typically assessed at room temperature (20°C to 25°C), but materials suitable for the present method may also be water-soluble at elevated temperatures (e.g., temperatures at which flaking can be performed). Although solubility is typically referred to as solubility in water, similar principles apply to the solubility of the material in any other solvent of interest. Solubility (or lack thereof) can be assessed visually; compositions that are soluble at a particular concentration (and / or at a particular temperature) are typically transparent, while insoluble materials form turbid dispersions.

[0033] While many taste substances are water-soluble, this is not a requirement for the present teachings; some ingredients known to provide taste and containing water-insoluble components (e.g., cocoa, coffee) can also be flaked. For the avoidance of doubt, this method is applicable to both water-soluble and water-insoluble materials, regardless of their intended use. Furthermore, materials can be dissolved in a liquid to form a single-phase solution, or suspended in solid form in different phases (forming a suspension or dispersion) for successful flaking.

[0034] For example, even water-soluble materials can be flaked at concentrations above their solubility in the water-based liquid carrier in question, or dispersed in a liquid carrier other than pure water (even though they may not be soluble therein, i.e., their solubility is less than 1 wt.%). In such cases, the water-soluble materials will be in a suspended state rather than a dissolved state. Alternatively, even water-insoluble materials can be flaked in liquid carriers other than pure water, in which they may be soluble (i.e., their solubility is greater than 1 wt.%). In such cases, the water-insoluble materials will be dissolved rather than suspended in the liquid serving as a solvent.

[0035] The teachings of the present invention do not necessarily change the absolute water solubility of a material (e.g., converting a water-insoluble material into a water-soluble version), but may still achieve a meaningful, detectable improvement in performance by significantly increasing the dissolution rate. For example, a quasi-insoluble material (e.g., with a solubility of less than 100 ppm in water) may not become highly soluble, but its solubility may be increased to a slightly soluble level using the methods taught by the present invention. Furthermore, solubility may not be the property that is desired to be modified by changing the material's morphology.

[0036] In certain embodiments, the dissolution rate of a sheet made from a flaked material is at least 20% higher, at least 30% higher, at least 40% higher, at least 50% higher, or at least 60% higher than the dissolution rate of its unflaked counterpart. The improvement in dissolution rate between unflaked and flaked versions of the same material can, in certain embodiments, be 2-fold or more, 3-fold or more, 4-fold or more, 5-fold or more, or 6-fold or more. In certain embodiments, the improvement in dissolution rate achieved by the present method can be measured in orders of magnitude and can be 10-fold or more.

[0037] While materials are characterized by their solubility (or insolubility) in water, this is not the only relevant liquid for evaluating dissolution rate enhancement. For example, if the intended liquid for the material's reaction during manufacturing is an alcohol, the dissolution rate enhancement can be evaluated using that alcohol. Furthermore, the liquid used for dissolution evaluation can be a mixture of multiple liquids or a liquid to which any relevant additives (e.g., pH adjusters) have been added under dissolution conditions. The dissolution rate of a material can be evaluated through routine experimentation using known methods.

[0038] Dissolution rate can be assessed by the time (e.g., seconds) required to dissolve a predetermined amount of material (e.g., 100 mg) in a specific volume (e.g., 100 ml) of liquid. An increase in dissolution rate corresponds to a decrease in dissolution rate, at any relevant temperature and / or pressure, using any specific stirring conditions, and / or in any apparatus suitable for such measurements. An increase in dissolution rate corresponds to a decrease in the time required to achieve complete dissolution of the test sample under the test conditions. For example, if a flaked material dissolves at twice the rate of its unflaked precursor, the time required for complete dissolution under similar test conditions will be halved.

[0039] Due to their size and form, conventionally prepared taste substances only partially dissolve in the mouth during consumption. Consequently, the majority of the taste substance is swallowed without contributing to the perceived flavor of the product. Without being bound by any particular theory, it is believed that the form according to the teachings of the present invention facilitates the dissolution of the taste substance, thereby enhancing the perceived flavor relative to the same amount of a less soluble counterpart. In other words, for the same taste intensity and duration, a lesser amount of taste substance using the present form is required than an equivalent taste substance using a conventional form.

[0040] While flavors are traditionally available in a variety of forms, shapes, and sizes, they typically exist as small particles with particle sizes ranging from 2 to 5 mm, or even up to approximately 10 mm in the case of coarse granules or flakes. Typical particle sizes range from 1 to 2 mm. Some flavors can be prepared as fine powders with particle sizes of 0.2 to 1 mm, or even smaller for specific applications (e.g., powdered sugar). For some flavors, due to the importance of reducing dosage for research, products with particle sizes down to micrometers (μm) have been developed, often with at least one dimension greater than 20, 30, or 40 μm. Many of these remain in the anecdotal stage, as such tiny particles are often difficult to flow and cannot be applied using conventional equipment. Aside from flavors, other materials can exist as large particles on the centimeter (cm) scale or as small as the millimeter (mm) scale, with particle sizes up to 10 mm. However, for the purpose of implementing this method, it may be advantageous to use smaller particles as starting materials.

[0041] The size of the particles (e.g., before and after treatment as described herein) can be estimated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), focused ion beam (FIB), confocal laser scanning microscopy, and / or light microscopy. For example, light microscopy can be used for particles a few micrometers in size or for particles estimated to be approximately 200 nanometers in size, scanning electron microscopy can be used to assess the planar dimensions of particles less than 200 nanometers in size, and the thickness or length of particles can be determined using focused ion beam (FIB) technology. Such sizes can be estimated by image analysis of at least one instrument field of view, obtained using appropriate microscopy techniques and magnifications, and by repeating the microscopic measurements on multiple particles for statistical significance, with representative particles located in one or more fields of view. Some microscopes incorporate image analyzers that can directly provide metrological parameters related to the population of particles captured within the relevant field of view. Depending on the microscopy technique, magnification, and the size of the particles being measured, a field of view can contain at least 5 particles, at least 10 particles, or at least 20 particles; alternatively, it can contain up to 200 particles, up to 100 particles, or up to 50 particles. In some embodiments, the field of view contains a number of particles in the range of 5 to 200, 10 to 100, or 20 to 50. In some embodiments, two or more independent fields of view are considered to achieve a sufficient number of particles to reasonably represent the particle population. As used herein, the average size reflects the average of that size over at least 10 particles, at least 20 particles, at least 30 particles, at least 40 particles, or at least 50 particles. Selecting a representative particle or a group of representative particles to characterize a population with sufficient accuracy (e.g., by particle characteristic measurements such as diameter, longest dimension, thickness, aspect ratio, or their averages) is within the skill of a trained operator.

[0042] According to one aspect of the present disclosure, a material (e.g., a taste substance or any other compound having a desired activity and / or providing any manufacturing advantage) is provided, which has a thin sheet shape and may be referred to herein as a sheet or taste sheet. The (taste agent) sheet can be defined by its thickness (or the average thickness of its planar dimensions; t) and its longest dimension (L) in the plane, and further characterized by the dimensionless aspect ratio (Asp = L / t) between the two. Taking taste agents as an example, as active ingredients that contribute to the efficacy of the final product (e.g., the taste of a food product), in sharp contrast to traditional taste agents, the sheet of the present invention has at least a thickness in the low micrometer range (e.g., a thickness of less than 200 μm). The thickness of the taste active ingredient sheet can optionally be in the submicrometer range (e.g., a thickness of less than 1 μm), or the nanometer (nm) range (e.g., a thickness of less than 200 nm, 150 nm, or 100 nm). Taste particle sheets with an average thickness between 1 and 200 μm can be called (taste) microsheets, taste particle sheets with an average thickness between 0.2 and 1 μm can be called (taste) submicrosheets, and flakes (tastants) with an average thickness less than 0.2 μm can also be called (tastant) nanosheets.

[0043] In certain embodiments, the average thickness t of the flakes (e.g., tastant) is no more than 200 μm, 175 μm, 150 μm, 125 μm, 100 μm, 90 μm, 80 μm, 70 μm, 60 μm, 50 μm, 40 μm, or 30 μm. In certain embodiments, the average thickness t of the flakes is no more than 20 μm, 18 μm, 16 μm, 14 μm, 12 μm, or 10 μm. In certain embodiments, the average thickness t of the flakes is no more than 9 μm, 8 μm, 7 μm, 6 μm, 5 μm, 4 μm, 3 μm, or 2 μm. In certain embodiments, the average thickness t of the flakes is no more than 1 μm, 0.9 μm, 0.8 μm, 0.7 μm, 0.6 μm, 0.5 μm, 0.4 μm, or 0.3 μm.

[0044] In certain embodiments, the platelets (eg, taste agents) have an average thickness, t, of at least 50 nm, at least 100 nm, at least 150 nm, or at least 175 nm.

[0045] In certain embodiments, the platelets (e.g., taste agents) have an average thickness, t, of between 50 nm and 200 μm, between 50 nm and 150 μm, between 50 nm and 100 μm, between 50 nm and 50 μm, between 50 nm and 20 μm, between 100 nm and 18 μm, between 100 nm and 16 μm, between 150 nm and 14 μm, between 150 nm and 12 μm, between 200 nm and 10 μm, between 200 nm and 5 μm, between 100 nm and 4 μm, between 100 nm and 2 μm, or between 100 nm and 1 μm.

[0046] In some embodiments, the average value of the longest planar dimension L of the (e.g., probe) sheet is at most 10,000 μm, at most 7,500 μm, at most 5,000 μm, at most 4,500 μm, at most 3,000 μm, at most 2,500 μm, at most 2,000 μm, at most 1,500 μm, at most 1,000 μm, at most 500 μm, at most 400 μm, at most 300 μm, at most 200 μm, at most 100 μm, or at most 50 μm.

[0047] In certain embodiments, the longest planar dimension of the (eg, tastant) flakes L is, on average, at least 5 μm, at least 7.5 μm, at least 10 μm, at least 12.5 μm, or at least 15 μm.

[0048] In certain embodiments, the longest planar dimension of the (e.g., taste stimulant) piece L is, on average, between 5 μm and 10,000 μm, between 5 μm and 7,500 μm, between 5 μm and 5,000 μm, between 5 μm and 500 μm, 7.5 μm to 4,000 μm, 7.5 μm to 300 μm, 10 μm to 2,000 μm, 10 μm to 1,000 μm, 10 μm to 200 μm, or 10 μm to 100 μm.

[0049] The ranges of thickness and longest planar dimension are generally related, so they can also be characterized by their relationship, which can be determined by calculating the dimensionless aspect ratio between the two. In some embodiments, the average aspect ratio (Asp = L / t) between the longest planar dimension and the thickness of the sheet (e.g., test piece) is at least 5, at least 10, at least 15, at least 20, at least 25, at least 30, at least 35, at least 40, at least 45, or at least 50. In certain embodiments, the average aspect ratio Asp is at most 200, at most 150, at most 125, at most 100, or at most 75. In certain embodiments, the average aspect ratio Asp is between 5 and 200, between 5 and 150, between 10 and 100, between 10 and 50, between 50 and 150, or between 20 and 75.

[0050] As will be described in further detail below, the present method and apparatus allow for a certain degree of control over the size of the flakes obtained thereby. While typically most flakes will have the aforementioned dimensions and aspect ratios, falling within the specified ranges, in certain embodiments, it may be desirable to achieve different values ​​(e.g., a narrower size distribution) to suit a particular intended use. In such cases, the initially obtained flakes can be further sorted into subpopulations by appropriate separation steps or equipment (e.g., sieves), each subpopulation having a size that falls within or does not fall within the desired range. In such cases, the particles that do not meet the requirements can be recycled back into the process as desired (e.g., dissolved or dispersed to become part of a liquid feedstock for subsequent use). Such recycling can be accomplished in a post-processing step performed after the flakes have been collected and sorted.

[0051] Advantageously, flakes of the above-mentioned sizes are expected to have good miscibility, good adhesion (thereby achieving more uniform surface coverage) and fewer dusting problems in foods, which are superior to their conventional counterparts. The above can be considered as manufacturing advantages of flakes, a term that also covers the steps before and after the actual product manufacturing (such as storage, transportation, packaging, etc.). The sizes in which they can be prepared can also be selected as required to provide the desired texture (such as crispness) or appearance (such as the visual effect of the ingredients), or other advantages brought about by the size of the flakes and their derived properties (such as dissolution rate). Such effects are more directly related to the activity that the taste substance or its flakes were originally intended to exert, and can be considered as efficiency advantages. The practicality of taste substance flakes may in some cases include both advantages at the same time, and the two are not mutually exclusive.

[0052] Because taste tablets have a higher surface area than their standard form, they dissolve more quickly, providing a richer mouthfeel at the same taste dosage, or achieving the same mouthfeel at a lower dosage, thereby reducing the taste content in the food. Food products can have any conventional texture, such as liquid, semisolid (e.g., spreads, pastes, gels), or solid at normal temperatures during storage or use. Taste tablets can be attached to the exterior of a food product (e.g., salt on snacks, sugar on cereals, spices on crackers or croutons), dispersed within it, or both. When a taste tablet needs to remain dispersed in the food until consumed, the taste is typically made from a material with low or no solubility in the food. For example, a water-soluble taste agent (e.g., salt) can be dispersed in a tablet and incorporated into a hydrophobic liquid (e.g., oil), a semisolid emulsion (e.g., mayonnaise or oil-based sauces), or a product that is relatively solid under normal storage conditions (e.g., butter). The above considerations regarding relative product viscosity and the distribution of flakes on and / or within the product apply equally to any other article that may benefit from flakes prepared as described herein.

[0053] Having a higher specific surface area may not only accelerate the dissolution rate of a particular material in a particular liquid, but may also enhance other beneficial interactions between molecules. For example, in chemical reactions, where a material acts as a catalyst, a catalyst with a relatively high surface area is expected to accelerate the rate of the chemical reaction it normally catalyzes more rapidly than a catalyst with a smaller surface area.

[0054] Taste tablets can impart sweet, salty, sour, bitter, or umami tastes and can be made from any known or under development taste substances with such tastes, or from combinations thereof. In certain embodiments, the taste particles comprise one or more of the following substances: acetic acid, citric acid, lactic acid, malic acid, ascorbic acid, tartaric acid, succinic acid, hydrochloric acid, phosphoric acid, sulfuric acid, sucrose, arabinose, ribose, xylose, glucose, galactose, xylose, fructose, lactose, maltose, raffinose, stachyose, saccharide trihydrate, trehalose, glycerol, erythritol, arabitol, xylitol, sorbitol, mannitol, lactitol, maltitol, corn syrup, aspartame, low molecular weight maltodextrin, bitter peptides, amino acids, alkaloids, amides, thiourea, polyphenols, sodium bicarbonate, sodium glutamate, disodium 5'-inosinate, disodium 5'-guanylate, sodium chloride, sodium chloride iodide, calcium chloride, potassium chloride, potassium chloride iodide, or a mixture thereof; the above list is only an example and does not limit other materials that have the function of providing taste.

[0055] Because the present method does not rely on the presence of taste-modulating compounds to alter the taste perception provided by the taste substance, the taste substance tablet (which can be composed of a pure compound or a mixture of natural taste substances) does not have an aftertaste. This may increase acceptance by consumers who seek clean alternatives that are as close as possible to the source of their natural taste substances. This is particularly true when the taste substance tablet is made of a single material (such as salt).

[0056] However, taste substances are provided as examples only; other materials taught by the present invention may also be formulated into sheets. Such materials are typically selected based on the potential benefits they may provide to products containing or made from them. The sheet-shaped structures taught by the present invention offer improved benefits compared to traditional forms (e.g., improved efficacy (optionally allowing for a reduction in the amount of material required to achieve a specific effect), simplified manufacturing, reduced costs, etc.). Materials are generally defined as "active ingredients" when they contribute to or influence the chemical, physical, and / or biological effects of a finished product. Catalysts, reinforcing materials, and active pharmaceutical ingredients are specific examples of such benefits. However, because the improvements provided by sheet-shaped materials are not limited to the chemical, physical, and / or biological effects they may at least contribute, "inactive ingredients" also include those ingredients that "simply" simplify product manufacturing in any way. Inactive ingredients can be considered to provide manufacturing advantages, and this term encompasses all technical steps before and after manufacturing. The efficacy of active ingredients prepared according to the present invention relates at least to the generally desired effectiveness of the ingredient itself or its final product, but may optionally further include manufacturing advantages.

[0057] Applicable materials (active or inactive ingredients) can be water-soluble or water-insoluble, organic (e.g., plastics or other non-polar compounds) or inorganic (e.g., ceramics, minerals, metal-based, etc.), and exist in various chemical families, serving a wide range of industries.

[0058] Water-soluble materials used in addition to flavoring agents or for purposes other than providing taste or improving the ingestion of a product include, for example, sodium chloride (NaCl), which is commonly known as table salt as a food seasoning and is also used as a de-icing agent, a reagent in chemical manufacturing, or a catalyst. Non-exhaustive examples of water-soluble materials include: ammonium nitrate (NH4NO3), which is used in fertilizers, explosives, and nitric acid production; calcium carbonate (CaCO3), which is used as a dietary supplement for human and animal food, as an antacid in medicine and in agriculture / industry, as a filler in the production of adhesives, sealants, coatings, paper, and plastics, and in the manufacture of cement and concrete; calcium chloride (CaCl2), which is used in addition to its use in food processing as a de-icing agent and in cement and concrete production; copper sulfate (CuSO4), which is used as an algaecide, It is a bactericide, fungicide, herbicide, molluscicide, and root killer, and can also be used as a catalyst. Ferric chloride (FeCl3) can be used to treat sewage, industrial wastewater, purify water, as an etchant for etching circuit boards, and in the production of other chemicals. Magnesium sulfate (MgSO4) can be used in agriculture as a fertilizer, in medicine as a laxative, in the production of paper and textiles, and as a catalyst. Manganese sulfate (MnSO4) can be used as a fertilizer and livestock supplement in areas where the soil is deficient in manganese, and is also used in some glazes, varnishes, ceramics, and fungicides. Nicotine salts can be used in tobacco substitute products (such as e-cigarettes or vaping devices) or in medicines for nicotine withdrawal symptoms. Potassium chloride (KCl) can be used as a fertilizer and is used to make potassium hydroxide (KOH), which is used in the production of soaps and detergents. In addition to being a pH adjuster in food processing, potassium hydroxide can also be used in the manufacture of soaps and detergents, as well as in the production of biodiesel. Potassium iodide (KI) can be used as a dietary supplement, for the treatment of hyperthyroidism, in radiation emergencies, and to protect the thyroid gland when using certain radiopharmaceuticals. It can also be used as a catalyst. Potassium nitrate (KNO3), in addition to being used in food preservation, can also be used in fertilizers and in the manufacture of gunpowder; sodium bicarbonate (NaHCO3), in addition to being used in food processing, can also be used in medicine as an antacid, or combined with organic acids such as citric acid and tartaric acid to provide a foaming effect for active pharmaceutical ingredients, and in fire extinguishers; sodium hydroxide (NaOH) can be used in the manufacture of soaps and detergents, pipe cleaners, and in paper production; and zinc chloride (ZnCl2), can be used as an electrolyte in dry cell batteries, a catalyst, a condensing agent, a dehydrating agent, a deodorant, a disinfectant, or a wood preservative.

[0059] Water-insoluble materials to which this method is applicable include carbonates, phosphates, sulfides, and oxides, and the above chemical families also include exceptions whose relative solubility is known or easily determined. Taking metal-containing materials as an example, such as calcium, calcium carbonate (CaCO3), calcium phosphate (Ca3(PO4)2), calcium sulfate (CaSO4), bone meal ((Ca(PO4)2)(CaF2), rock phosphate (Ca3(PO4)2CaF2), and other similar phosphate minerals can be widely used as water-insoluble materials. Other common water-insoluble materials include barium carbonate (BaCO3), barium sulfate (BaSO4), copper carbonate (CuCO3), iron oxide (Fe2O3), lead chromate (PbCrO4), lead chloride (PbCl2), lead sulfate (PbSO4), silicon dioxide (SiO2), silver chloride (AgCl), magnesium hydroxide (Mg(OH)2), magnesium stearate (Mg(C 18 H 35 O2)2) and zinc oxide (ZnO).

[0060] As shown in the non-exhaustive list of exemplary materials above, many of them are salts and exist in various hydrate and / or crystal forms, some of which have different effects, but all of which demonstrate that the teachings of the present invention can benefit a wide range of industries and all of which are encompassed as materials (e.g., active ingredients) suitable for use in the present flaking methods.

[0061] Regardless of the type of material comprising the tablet, a tablet is considered to be made of pure material if the material comprises at least 95% by weight of the tablet. Purity is assessed by weight content and is preferably at least 96 wt.%, at least 97 wt.%, at least 98 wt.%, at least 99 wt.%, or at least 99.5 wt.%. The purity of a material (or mixture of materials) in a tablet can be determined by any analytical method suitable for measuring a particular property (e.g., elemental composition, physicochemical properties, etc.).

[0062] As previously mentioned, the present method is suitable for preparing tablets composed of two or more materials. This may be advantageous when the materials in the mixture are able to interact (either individually or synergistically) when in close proximity, and / or when the desired effect of the materials may benefit from a relatively uniform distribution of them overall. For example, taking a food product that needs to be coated with different tablets, each tablet providing a different flavor (e.g., salt and pepper), if the tablets are not distributed evenly across the surface of the food product, the consumer may perceive different flavors in different areas of the product (e.g., different bite points). While this is not necessarily the case for all products, in some cases, using a tablet made of two or more materials can allow the tablet to produce a uniform effect (e.g., similar taste characteristics, aroma, color, etc.) in every part of the product (e.g., food) to which it is applied or incorporated.

[0063] By way of non-limiting example, if one of the materials is a taste substance (e.g., a salt such as sodium chloride or a sugar such as sucrose), the other materials that can be mixed with it in the tablet prepared according to the present invention can be selected from the group consisting of flavoring agents, seasonings, essences, spices (e.g., basil, cardamom, chili, cinnamon, coriander, cumin, garlic, ginger, nutmeg, oregano, paprika, pepper, rosemary, sage, thyme, turmeric, etc.), extracts, colorants, masking agents, enhancers, nutrients, minerals, vitamins, emulsifiers, stabilizers, anti-caking agents, dietary supplements, antioxidants, and combinations thereof. One material can serve as a carrier for another material.

[0064] In certain embodiments, (eg, taste ingredients) the tablet has at least 0.001 m 2 / g, at least 0.005m 2 / g, at least 0.01m 2 / g, at least 0.05m 2 / g, at least 0.1m 2 / g, at least 0.2m 2 / g, at least 0.3m 2 / g, at least 0.4m 2 / g, or at least 0.5m 2 / g. Usually, the specific surface area of ​​the taste agent particles does not exceed 10m 2 / g, and its specific surface area is usually up to 8m 2 / g, up to 6m 2 / g, up to 4m 2 / g, or up to 2m 2 / g.

[0065] Therefore, in some cases, the specific surface area of ​​the sheet of the present invention is 0.001m 2 / g to 10m 2 / g, within 0.01m 2 / g to 8m 2 / g, within 0.1m 2 / g to 6m 2 / g, within 0.2m 2 / g to 4m 2 / g, or between 0.5m 2 / g to 2m 2 / g.

[0066] For reference, a material with the same density but approximately spherical particles and an average diameter of 50 μm (e.g., the substance to be tested) may have a specific surface area of ​​no more than about 0.2 m 2The surface area of ​​a material can be conventionally determined by any suitable method, for example by nitrogen adsorption and analysis using the Brunner-Emmett-Teller (BET) or Langmuir procedure, using any suitable instrument, and calculating the specific surface area based on the mass of the sample measured.

[0067] The (e.g., taste agent) tablet may additionally or alternatively have the following characteristics: its bulk density (ρ B ), also known as apparent density, is the mass of an uncompacted (thus including the volume of interparticle voids) powder sample divided by its volume (V B ) ratio, and the bulk density is relatively low relative to its standard counterpart. In other words, for the same volume of taste substance particles (for example, one teaspoon), when the taste substance is in the form of a flake as described in the present invention, its weight will be relatively reduced. If the taste properties of the taste substance are not impaired by the reduction in bulk density, the weight content of the taste substance in the food can be reduced accordingly. However, if the taste is impaired due to the flake formation of the taste particles, the weight reduction of the taste particles added to the food will no longer be proportional to the reduction in bulk density, because additional taste particles may need to be added to compensate for the decrease in taste caused by the initial "weight loss".

[0068] In certain embodiments, the bulk density of the flavoring (e.g., flavoring) tablet is at least 20%, 30%, 40%, or 50% lower than the bulk density of its standard counterpart. For example, the bulk density of standard granular salt is approximately 1.25 g / cm 3 At this time, the volume density of the taste substance sheet should not exceed 1.00g / cm 3 (i.e. 1.25g / cm 3 80% of the total weight), not exceeding 0.88 g / cm 3 , up to 0.75g / cm 3 , or a maximum of 0.62 g / cm 3 The volume density of the taste particles can be even lower, for example not more than 0.50 g / cm 3 , not exceeding 0.40g / cm 3 , or not more than 0.30g / cm 3 , but usually does not need to be less than 1% or even 5% of the volume density of the original taste particles. Therefore, in some embodiments, the volume density of the taste agent particles is 0.01 g / cm 3 Up to 1.00g / cm 3 Between 0.01g / cm 3 to 0.80g / cm 3 Between 0.05g / cm 3 , 0.05g / cm 3 to 0.50g / cm 3 , 0.10g / cm3 to 0.75g / cm 3 , 0.10g / cm 3 to 0.70g / cm 3 , 0.05g / cm 3 to 0.65g / cm 3 , or 0.20g / cm 3 to 0.62g / cm 3 The apparent bulk density of a particulate material can be determined by routine experimentation using standard methods, such as those described in ASTM B527.

[0069] When a flake (e.g., a test substance) is mixed with other dry powders (e.g., other flakes) for its intended use, it may be advantageous for all mixed powders to have relatively similar bulk densities to minimize powder segregation and maintain mixing uniformity. The bulk densities of a mixture are considered relatively similar if the bulk density of a single component does not deviate from the overall bulk density of the mixture by more than 20%.

[0070] (e.g., MSG) tablets can also, or alternatively, be characterized by their tap density (ρ T ) is relatively low compared to its standard counterpart. Unlike bulk density, the tap density measurement involves vibrating the sample to reduce the interparticle spaces and assess the packing ability of the powder. For a given mass of powder, bulk density is measured by measuring the volume V occupied by the powder mass. B The tap density is calculated by measuring the volume V after tapping. T The volume is usually reduced by the rearrangement of the powder during the tapping process. Generally, unless the powder is completely free-flowing, its tap density is higher than the bulk density, but the difference between the two depends on the intrinsic properties of the particles (e.g., particle size, shape, porosity, etc.), the particle size distribution (e.g., uniformity, separability, etc.), and the interactions between the particles, which may also be caused by their environment (e.g., humidity, temperature, etc.).

[0071] In certain embodiments, the tapped density of the tablet (e.g., a flavoring agent) is at least 20%, at least 30%, at least 40%, or at least 50% lower than the tapped density of a standard counterpart, but generally need not be less than 5% of the original tapped density of the conventional material. For example, the bulk density of a standard granular salt is about 1.45 g / cm 3 At this time, the volume density of the taste agent tablet can be reduced to a maximum of 1.16g / cm 3 (i.e. 1.45g / cm 3 80% of the total), up to 1.02 g / cm 3 , up to 0.87g / cm 3 , or a maximum of 0.73g / cm3 If further reduction is required, the tap density of the taste test tablet can be as low as a maximum of 0.50 g / cm 3 , maximum 0.40g / cm 3 , or a maximum of 0.30g / cm 3 , but generally should not be less than 5% of the original tap density of a conventional taste tester. Therefore, in certain embodiments, the bulk density of the taste agent tablet is 0.07 g / cm 3 to 1.02g / cm 3 Between 0.07g / cm 3 to 0.87g / cm 3 Between 0.10g / cm 3 to 0.73g / cm 3 Between 0.07g / cm 3 and 0.50g / cm 3 Between, or 0.20g / cm 3 and 0.73g / cm 3 between.

[0072] The relatively low bulk density and / or tapping density exhibited by the flavoring tablets of the present invention is believed to be advantageous, particularly when the flavoring is to be applied to the surface of dry snack foods, such as potato chips or nuts. For such foods, conventional flavorings often have poor adhesion and / or a high tendency to fall off during processing, resulting in significant flavoring loss, especially when the food is consumed. This phenomenon results in unnecessary waste of flavoring.

[0073] While forming a flavoring into a flake form may inherently increase the likelihood of food contact, thereby promoting adhesion, compared to granular flavorings, this is only a basic requirement. Flavoring flakes should also remain attached to the product surface during subsequent processing steps and subsequent food handling, such as packaging, transportation, and storage. Studies have shown that flavorings with lower relative densities are less likely to fall off the food surface than those with higher relative densities. This can be attributed in part to the fact that particles with lower bulk density and correspondingly smaller mass are less affected by gravity, while particles with higher bulk density / larger mass are more affected by gravity, so such flavoring flakes are better able to maintain their adhesion to the food until ingested.

[0074] In some cases, the size of the particles and their relatively high aspect ratio compared to conventional products result in the particles having high compressibility, which can aid in packaging, storage, or transportation. The compressibility of the particles can be determined by calculating the dimensionless ratio between the density of the particles before and after compression. This ratio can also be used to assess the correlation between the aspect ratio of the flaky particles and their compressibility. Such factors (e.g., F5 and F6) and their measurement methods can be determined as described in Example 10 below in this specification, which also provides numerical ranges that can be used alone or in combination with other characteristics to characterize the flaky particles of the present invention.

[0075] In certain embodiments, the flakes (e.g., test samples) may be made of a water-soluble or water-insoluble material having a crystalline structure. In this case, for certain materials, the flakes may additionally or alternatively be characterized by a specific crystalline structure detectable by X-ray diffraction (XRD), wherein the XRD detectable structure is selected from the group consisting of: the position of a diffraction peak, the relative intensity of a diffraction peak at a specific position, the intensity ratio of any two diffraction peaks at two specific positions, the diffraction peak width, the grain size, the microstrain value within a specific diffraction peak or within a scanned spectrum, and the dislocation density, as well as other similar parameters indicative of crystalline structure.

[0076] In certain embodiments, at least one of the above-mentioned crystal parameters measured on the (e.g., sample) sheet by XRD or other suitable method differs by at least 20% compared to the same parameter measured in a reference (e.g., unsheeted or otherwise prepared) crystalline material. In some cases, the parameter value measured in the sheet may deviate by being at least 20% lower or 20% higher than the same parameter measured in a standard grown / prepared crystal. In certain embodiments, at least one crystallographic parameter measurable on the sheet differs by at least 30%, 40%, or 50% from the corresponding parameter in a reference standard unsheeted crystal. For certain crystallographic parameters, the difference between the value measured in the sheet and the value measured in the relevant reference crystal may even be at least 2 times, at least 3 times, or at least 4 times.

[0077] For example, the grain size and microstrain values, which may indicate the relatively higher compression experienced by the precipitate during crystal growth and when it passes through the rollers, are present in the specimens made from the salt, compared to the standard salt.

[0078] An XRD structure detectable in a raw, unflaked material (e.g., a taste sample) before being processed according to the present method or using an apparatus according to the present teachings may be referred to as an XRD-detectable first structure, while a corresponding structure detectable after the (e.g., taste sample) flake preparation may be referred to as an XRD-detectable second structure. Structures in the raw (e.g., unflaked) material and the flake version of the same material are considered corresponding if they relate to similar parameters when analyzed at similar locations or along similar spectral ranges, as it is clear that the crystal structure of a crystalline material may vary in certain embodiments, which may itself result in slight shifts in diffraction peaks. Thus, corresponding structures need not be identical, but the claimed parameters should essentially be of the same class.

[0079] In the above description, the (e.g., test sample) sheet is characterized by a single parameter, such as: i) thickness, ii) length, iii) its aspect ratio, iv) its specific surface area, v) its bulk density, its tapped density, or any ratio of these two densities, or vi) any crystallographic specification applicable to crystalline materials. If the material is crystalline, it will be readily understood by those skilled in the art that the sheet prepared by the present method can be characterized by any combination of two or more of the above parameters. For example, a taste sheet may have both bulk density and crystallographic behavior as described above. In certain embodiments, the taste sheet having the above-described characteristic parameters is further made of pure taste substance (e.g., accounting for more than 95% of the mass of the sheet).

[0080] For example, taste particles according to the teachings of the present invention can be: a) made of pure salt, such as containing more than 95% by weight of sodium chloride; b) have a relatively low bulk density, not exceeding 0.60 g / cm 3 , optionally not exceeding 0.55 g / cm 3 , not exceeding 0.50g / cm 3 , not exceeding 0.45g / cm 3 , not exceeding 0.40g / cm 3 , not exceeding 0.35g / cm 3 , not exceeding 0.30g / cm 3 , not exceeding 0.25g / cm 3 , not exceeding 0.20g / cm 3 , not exceeding 0.15g / cm 3 , or a maximum of 0.10g / cm 3 ; and c) having a structure detectable by XRD and satisfying at least one of the following conditions: i) a microstrain value of at least 0.050%, at least 0.075%, at least 0.100%, at least 0.125%, at least 0.150%, or at least 0.175%; and ii) a grain size not exceeding 1,000 angstroms Not more than 750 angstroms, not more than 625 angstroms, or not more than 500 angstroms.

[0081] When the term "salt" is used in this specification to refer to sodium chloride, the raw materials used to prepare salt wafers can include all available sources of salt, whether naturally occurring (e.g., sea salt, ocean salt, mineral salt, etc.) or further processed (e.g., smoked salt, flavored salt, added salt such as iodized salt, etc.) and the wafers produced therefrom can have similar names.

[0082] The flakes of the present invention can be characterized by additional features that can be used to calculate the relationship between two or more structural features. The aspect ratio of a flake is just one example of how the proportional relationship between two measurable features (longest planar dimension to thickness) can provide complementary, valuable, and unique information. Alternative or additional calculated ratios are exemplified by factors F1 through F6 described in Examples 7, 9, and 10.

[0083] For the sake of brevity, the following paragraphs only list the mathematical expressions of the aforementioned exemplary factors. F1 is the ratio of the aspect ratio ASP of the sheet to its dissolution rate (DT), which can be mathematically expressed as F1 = ASP / DT (units are seconds - 1 ). F2 is the bulk density ρ of the flake T and volume density ρ B The dimensionless ratio between them can be expressed by the mathematical expression F2 = ρ T / ρ B F3 is the volume ratio of the sheet ASP and the volume density ρ B The ratio between them can be expressed by the mathematical expression F3 = ASP / ρB (unit is cubic centimeters per gram). F4 is the aspect ratio ASP of the sheet and its volume density ρ T The ratio between them can be expressed by the mathematical expression F4=ASP / ρ T Indicates (unit: cubic centimeters per gram). F5 is the density of the sheet after compression ρ C and the bulk density ρ before compression B The ratio between them can be expressed by the mathematical expression F5 = ρC / ρB. F6 is the ratio of the aspect ratio ASP of the sheet to its compressibility (estimated by F5), which can be expressed by the mathematical expression F6 = ASP / F5. As for the measurable characteristics, the factors in this study can be combined with each other or with the measured characteristics (for example: i) thickness t, ii) longest plane dimension L, iii) specific surface area SSA, iv) dissolution rate DT, v) bulk density ρ B ,vi) Tap density ρ T , vii) compression density ρ C , viii) any crystallographic specifications, etc. ) to characterize and differentiate the present flakes.

[0084] For example, the current sheet may have at least two, at least three, at least four or at least five of the following characteristics. For the sake of brevity, this paragraph only illustrates one of the multiple restrictions that each characteristic may meet: 1) the average thickness t does not exceed 200 μm; 2) the aspect ratio ASP is at least 10; 3) the F1 factor is not less than 5; 4) the F2 factor is not less than 1.25; 5) the F3 factor is not less than 25; 6) the F4 factor is not less than 20; 7) the F5 factor is not less than 1.6; and 8) the F6 factor is not less than 6.

[0085] In certain embodiments, two or more features characterizing the sheeting of the present invention include any combination of 1) and 2), 2) and 3), 2) and 4), 2) and 5), 2) and 6), 2) and 7), and 2) and 8), as well as the respective limitations described herein. In certain embodiments, three or more features include the above-listed items 1), 2) and 3); 2), 3) and 4); 3), 4) and 5); 3), 5) and 7); 3), 5) and 8), as well as any respective limitations described herein. In certain embodiments, four or more features include the above-listed items 1), 2), 3) and 4); 2), 3), 4) and 5); 3), 4), 5) and 7); 2), 3), 5) and 7); 2), 3), 5) and 8), to name a few, as well as the respective limitations described herein.

[0086] According to another aspect of the present invention, there is provided a method of making a tablet (e.g., a taste tablet), the method comprising:

[0087] a) providing a liquid raw material, wherein the liquid raw material comprises at least one solid material dissolved or dispersed in the liquid;

[0088] b) applying a liquid feedstock to the first movable surface to form a film thereon;

[0089] c) cyclically

[0090] i) removing at least a portion of the liquid from the film to increase the concentration of solid particles in the film, and

[0091] ii) applying pressure to the film by passing the film through at least one nip formed by relatively tight rollers to gradually form a sheet-like layer comprising compacted and / or agglomerated solid particles,

[0092] The cycle is repeated until the liquid content in the tablets is less than 5 wt.%.

[0093] The sheet prepared by the method may have an average thickness t not exceeding 200 μm and not exceeding the thickness of the layer. In further embodiments, the average aspect ratio ASP between the longest planar dimension L and the thickness t of the sheet (e.g., test sample) is at least 10.

[0094] The numerical values ​​mentioned in the above method introduction are only examples and can be replaced by other parameters related to the monitored characteristics in accordance with the present invention to determine the termination conditions of the flaking method.

[0095] In the present invention, the layer that ultimately forms the sheet need not be a continuous layer, but may refer to discrete aggregates of dispersed particles that are aggregated and held together by any suitable force. Without wishing to be bound by any particular theory, it is believed that in the present method, as the liquid is removed, the particles of solid material may aggregate by pressure agglomeration, partial sintering or melting, and / or by stacking crystallization as they gradually separate from the liquid, depending on the material in question.

[0096] Since agglomeration does not require a specific pattern of particles coming together to form a solid mass, such an assembly can assume any shape and size, if it were to form naturally. Since the solid particles in the present method agglomerate during the periodic compaction, at least the thickness of the layer (e.g. when the liquid content is below 5 wt.%) can be predetermined (e.g. empirically), for example based on the size of the solid particles that may be present in the liquid material, their hardness and the thickness of the layer in the gap between the compacting rollers (e.g. Since the sheets can be considered as part of the layer that originally constituted them, they can be separated from adjacent sheets and / or the underlying surface step by step or at the end, and thus can also be considered as agglomerates of solid particles. Since the present process also involves compaction, the particles that constitute the sheets (or the layers that can be separated therefrom) can be considered as aggregated and compacted, or vice versa, compacted and aggregated, and it is very likely that these two effects occur simultaneously, and their order in any particular sentence does not imply a specific order of the particles in time.

[0097] As is readily understood, a sheet of aggregated and compacted particles does not necessarily consist of just one particle; the number of particle layers depends on the material and operating conditions. For example, in the case of crystals of a solid material, which can be gradually separated from a liquid mother solution, an aggregated crystal layer can consist of multiple crystals adjacent to each other in three-dimensional space.

[0098] It should be noted that when the two cylinders are pressed into contact (e.g., by pneumatic or hydraulic pistons, the latter optionally equipped with an accumulator, which may be spring-type or gas-type to compensate for the incompressibility of the hydraulic fluid and provide a certain elastic behavior of the piston), the two cylinders should be at a substantially zero distance (e.g., 1 micron or less) when no material is fed into the nip, but this distance may increase when material is present. The actual distance between the two cylinders in the nip may depend on the volume and / or size of the material fed, its concentration, the rotational speed, the pressure applied to achieve contact, the time since the initial application, and similar factors. In certain embodiments, when an embossing roll is formed between two rotating cylinders, the initial spacing may be 400 μm, 300 μm, 200 μm, 100 μm, 80 μm, 60 μm, 40 μm, 20 μm, 10 μm, or 5 μm, and this distance is gradually reduced as liquid is removed and the rollers are pressed into contact in the presence of the material to be sheeted (e.g., the concentration of solid particles increases, causing the particles to agglomerate and compact to form a sheet).

[0099] As the stripping process progresses, dynamic adjustment of the nip gap size occurs naturally, without the need for specialized devices to controllably adjust the nip spacing directly (e.g., by fixing a cylinder at a predetermined distance). The periodic closing of the gap as the liquid material is sheeted (and liquid removed) in the nip, and the gradual opening of the gap as new liquid material enters the nip, can be considered a spontaneous elastic process. Therefore, the relative gap between the nip or nip-forming surfaces can be referred to as a "dynamic" gap to reflect this continuous phenomenon.

[0100] If a hydraulic system is used to push the cylinders into contact, the system may include an accumulator to provide the required gap change in the absence or presence of material. During the initial stages of the process, the rotating cylinders are considered to be in contact if they are temporarily separated by no more than 400 μm in the nip zone, even if this “contact” is mediated by the presence of intervening material or liquid.

[0101] The dry sheet obtained from this initial embossing gap is thinner, usually no thicker than the thickness corresponding to the solid content of the applied liquid raw material, and sometimes even thinner. For example, for a solution containing 25 wt.% sodium chloride, when the initial gap when the rollers are forced into contact in the nip is 400 μm, the thickness of the resulting sheet is at most about 100 μm.

[0102] In some embodiments, the gradually thinning material is recycled to the same nip where the flakes are collected. In other embodiments, the recycling may be to one or more nips different from the initial feed nip, which may be referred to as the first nip. Where there are multiple nips, each nip may consist of a pair of rollers that are non-contacting with the other nip rollers. However, in some embodiments, multiple nips may share common rollers. The rotating rollers of each nip, and of different nips, need not be identical. While they typically have similar axial lengths for efficiency, they may have different diameters, and / or be made of different materials, and / or coated with different substances, and / or be heated or cooled to different temperatures, etc.

[0103] In one embodiment, the material (e.g., flavor) is provided in the form of dry particles. While this method is applicable to any flavor in dry form (e.g., plant flavors from roots, stems, bark, leaves, flowers, or seeds), it is particularly suitable for flavors that cannot be dispersed or dissolved in a medium and can be relatively easily and efficiently separated from the medium. This "dry method" typically dilutes the flavor by at least five times from its initial size (e.g., diameter, edge, thickness) to its final thickness, followed by final recovery of the diluted flavor by rollers. This method is generally applicable to the preparation of microchips.

[0104] In one embodiment, the material (e.g., taste) is provided in the form of a relatively viscous paste (e.g., having a dynamic viscosity greater than 5,000 millipascal seconds (mPa·s) at room temperature (about 23° C.)). The viscosity of the paste can be achieved by dispersing a relatively large amount of the taste in a relatively small amount of liquid, or by using a liquid that itself has a relatively high viscosity. The dispersion medium should be compatible with the material to be formed into the tablet (e.g., if it is a taste stimulant, it should not affect its taste) and should be separable from it when necessary or desired. The dispersion medium itself can have a relatively high viscosity, and its selection should be based on the future use of the taste stimulant tablet. For example, the taste can be cocoa, and the viscous medium can be cocoa butter (both of which are insoluble in water) or sugar and molasses (both of which are soluble in water), and at least one rotating drum can optionally be heated or cooled to maintain the desired viscosity of the paste. This example is only illustrative and not limiting, and the dispersion (e.g., viscous) medium does not need to be from the same source or of the same type as the taste agent. This "paste method" typically allows the flavoring agent to be diluted from its initial size (before forming the paste) to its final thickness, after which the diluted flavoring agent can be recovered by rollers. This method is suitable for preparing microflakes and submicroflakes.

[0105] A dispersion medium suitable for forming a relatively viscous paste with the material can be an inherently viscous product (e.g., honey for flavors) or prepared by increasing the viscosity of a non-viscous liquid. By using a relatively high dosage of the material (e.g., flavors) and / or adding a thickener to the dispersion medium, the paste can exhibit a dynamic viscosity of at least 5,000 mPa·s at room temperature. If the material to be tableted is intended to impart flavor or be used in an edible product, the thickener should be as flavorless as possible and preferably (but not necessarily) certified food grade to ensure that residual amounts are not removed from the surface of the flavor tablet. Such thickeners can be natural or synthetic, and known types include alginic acid (E400), sodium alginate (E401), potassium alginate (E402), amino alginate (E403), calcium alginate (E404), propylene glycol alginate (E405), agar (E406), carrageenan (E407), branched cellulose (E408), tamarind gum (E410), oat gum (E411), guar gum (E412), tragacanth (E413), gum arabic (E414), and gluten (E415). 14), xanthan gum (E415), carrageenan (E416), tara gum (E417), gellan gum (E418), pectin (E440), gelatin (E441), cellulose (E460), methyl cellulose (E461), ethyl cellulose (E462), hydroxypropyl cellulose (E463), hydroxypropyl methyl cellulose (E464), methyl ethyl cellulose (E465), carboxymethyl cellulose (E466), natural or modified starch (E1400 series), and combinations thereof.

[0106] In one embodiment, the material (e.g., a flavoring agent) is present in a dispersed or dissolved form in a relatively non-viscous liquid (e.g., water) having a dynamic viscosity of less than 1,000 mPa·s, less than 100 mPa·s, or less than 10 mPa·s or less at room temperature. The liquid should be compatible with the material (e.g., not affect its taste, if it is a flavoring substance) and should be separable from it if necessary or desired. Flavoring substances suitable for this method are generally, but not limited to, soluble in the liquid, even if added at a concentration above its solubility limit, the flavoring substance is accordingly dispersed rather than completely dissolved in the liquid. This "liquid method" generally allows for a dilution of the flavoring substance from its initial size (before mixing with the liquid) to a final thickness of at least 15 times, followed by final recovery of the diluted flavoring substance by embossing rollers. This method is generally applicable to the preparation of microsheets, submicrosheets, and nanosheets.

[0107] As previously mentioned, it is emphasized that the selection of liquid carriers, additives, materials or coatings for various parts of the apparatus, and compatibility with any materials to be prepared in the present method and / or the apparatus should all be guided by the principle of compatibility. The materials should be chemically compatible. Fundamentally, a material or chemical composition is compatible with (or inert to, if desired) another material if it does not inhibit the activity of the other material or reduce its activity to a degree that would significantly affect its intended use. For example, a liquid carrier is incompatible with the material to be sheeted if it affects the taste of the material to be sheeted (as an edible substance) or affects the potency or reactivity of the material used in the manufacturing process. The materials should also be physically compatible. For example, the liquid carrier should be sufficiently volatile at temperatures that it does not affect the material to be sheeted. Thus, the materials should also be compatible with the manufacturing method and its operating conditions, and vice versa. For example, the liquid precursor used to dissolve or disperse the material to be sheeted should not corrode the surface to be coated, or the surface should be inert to the precursor and the sheet produced therefrom. Such general considerations are not discussed here in detail as they are well known to those skilled in the art of chemical manufacturing.

[0108] However, in some embodiments, the liquid may be selected to intentionally trigger a reaction with the material being flaked. In this case, the chemical composition of the material before and after flaking may be different. Therefore, the term "flaky material made from a material" encompasses both flakes that retain their original chemical composition after being processed by the flaking method, as well as flakes that contain modified versions of the material. For example, if calcium carbonate is flaked in neutral water, the resulting flake will be composed of calcium carbonate. However, if calcium carbonate is flaked in acetic acid, the resulting flake may be composed of calcium acetate, and the reaction of the carbonate with acetic acid also produces water and carbon dioxide.

[0109] Regardless of the form in which the material (eg, to be treated) is fed (eg, dry, pasty, or dissolved or dispersed in a liquid) to either or both surfaces forming the specific nip, the application may be continuous or intermittent.

[0110] In certain aspects, a method for preparing a sheet from a material dispersed or dissolved in a non-viscous liquid is contemplated, wherein one embodiment comprises:

[0111] a) providing at least one material (e.g., a taste agent or other active or inactive ingredient) dispersed or dissolved in a liquid to form a liquid (e.g., a taste agent) stock solution;

[0112] b) applying the liquid (eg, taste substance) material to a movable surface to form a thin film of the liquid (eg, taste substance) material;

[0113] c) removing at least a portion of the liquid from the thin film of liquid (e.g., taste stimulant) to form a thin layer of solid particles (e.g., precipitated taste stimulant), the thin layer optionally having a thickness of no more than 400 microns; and

[0114] d) aggregating and compacting the particles in the thin layer so that after most of the liquid is removed from the coating, the constituent components (e.g., taste substances) are essentially dry flakes (e.g., having a liquid content of less than 5 wt.% and optionally a thickness of no more than 200 μm, with a ratio of the longest planar dimension to thickness of at least 10:1).

[0115] While the liquid raw material can theoretically be applied to any initial thickness, thicker films are expected to require longer processing times compared to other conditions being equal. Therefore, in certain embodiments, the initial film thickness of the liquid raw material is 400 μm or less, 325 μm or less, or 250 μm or less, and the material should be uniformly dispersed or dissolved (or both) in the liquid upon application. The liquid raw material in which the material to be sheeted is dissolved in the liquid can be referred to as the "mother liquid." The liquid raw material in which the material to be sheeted is dispersed in the liquid can be referred to as the "dispersion liquid."

[0116] For similar reasons, although in theory the liquid feedstock can be used at any initial concentration, all other things being equal, it may be advantageous to use a relatively concentrated feedstock because its expected processing time is shorter than that of a relatively dilute feedstock. Obviously, a relatively high proportion of a material in a liquid will affect its viscosity. Therefore, it is emphasized that although the liquid carrier used to form the liquid stock solution may itself be non-viscous (e.g., having a dynamic viscosity of less than 1,000 mPa·s), the liquid stock solution itself may have a slightly viscous nature. Therefore, although the liquid stock solution may also be non-viscous, in certain embodiments, the dynamic viscosity of the liquid base may be as high as 5,000 mPa·s, 4,000 mPa·s, 3,000 mPa·s, 2,000 mPa·s, 1,500 mPa·s, or 1,250 mPa·s, measured at room temperature. As known to those familiar with the evaluation of the rheological properties of materials, the dynamic viscosity of the liquid feedstock may also depend on the probe of the equipment used for analysis, as well as its oscillation frequency and / or shear rate (if operated under continuous rotation conditions). These parameters may need to be adjusted depending on the behavior of the material being tested, so suitable settings are usually screened within a certain range, for example, oscillation frequency between 0.1 and 100 Hz (usually for materials with higher viscosity) and shear rate between 1 and 1,000 s -1 For relatively non-viscous products, the shear rate range is typically about 1 to 100 s -1The viscosity values ​​reported herein can be measured using a suitable rheometer, its components, and operating conditions within the stated operating range. In certain embodiments, the dynamic viscosity (e.g., the dynamic viscosity of a liquid carrier or a liquid feedstock prepared therefrom) is measured at a shear rate in the range of about 10 to 250 s-1 or about 50 to 150 s-1.

[0117] In some cases, it may be necessary to pre-treat the liquid feedstock and its components before applying them to the intended embossing surface. Pre-treating can include at least one of the following methods: a) reducing the particle size of the material to be dispersed, b) heating the liquid to promote dissolution or dispersion of the material, c) homogenizing the feedstock dispersion, and d) heating the liquid feedstock prior to application. From an apparatus perspective, an apparatus for providing such pre-treatment can be referred to as a pre-treatment station.

[0118] In certain embodiments, the surface to which the liquid material is applied can be wetted by the liquid material, and the liquid can spread evenly over the surface.

[0119] In certain embodiments, a film (e.g., a liquid flavoring agent material) is formed by intermittently or continuously applying the liquid material to a wettable surface (e.g., a wettable surface) that is movable, and interalia, by passing the applied material through a nip formed by contact between the movable surface and an opposing surface. The movable surface and the opposing surface facing each other at the indentation may also be referred to as the indentation-forming surface. When the two opposing surfaces are in motion, such as when an indentation is formed at the contact line of counter-rotating cylinders, all portions of the outer surface of the cylinders may periodically (cyclically) constitute the indentation-forming surface.

[0120] The applicator for the liquid raw material used as a metering device and the first movable surface are typically in relative motion relative to each other. Throughout this specification, the terms "taste raw material(s)," "liquid raw material," "raw material liquid," or "raw material" are used interchangeably to refer to a liquid (e.g., raw material) containing a dispersed or dissolved material (e.g., raw material). The raw material's liquid carrier can be composed of one or more fluids (and optional additives therein) that are relatively non-viscous (i.e., having a dynamic viscosity of less than 1,000 mPa·s at room temperature), such that the raw material has a viscosity of no more than 5,000 mPa·s when applied to the movable surface.

[0121] In certain embodiments, compaction of a thin layer of precipitated material (e.g., a taste substance or any other solid particles that are gradually separated from a mother liquid) is achieved by passing the thin layer of precipitated material (e.g., a taste substance or any other solid particles that are gradually separated from a mother liquid) through the same or at least one different roller used to flatten the liquid mother liquid into a thin liquid film, so that the material gradually precipitates from the liquid and the solid particles aggregate into larger structures (e.g., agglomerates), such that the resulting (e.g., taste substance) sheet has a thickness of no more than 200 μm, no more than 150 μm, no more than 100 μm, no more than 50 μm, no more than 20 μm, no more than 10 μm, no more than 5 μm, or no more than 1 μm, and the average ratio of the longest planar dimension to the thickness of the sheet (e.g., taste substance) is at least 10:1, 20:1, or 30:1 (also referred to as at least 10, at least 20, or at least 30 for simplicity). The thin coating (including the solid particles) is repeatedly passed through the liquid during evaporation, ultimately forming a sheet composed of aggregated and / or compacted solid particles. However, this semantic distinction can sometimes be arbitrary, as some areas of a thin coating may form sheets before the overall coating has dried sufficiently to allow the solid particles to compact into as many sheets as possible.

[0122] Importantly, the roller gap need not remain constant during the sheet formation process. Instead, the roller gap preferably varies dynamically as the steps or cycles proceed and / or complete. Although the rollers in the sheet formation method of the present invention can be considered "dynamic rollers," with their gap essentially varying with process conditions and states, for simplicity, they will be referred to herein as "rollers."

[0123] As shown in the exemplary embodiments described above, the thin liquid film and the resulting material layer are compressed between the compacting cylinders through one or more passes between one or more dynamic nips, and may also provide a "breaking" step to convert the material deposited in the material layer and the resulting dry layer into flakes. Thus, the breaking step can occur naturally in the aforementioned steps, without the need for additional operations. Breaking can also be achieved by actively separating or breaking up a dry layer containing aggregated particles, converting it into flakes of precipitated material consolidated by periodic compaction, and separating them in flake form. Breaking up a coating or dry layer that contains little liquid (e.g., having a water content of less than 5 wt.%) into flakes of compacted solid particles typically involves the natural detachment of flakes from the thin coating and / or the detachment of the layer containing flakes from a movable surface by auxiliary means, as well as the inherent or forced breaking up of the relatively dry layer into individual flakes. Since the formation of flakes involves different mechanisms that can be viewed separately as separation processes—either separation from the underlying surface or material or partial conversion into flakes from adjacent coatings—thus, thin coatings of precipitated solid particles, and layers in which the vast majority of their particles are aggregated and compacted, can be viewed as separable into flakes or composed of flakes.

[0124] To improve efficiency, the material (e.g., the substance to be tested) can be of a size that facilitates its dispersion or dissolution in the liquid, for example, by grinding to a maximum size of no more than 5 mm (e.g., if the material is soluble and the size reduction is intended to accelerate dissolution), or other sizes are used according to the pretreatment requirements of preparing the liquid solution to be used (e.g., reducing the material size to 10 microns or less, 7.5 μm or less, or 5 μm or less, if the material is not soluble in the liquid, such size reduction is intended to facilitate the initial passage of the dispersion through the press zone). The grinding pretreatment of the raw material can be carried out using any standard equipment, such as a coffee grinder, mortar and pestle, hammer mill, ball mill, jet mill, and other known equipment. Similarly, before applying the liquid raw material to the press roller, the liquid raw material can be pretreated by any suitable equipment (e.g., using a heater to heat the liquid, using an ultrasonic generator to accelerate dissolution, etc.). In addition, the apparatus for implementing the present method can be modified to achieve in-line pretreatment of the material to be sheeted (whether solid raw material or liquid raw material).

[0125] When the material is soluble in the liquid carrier of the slurry, the process can be accelerated by using a saturated or near-saturated solution, or by using both methods. A saturated solution is one in which the solute content has reached a level where, if further solute is added, it will not dissolve but instead precipitate out of solution as a solid. The maximum concentration of any substance (e.g., the analyte) in a saturated solution depends on the substance itself, its initial specific surface area, the dissolved liquid, the solution temperature, the applied pressure, and any other conditions (e.g., agitation) that maintain a uniform concentration of the substance in the solution. Thus, a solution that is saturated at a relatively high temperature may be supersaturated (contain more soluble substance than expected) at a relatively low temperature. A near-saturated solution contains less than the maximum amount that can be dissolved under the conditions set during solution preparation. Such a concentration (e.g., 70% to 90% of the maximum concentration) may be sufficient to achieve saturation under the various conditions encountered during tablet preparation.

[0126] In other words, although a solution can be prepared as a near-saturated, saturated, or supersaturated state upon completion of preparation, this classification may change during the process. For example, a near-saturated solution may become a saturated solution after the liquid is removed, or even become a dispersion when the material (e.g., the substance to be tested) begins to precipitate out of the solution (e.g., by crystallization of the material). In this context, a dispersion of a material that is soluble in a liquid indicates that the concentration of the material is higher than the allowable concentration for forming a supersaturated solution. Alternatively, the material can be dispersed in a liquid in which it is insoluble. For example, a material that is soluble in water is not necessarily soluble in alcohol.

[0127] As used herein, "precipitate," "precipitate," and their grammatical variations are not intended to refer exclusively to processes that result in the formation of a substance that is permanently insoluble in the liquid from which it is precipitated. Rather, these terms also include any process that results in the concentration of a substance or the formation of an insoluble substance to such an extent that it can be separated from a liquid as a solid, typically in the form of discrete solid particles, the extracted solid optionally being soluble in the liquid under varying conditions. Thus, a substance that is precipitated from a liquid may have previously been dissolved or dispersed therein. Crystallization is a special type of precipitation process in which a substance becomes ordered in structure as it solidifies due to a decrease in solubility. A particular material (e.g., a taste substance) may have multiple polymorphs if it is a crystalline substance, and such polymorphs are encompassed by this specification.

[0128] In certain embodiments, the step of dispersing or dissolving the material (e.g., the test substance) in the liquid is performed at a temperature above room temperature and not exceeding the boiling point of the liquid. Taking water as an example, the dispersing or dissolving step can be performed at a temperature of at least 30°C, at least 40°C, or at least 50°C; and not exceeding 95°C, not exceeding 90°C, or not exceeding 85°C. If the liquid is alcohol or contains a sufficient amount of alcohol, or contains any substance with a boiling point lower than that of water, the upper limit of the above temperature range should be lowered accordingly based on the relative proportion of the volatile liquid in the liquid, and the dispersing or dissolving step can be performed, for example, within a temperature range of 30°C to 75°C. The temperature that should not be exceeded in this step should also take into account the heat resistance of the material (or the heat resistance of the most sensitive material, if multiple materials are used). In the case of a taste substance, the temperature should preferably be below the temperature at which the taste of the taste substance is detectably impaired, which can be determined through sensory testing.

[0129] Regardless of the temperature at which the dispersing or dissolving step may be performed, the step may also be performed at non-atmospheric pressure. Furthermore, regardless of the temperature and / or pressure conditions, the dispersing or dissolving step may continue to agitate the liquid while dispersing or dissolving the material, and maintain the liquid uniformity during the formation of a continuous film (i.e., when applied to a surface). Regardless of the conditions selected for preparing the liquid feedstock, it may be applied to the removable surface at a temperature above ambient temperature. This is particularly true when the surface itself is heated to a temperature equal to or different from ambient temperature.

[0130] In certain embodiments, the removal of at least a portion of the liquid from the (e.g., flavoring) liquid material to form a thin, continuous film on the surface is rapid. Without being bound by any particular theory, it is believed that if the removal rate is rapid enough, liquid removal (e.g., evaporation) can occur while the material (e.g., flavoring substance) is still relatively uniformly dispersed or dissolved in the film. Rapid liquid removal at this stage can allow the precipitated material (e.g., flavoring substance or other solid particles) to form a relatively uniform coating, which in turn may promote densification of the coating (through agglomeration of solid particles) and its fragmentation into sheet-like structures having relatively uniform thickness. A structure has a relatively uniform thickness if the ratio of the maximum thickness to the minimum thickness, or the ratio of the maximum average thickness to the minimum average thickness, of the liquid film, dry coating, sheet, or nanosheet is less than or equal to 10, 8, 6, 5, 4, 3, or 2, respectively.

[0131] Preferably, the liquid removal rate in the present method is such that the formation of the precipitate (e.g., taste substance) coating can be completed within 1 minute after the liquid raw material film is formed. In certain embodiments, the liquid removal step takes 50 seconds or less, 40 seconds or less, or 30 seconds or less. If the liquid removal method also includes or further includes heating the surface on which the coating liquid solution forms a film, the liquid removal step may also be referred to as an accelerated evaporation step. In certain specific embodiments, the liquid removal or evaporation step takes 20 seconds or less, 15 seconds or less, or 10 seconds or less. The liquid removal or evaporation step can be carried out while blowing or suctioning away at least a portion of the liquid to be removed or its vapor.

[0132] While any liquid can be selected based on its ability to dissolve or disperse the material and the ease of removal for improved process efficiency, when taste substances or materials to be ingested by a living organism are involved, it may be advantageous to select a liquid that is approved for consumption by animals (e.g., humans). Such liquids are known and need not be described in detail, but examples thereof include water, alcohols, fatty alcohols, glycerol (also known as glycerin), propylene glycol, and combinations thereof. When the water-soluble material is not a taste substance, or is intended for animal ingestion (e.g., dietary supplements, medications, etc.), the liquid can be further selected from a wider range of fluids, but the intended use of the sheet material must still be considered. For example, if the sheet material is used in a manufacturing process, the liquid needs to be compatible with the process (e.g., not inhibit the intended reaction).

[0133] Preferably, but not necessarily, the liquid used to prepare the liquid stock solution (whether pure or mixed) should be capable of dissolving the material (e.g., taste substance) to a concentration of at least 1 gram of taste substance per 100 grams of liquid (1 weight percent), or at least 5 grams of taste substance per 100 grams of liquid (5 weight percent), at least 10 grams of taste substance per 100 grams of liquid (10 weight percent), or at least 20 grams of taste substance per 100 grams of liquid (20 weight percent), as measured at room temperature. If liquid remains on the outer surface of the tablet, the liquid should preferably be compatible with the intended use of the material. For example, the content of the taste substance should not exceed a level considered harmful to humans. In other words, when the material is intended for ingestion, the liquid should preferably be generally recognized as safe (GRAS), food grade, and / or labeled with any other similar designation indicating that it is suitable for oral administration.

[0134] Alternatively, the liquid, whether pure or mixed, should only be able to disperse the material (eg, tastant), in other words, the material should be dissolved in a concentration of less than 1 gram per 100 grams of dispersion (<1 wt %).

[0135] In certain embodiments, the movable surface (e.g., a surface wettable by a liquid) is the surface of a rotating cylinder. In this case, assuming the presence of a single extrusion point, the liquid removal step configured to remove at least a portion of the dissolved or dispersed liquid is preferably completed within no more than 60 cycles of the rotating cylinder. The number of cycles required depends on factors such as the initial concentration of the material (e.g., taste substance) in the liquid, the rotational speed of the cylinder, the surface temperature of the cylinder, the number of extrusion points arranged along the rotating cylinder, etc. In certain embodiments, the liquid removal or evaporation step is completed within 50 cycles or less, 40 cycles or less, 30 cycles or less, 20 cycles or less, or 10 cycles or less. Preferably, the liquid removal or evaporation step should be completed within 8 cycles or less, 6 cycles or less, 4 cycles or less, or 2 cycles or less, and ideally 1 cycle or less.

[0136] For the avoidance of doubt, it is emphasized that the gradual removal of liquid from the feedstock film does not require complete removal to initiate precipitation of materials (e.g., flavor substances). Thus, a coating of precipitated material can be compacted to form a sheet before the complete removal of liquid. In other words, removing a first portion of liquid may cause a first portion of solid particles to precipitate, while this first portion is being compacted (e.g., causing particles to agglomerate), removing a second portion of liquid may cause a second portion of the solid particles of the material to precipitate, and so on. Thus, while the steps of applying the liquid feedstock, partially removing the liquid until partial precipitation occurs, and compacting to partially break the precipitated material into sheets are sequentially correct, subsequent steps can be initiated without waiting for the complete completion of previous steps, and some steps may occur simultaneously in different regions of the liquid feedstock film, the precipitated coating, and the resulting compacted layer of aggregated particles. Based on the process principle of allowing different phases to coexist simultaneously, it is understood that if all steps are ideally completed in a single cycle through the nip, different regions of the movable surface (e.g., a rotating drum) may exhibit relative enrichment of different product phases.

[0137] When the liquid raw material (e.g., substance to be detected) film is converted into a thin layer of sediment (e.g., substance to be detected) and the surface on which the lamella is further formed is the outer surface of the rotating cylinder, the compaction of the particles can be achieved by passing through the nip zone multiple times in the nip zone between the rotating cylinder and the opposing surface that contacts each other through the mechanical mechanism. The reaction surface can be stationary, in which case the surface covered by the sediment material is in relative motion with the reaction surface. The reaction surface can also be movable, for example, can be a second rotating cylinder. In this case, the two surfaces can enter the nip zone at the same or different speeds, and the two cylinders can rotate in the same direction, or more typically, rotate in opposite directions.

[0138] While a nip (e.g., formed by two rotating drums pressed together) has been described as serving to confine a thin film of liquid feedstock, compact the coating of precipitated material (e.g., flavor), and optionally break the coating into flakes, this may not be the only function of the nip in this process. Without being bound by any particular theory, the pressure exerted by the nip on the thin film of liquid feedstock at room temperature is believed to facilitate the removal of at least a portion of the liquid from the film without further heating the drum surfaces. Regardless of the specific mechanism of action associated with the confined volume of liquid feedstock, its film, the precipitated coating, and / or the resulting flakes, these materials may pass through the nip one or more times. Control of the nip (e.g., through its operating parameters, such as rotational speed, temperature, contact pressure, etc.) is believed to determine, for example, certain characteristics (e.g., size, morphology, etc.) of the (e.g., flavor) flakes produced by the nip and / or process efficiency (e.g., production rate).

[0139] In some embodiments, the pressure applied by the nip is at least 10 MPa, at least 50 MPa, or at least 100 MPa. Typically, in the present method, the pressure applied along the desired contact line involving one or more nip surfaces does not exceed 1,500 MPa, and sometimes does not exceed 1,250 MPa, or does not exceed 1,000 MPa. If multiple nips are used in the present method, the pressure applied by one nip does not necessarily have to be the same as the pressure applied by another nip. This can occur when multiple indentations are arranged radially around a common central cylinder, with each outer rotating cylinder being pressed into contact with the central cylinder at a different pressure. In certain embodiments, the pressure applied at each indentation can independently be between 10 MPa and 1,500 MPa, between 50 MPa and 1,250 MPa, or between 100 MPa and 1,000 MPa. These pressure values ​​are calculated based on the maximum Hertzian contact pressure values ​​that can be applied to bring the surfaces of each indentation into contact.

[0140] The force / pressure used to cause the surfaces of the method / device to contact to form at least one nip need not be constant during the execution of any step of the present disclosure. For ease of illustration, assume that a material (e.g., a test object) is fed into a single nip in the form of a dry powder, and the powder needs to pass through the nip multiple times before it can be formed into a sheet. At this time, the force applied by the compression mechanism and the pressure felt at the nip can be gradually increased until a peak or plateau value within the above-mentioned suitable pressure range is reached. Alternatively, the force applied by the compression mechanism can be constant, but the pressure felt at different nip zones in a series of nip zones compressed by the same mechanism may be different. For example, consider a series of linearly arranged nip rollers, consisting of a series of rotatable cylinders of gradually decreasing diameter. The pressure felt at the nip rollers between the relatively smaller cylinders will be higher than the pressure felt at the nip rollers between the relatively larger cylinders, so that under the same applied force, the pressure increases as the diameter decreases.

[0141] Interestingly, the same mechanical mechanism can simultaneously act on two or more series of rotating cylinders / nips, with each series forming a separate module capable of producing the same or different (e.g., different mouthfeel) sheets, as described herein. For example, the same compression mechanism can apply force to a first set of rotating cylinders to form a first set of nip points (e.g., producing a sheet of a first material) while simultaneously applying force to a second set of rotating cylinders to form a second set of nip points (e.g., producing a sheet of a second material). The first and second sets of nip points are physically separate and can be arranged in parallel or in series.

[0142] This type of configuration can prepare two or more sheets of different materials on different sets of rollers at the same time, which has advantages when preparing sheet materials that need to be mixed. In this case, if the first material itself is a flavoring agent, the second material does not need to provide flavor separately. For example, the sheet-like first material prepared on the first series of rollers can be baking soda. According to the present invention, its flaking process is expected to reduce the sodium content in baking soda, thereby ensuring its effectiveness as a leavening agent when used in food. Since baking soda may need to add an acidic agent to react with it in products lacking natural acid to release carbon dioxide (ultimately making the product leavened in the batter), it is appropriate to flak a suitable second material at the same time. For example, a weak acid in crystalline form, such as acetic acid (CH3CO2H; E260), acidic calcium phosphate (ACP; Ca(H2PO4)2; E341), acidic sodium aluminum phosphate (SALP; E541), citric acid (HOC(CO2H)(CH2CO2H)2; E330), tartaric acid (C4H6O6; E334), or acidic sodium pyrophosphate (SAPP; Na2H2P2O7; E450), can be crushed in a second set of rollers to form a flake from a mixture of the two materials, thereby preparing baking powder or other foods (e.g., flour) that typically contain such agents. Similarly, when the materials to be flaked are not flavoring agents, they can be two or more materials suitable for use in the same manufacturing process, and potential "contamination" between flakes of the first material and flakes of the second (or third, etc.) material will not adversely affect the intended manufacturing process.

[0143] In view of the relatively high pressures that can be applied at the extrusion point, the rotating cylinder and the counter-pressure surface are preferably made of a material having sufficient hardness or other mechanical compressive resistance to avoid significant deformation and / or wear when subjected to such pressures. The rotating cylinder and the counter-pressure surface can be made of metal (e.g., stainless steel), or coated with metal (e.g., stainless steel), or coated with ceramic (e.g., tungsten carbide (WC)), or polymer (e.g., ), so their outer surfaces in contact must have a Vickers hardness of at least 50 HV, at least 100 HV, at least 150 HV, or at least 200 HV. Although the hardness of the material is not limited, it is usually not more than 10,000 HV (for example, if coated with a diamond-like carbon (DLC) film), and is often less than 5,000 HV, less than 3,500 HV, less than 2,000 HV, or less than 1,500 HV. The required hardness of any surface may decrease as the pressure applied to it decreases.

[0144] The hardness of the cylinder or its outer surface depends on: a) the specific composition of each cylinder and its coating (if any), and b) whether the base material has been further treated (e.g., annealed, cold worked, quenched, heat treated, or tempered), and the degree of treatment (e.g., stainless steel can be tempered to 1 / 16, 1 / 8, 1 / 4, 1 / 2, 3 / 4, or full hardness). Although the relative toughness of rotating cylinders is expressed in terms of hardness as described above, those familiar with the materials and their physical properties can easily convert such requirements into other terms such as strength, yield point, etc. All such alternative or additional parameters should be selected to avoid or minimize deformation and / or wear of the cylinder surface under the operating conditions of the method or apparatus.

[0145] In some embodiments, the rotating cylinder and the reaction surface are not only made of sufficiently hard and tough materials, but also have a desired surface topology (e.g., smooth or textured, whether random or not). In some embodiments, the surfaces pressed against each other are relatively smooth. In this case, their surface roughness (R a ) can be 500 nm or less, 400 nm or less, 300 nm or less, 200 nm or less, or 100 nm or less. Although a perfectly smooth surface would ideally exhibit an average surface roughness of zero, typically R a Greater than 20 nanometers.

[0146] The temperature of the rotating cylinder and the counter-surface can be adjusted using any suitable internal or external heating or cooling device. The temperature of the rotating cylinder and the counter-surface can be selected based on principles similar to those used when preparing a liquid standard solution (e.g., of an analyte). However, when using a liquid standard solution, there is no longer a need to avoid exceeding the boiling point of the liquid; the only consideration is the thermal sensitivity of the material.

[0147] Heating can be achieved through conduction, convection, and / or radiation, depending on the desired temperature. Conduction can be achieved by placing heating elements beneath the surface or liquid to be heated, or by circulating a hot liquid (such as heated oil or water) through appropriately placed pipes, chambers, or jackets. Convection heating can be achieved by blowing a hot gas (usually air) over the surface to be heated. Radiative heating can be achieved using microwaves (in an adapted cavity), but more commonly, infrared lamps are used to radiate heat toward the surface or material in question.

[0148] As known to those skilled in the art, the rate of supply of the liquid (e.g., the substance to be tested) depends on a variety of factors, including the surface tension of the liquid, the surface energy of the surface, the desired film thickness, the rate of removal of the liquid (e.g., evaporation rate) under the operating temperature and pressure conditions, the velocity of the surface at the nip, the size of the nip, and the like. The flow rate or intermittently applied dosage metering can be determined experimentally and adjusted as needed.

[0149] The film can be formed by passing the surface to be coated through a bath containing a liquid material (e.g., a solvent), or by dripping or spraying the liquid material onto the surface through one or more nozzles parallel to the axial length of the scoring line / rotating cylinder, the nozzles being arranged, for example, along the width of the movable surface, or by providing a device for smoothing the liquid material upstream (e.g., a doctor blade, air knife, scraper, etc.), or by other methods suitable for forming a very thin liquid film on the surface. As will be appreciated, in some embodiments, the liquid need not be applied as a film upstream of the pressure roller, and the pressure roller itself is used to flatten the excess liquid material forming the initial (optionally transient) upstream liquid pool into a downstream film.

[0150] As will be readily appreciated, for a predetermined concentration of material (e.g., a flavoring agent) in a liquid, a thinner film of the liquid feedstock (e.g., a flavoring agent) can achieve a faster rate of liquid removal, or at least a partial removal rate, than a thicker film, with all other conditions of the method being the same. In certain embodiments, the film has an initial thickness upon application to the surface (before any significant liquid removal) of 400 μm or less, 325 μm or less, 250 μm or less, 125 μm or less, 70 μm or less, or 35 μm or less. Typically, the film has an initial thickness of at least 250 nm, at least 500 nm, at least 750 nm, or at least 1 μm.

[0151] The above values ​​refer to initial thicknesses, as the method is intended to gradually remove some of the liquid over time, causing the thickness of the (e.g., to be measured) liquid to gradually decrease until the material settles to form a thin layer, first partially and then completely when the liquid is essentially completely removed in the final separable sheet. The thickness of the thin layer of precipitated material may also decrease with time and repeated compaction. As will be understood, "complete removal" of liquid is considered to have been achieved at the end of the flaking process, and does not mean that the formed flaky layer (composed of aggregated and / or compacted particles) or the flakes that can be separated therefrom will be completely free of liquid, which may remain in the "dried" coating in relatively trace amounts or adsorbed on the surface of the flakes. Any amount of liquid remaining in the layer of particles at the end of the process is acceptable, as long as the particles are present in a compacted and agglomerated form and can be crushed into commercially valuable flakes. In certain embodiments, at least partial removal of the liquid (e.g., partial evaporation) can produce a dry layer and / or broken (e.g., edible) flakes having a moisture content of 5% by weight or less, which can be determined by monitoring weight loss under appropriate conditions (e.g., temperature and time) to ensure that substantially all of the liquid has been removed without affecting the remaining solids. In certain embodiments, the flakes contain less than 4% by weight, less than 3% by weight, or less than 2% by weight of the liquid (based on the weight of the flakes). In other embodiments, the liquid content is 1% by weight or less, 0.8% by weight or less, 0.6% by weight or less, 0.4% by weight, 0.2% by weight, 0.1% by weight, or 0.05% by weight or less. The same upper limits on liquid content also apply to the compacted and / or agglomerated granular layer prior to comminution into flakes, which layer can be considered a representative sample of the dry layer.

[0152] While the present method for preparing tablets (e.g., flavor enhancers) would ideally be continuous, it can also be performed in an alternating "stop-and-go" manner when multiple rollers are used. In this case, one dose of liquid is applied first, and only after the first dose has been converted into tablets is the second dose applied, and so on. When the process involves multiple rollers, the second dose can be applied before the last roller collects the tablets. Therefore, it is believed that increasing the number of rollers could potentially shorten the time between separate dose applications and even make the process continuous.

[0153] The flakes (e.g., flavor enhancers) may be collected naturally in a collector where they are compressed as they pass through rollers and spontaneously fall off from a thin layer formed on the surface, gradually forming a layer of flakes; the flakes squeezed out from the rollers flow into the collector under the action of gravity. The flakes may also be actively collected in other ways, such as by using a blade, a gas flow (e.g., air or hot air), or other means suitable for peeling the flakes from the compacted granular layer or its underside. Typically, flakes that spontaneously detach from the rotating surface during formation are relatively large and / or thicker, while flakes that are actively detached by means of a detachment device are smaller. Generally, the flakes that detach spontaneously are made of a more brittle material.

[0154] The flakes obtained by this method (e.g., test samples) may not be sufficiently thinned to form microflakes, submicroflakes, or nanoflakes of the desired size after a single pass through the nip. In such cases, the flake product collected in the first nip can be further fed to one or more additional nips until the collected product exhibits the desired flake properties. It is believed that passing the flake through additional nip rollers, after most of the liquid has been removed or evaporated after circulating through the first nip rollers, helps remove any residual liquid that may have adhered to the surface of the flake.

[0155] Alternatively, or in addition, the tablets (e.g., flavor enhancers) obtained by this method may contain residual liquid that is incompatible with the intended use and / or storage stability. Regardless of the reason for eliminating the residual liquid, the method may further include a step specifically for removing the residual liquid, if any. For example, the tablets may be dried.

[0156] Because the tablets (e.g., flavor enhancers) prepared according to the present invention have a relatively higher specific surface area than their conventional, unflaked counterparts, some tablets may exhibit a greater tendency to absorb ambient moisture. This phenomenon may cause the tablet to clump, hindering its fluidity and making transportation, handling, storage, and application difficult. In such cases, the tablets may be treated with an anti-caking additive, which the method may further include. Alternatively or additionally, the treatment may be physical, such as drying the tablets before storing them in an environment free from other harmful factors (e.g., storing the dried tablets under vacuum or inert gas conditions or in a liquid that is impermeable to these factors and in which the tablets are stable (insoluble)). For example, tablets made from water-soluble flavoring substances can be stored in edible oil (or similar semi-solid or substantially solid lipophilic products) in which they are substantially insoluble, with the (e.g., vegetable) oil delivering the dispersed flavoring substances to the food before preparation or consumption.

[0157] In certain embodiments, the method may further include sorting the flakes (e.g., taste substances) by size to improve the size uniformity of each sorted subpopulation. For example, the flakes may be sieved through a screen having a desired pore size. A population of flakes having relatively uniform particle size is expected to provide a relatively more consistent effect, which is particularly important when standardized properties are desired for the flakes or products containing the flakes.

[0158] All optional steps performed after collecting the flakes (not limited to the examples above) can be referred to as post-processing steps or post-flaking steps. In an apparatus for manufacturing such flakes, the equipment or subsystems used to perform these steps can be referred to as post-processing stations or post-flaking stations, respectively.

[0159] While this method has been described for a single material (e.g., a taste stimulant), it can also be used to prepare tablets made from two or more materials. For example, if each material is crystalline, the method can be used to achieve co-crystallization, or to prepare tablets made from mixed materials (e.g., taste stimulants) by compaction. The terms "material(s)" or "taste stimulant(s)" may be used throughout this specification to indicate that one or more materials or taste stimulants can be used in the described process, device, or product.

[0160] Regardless of the variety of materials (e.g., flavor substances) used in the preparation, the tablets prepared according to the present invention typically comprise one or more individual elements of the precipitated material, such as individual crystals of the flavor substance having a crystalline structure when precipitated. The tablet is typically composed of a plurality of such elements, typically forming a continuous mosaic of the precipitated material (e.g., a plurality of salt or sugar crystals if the material is a crystalline flavor substance), while the coating of aggregated elements is not necessarily continuous. Preferably, in certain embodiments, the mosaic of precipitated material exhibits a substantially fused / substantially void-free state within the formed tablet, with virtually no gaps between the individual elements comprising the tablet.

[0161] Some implementations of this method and its steps include Figure 1 As shown, boxes with dashed outlines represent optional steps.

[0162] In a first step, S01, one or more materials (e.g., taste substances) to be formed into a tablet are provided. Typically, the materials are provided in the form of dry powders of various shapes and sizes. If the materials are provided in a paste or liquid form, the method can begin at step S03 to achieve the desired concentration of the material and / or viscosity of the liquid raw material, or even at step S04 if the material already has a desired concentration (e.g., suitable for forming at least a near-saturated solution) and / or the liquid raw material has a desired viscosity (e.g., not exceeding 5,000 mPa·s at the dispersion, dissolution, or application temperature).

[0163] If the materials (e.g., taste substances) are provided in dry powder form and one of the materials has a relatively large initial particle size (e.g., at least one dimension greater than 5 mm), the materials can be subjected to particle size reduction by any suitable method, preferably to a particle size not exceeding 5 mm in all dimensions, or even smaller, down to the micrometer scale, depending on the specific needs. For example, the second step S02 can include optionally grinding at least one of the materials provided in S01.

[0164] In a third step S03, at least one material (e.g., a taste substance) (which may have been ground to any desired particle size, such as a particle size in the low millimeter range (e.g., 0.5 to 5 mm) or low micrometer range (e.g., 0.5 to 10 μm)) is dissolved or dispersed in a liquid (the number of phases in the liquid depends on the relative amounts and / or the nature of the liquid and the ability of the material to dissolve therein). This step can be carried out under stirring, heating, and / or pressure, the specific methods being as described above and adjusted according to the liquid to be obtained.

[0165] In the fourth step S04, a liquid material (e.g., a substance to be tested) is applied to a movable surface (which may optionally be wetted by the liquid material). Typically, a device applying the liquid material contacts the surface to be coated in relative motion, causing the liquid material to form a thin film. The applied liquid can be set to a desired initial thickness using a dedicated leveling device, or the applied liquid (or a thin liquid film having a first thickness) can be moved toward a nip formed between the movable surface and an opposing surface to form a thin film.

[0166] The nip between two surfaces is formed by pressing one surface against the other, e.g. Figure 1 The pressing area can be a single pressing area or multiple pressing areas. The specific details will be described in the reference Figures 2 to 7 It is important to emphasize that, unlike conventional flattening or thinning devices, which are configured to maintain a constant distance from the material being processed, the indentations formed by the present invention under continuous extrusion pressure fluctuate in spacing as the thickness of the liquid feedstock changes. When the feedstock thickness drops to 1 micron or less, the indentation spacing can be reduced to 400 microns, or to this spacing after all sheet materials have detached from the forming surface.

[0167] Although the step S06 of optionally heating at least one movable surface or reaction surface appears to follow S05, this is not the only possible sequence of events. The operation of optionally heating the surface (or one of the surfaces) may alternatively or additionally be performed before the liquid raw material is applied (i.e., before S04) and / or before the liquid raw material reaches the nip (i.e., before S05).

[0168] In step S07, at least a portion of the liquid is removed from the thin film of liquid raw material (e.g., a flavoring agent) to increase the relative concentration of the material in the liquid phase and gradually separate it as solid particles. Ideally, the liquid should be removed rapidly to ensure that a thin layer of completely precipitated material (e.g., a flavoring agent) is formed during a single pass through a single nip, thereby allowing for continuous application of the liquid raw material, but this is not a requirement. The method can also be performed in a continuous manner, whereby a thin film of liquid raw material with increasing concentrations of solid particles is passed through a series of nips, with the precipitated layer typically transforming into a layer of dry aggregate particles after the last or penultimate nip. Alternatively, the method can be performed in a batch-like manner, whereby the thin film of liquid raw material is passed through the same nip or a series of nips multiple times, with the gradually precipitated layer of material typically transforming into a layer of dry aggregate particles after the last or penultimate nip. The gradual removal of liquid (e.g., by evaporation, which can be accelerated by heating the nip surface) results in material precipitation, which can also be a continuous process until the liquid is substantially completely removed. For example, in the case of a taste substance made from a crystalline material, the first precipitation of the taste substance may result in the formation of initial crystals, which in turn serve as nucleation centers for subsequent precipitation of the taste substance from the liquid mother liquor.

[0169] In the eighth step S08, the thin layer formed by the precipitated material (e.g., taste substance) is compacted (and optionally broken into flakes during the process, which naturally separate from the fully compacted portions of the thin layer). Similar to the gradual removal of liquid, the process of separating the solid particles from the liquid and gradually compacting them may occur once or multiple times in the same or different pressure zones. For simplicity, this step is referred to as "compacting," but it may actually achieve a variety of effects, which may occur simultaneously and not necessarily distinguishable, and may not all occur. Advantageously, as the liquid evaporates, the solid particles are gradually separated from the liquid and compacted. Regardless of the method or means used to achieve this, it is believed that this will cause the precipitate particles to aggregate into agglomerates with relatively high cohesion between the various components of the precipitate, and the thin layer formed by the agglomerated particles is relatively more uniform (e.g., in terms of thickness, etc.) than the sheet formed therefrom, compared to the layer formed by the same material through "pressureless precipitation." Thus, while conventional precipitation may form relatively loose aggregates of precipitate, the repeated passage of the liquid stream through the nip(s) and the resulting compaction of the precipitated material in the present invention is believed to initially involve a mixing process in which the individual precipitated elements can be seen to fuse with one another. Consequently, the flakes obtained by the present method may have a relatively low porosity and / or a relatively high transparency. In certain embodiments, the porosity of the (e.g., flavoring agent) flakes is 30% or less, 25% or less, 20% or less, or 15% or less. In certain embodiments, the porosity of the flakes is 1% or more, 2% or more, or 5% or more.

[0170] Although in the present figures the removal of the liquid (S07) is shown as taking place before the separation of the particles from the liquid matrix and the compaction to form the solid element (S08), in practice these two steps are typically repeated in a cyclic manner and may therefore occur simultaneously. Taking the example of a rotating cylinder to illustrate the formation of flakes on a movable surface, compaction can take place within the nip formed by the contact between the cylinder and the opposing surface, while the surfaces upstream and downstream of the nip are exposed, allowing the liquid to evaporate.

[0171] In step S09, the flakes formed by the thin layer of precipitate (e.g., the test substance) can be collected from the last surface. When the method is performed in multiple nip zones, collection can be performed in different nip zones. If the collected fractions have similar properties (e.g., similar size), different nip zones can be used to improve the production efficiency of the method. If the fractions collected in different nip zones have different properties (e.g., size, aspect ratio, etc.), different nip zones can be used to sort the flakes produced by the method.

[0172] The exemplary different pressing zones and their corresponding devices related to the present method will be referred to in their schematic diagrams (eg Figures 2 to 7 A brief description of the disclosed method steps is provided (see Figure 2). For clarity, some devices or components implementing the disclosed method steps are not shown in these non-limiting nip configurations. Omitted devices may be essential, including, for example: a compression mechanism for pressing at least one pair of surfaces together to form a nip roller; a drive mechanism (e.g., a motor, a connector, etc.) for rotating at least one rotatable cylinder; and a metering device capable of periodically providing a predetermined dose or a predetermined continuous flow of a liquid material to the applicator. Omitted devices may be optional, including, for example: a leveling device capable of forming a thin liquid layer of a desired thickness; a heating device capable of heating the coated surface during the coating process (heat can be applied from behind and / or in front of the surface); and a stripping device capable of "scraping" off the thin layer of precipitated material (e.g., flavoring agent) and breaking the resulting layer into the flakes that constitute it, with the device optionally being retractable, depending on the selected nip configuration. The aforementioned devices, as well as other equipment that may be used in conventional flake preparation processes (e.g., dryers, chambers, flake sorters, etc.), are well known in the art and will not be described in detail here. Furthermore, all devices may be mounted on and carried by a suitable structure or support frame.

[0173] For the sake of brevity, the operating principles common to all roller configurations are not necessarily repeated in the following description. To avoid ambiguity, although in these figures, the various roller configurations are shown with the roller surfaces in contact, in devices incorporating such roller configurations, the surfaces can be separated to allow maintenance (e.g., cleaning) or replacement of the surfaces when necessary. In addition, although in certain exemplary embodiments, the plane in which the rotational axes of the rotating cylinders are located is shown in a horizontal direction, this should not be considered limiting. For example, a pair of counter-rotating cylinders can be tilted relative to the horizon, with the liquid raw material applied at the upper end of the tilted rollers and the sheet collected at the lower end of the rollers. In theory, if the cylinders are of appropriate size (e.g., long enough), under appropriate operating conditions (e.g., liquid raw material flow rate, cylinder speed and temperature, pressure applied at the nip, etc.), such a structure can advantageously achieve continuous coating of the raw material and collection of the sheet produced thereby.

[0174] Figure 2 A schematic diagram illustrates a nip 200 formed by the mutual compression of a rotating cylinder 210 (whose outer surface 210' is a wettable material) and a planar (typically, but not necessarily, stationary) opposing surface 220 (whose outer surface 220' faces the cylinder). In this figure, an applicator for liquid material (e.g., flavoring agent) is represented by arrow 260, while a collector for flavoring agent particles is represented by container 270.

[0175] Although the applicator 260 can be any device capable of dispensing a liquid (e.g., a nozzle) or applying it to a surface (e.g., a brush) to cover the surface, the term is often used in this specification to refer to a device capable of applying a liquid material in the form of a continuous stream at a predetermined repeated application rate (e.g., 1 ml per minute) or at a predetermined flow rate (e.g., 1 ml / minute), where the amount of liquid repeatedly applied or the flow rate continuously applied is selected to avoid excess liquid material overflowing from the surface forming the nip area.

[0176] While collector 270 is depicted downstream of nip 200 for simplicity, it could be located anywhere along the path of rotating surface 210'. Because cylinder 210 not only rotates about its axis but also moves along stationary reaction surface 220 (as shown, moving up and down), flakes can be collected into collector 270 from a thin layer formed on surface 220'. This can be accomplished by keeping the axis of rotation of cylinder 210 stationary and moving counter surface 220 relative to it (as shown, moving up and down), or by offsetting the axis of rotation of cylinder 210 and counter surface 220 in the Z direction (as shown in this figure), while ensuring that the two surfaces remain in contact (i.e., maintaining nip 200). Flake collection can occur through spontaneous shedding of flakes, as the liquid or a portion thereof is gradually removed, forming a thin layer of sediment that is compacted as it passes through the nip, each of which lasts for one or more rotations of cylinder 210 and passages through nip 200. The collection of the flakes may also involve a detachment device that can be controlled to operate after a relatively dry layer (composed of precipitated and agglomerated material flakes) has formed, where the flakes typically contain no more than 5 wt.% of liquid. For example, the detachment can be promoted by, when necessary, directing a stream of air onto the layer composed of flakes, or by placing a suitable mechanical obstacle (e.g., a blade) close to the layer to scrape it off from the bottom surface into individual flakes.

[0177] Figure 3 A schematic depicts a nip 300 formed by the contact of opposing surfaces of a first rotating cylinder 310 (whose outer surface 310' is wettable) and a second rotating cylinder 320 (whose outer surface 320' is wettable). In this figure, the two cylinders rotate in the same direction (e.g., clockwise), creating sliding motion along the line of contact. An applicator for a liquid material (e.g., a probe) is represented by arrow 360, while a collector for the (e.g., probe) flakes is represented by container 370, which can be located anywhere downstream of indentation 300, but can also be located anywhere along the path of rotating surface 310', preferably along the path of rotating surface 320'.

[0178] Figure 4 The diagram schematically shows a pressing point 400 formed by the mutual pressing of the opposing surfaces of a first rotating cylinder 410 (having a wettable outer surface 410') and a second rotating cylinder 420 (having a wettable outer surface 420'). Figure 3In contrast, the two cylinders rotate in opposite directions (e.g., one clockwise and the other counterclockwise). Ideally, if the two cylinders rotate at the same speed, slippage at the contact line is avoided, but this is not a requirement. An applicator for a liquid (e.g., a test substance) is represented by arrow 460, and a collector for particles (e.g., a test substance) is represented by container 470. This container can be positioned at any position downstream of roller 400, but can also be positioned at any position along the path of rotating surface 410', and is preferably positioned at any position along the path of rotating surface 420'.

[0179] Figure 5 A series of linearly arranged nip rollers 500a, 500b, and 500c are schematically shown. Nip roller 500a is formed by the interaction of opposing surfaces of a first rotating cylinder 510 (whose outer surface 510' is a wettable material) and a second rotating cylinder 520 (whose outer surface 520' is a wettable material). Nip 500b is formed by the contact between the second rotating cylinder 520 and the reaction surface of a third rotating cylinder 530, where the third rotating cylinder 530 has an (e.g., wettable) outer surface 530'. Nip 500c is formed by pressing the third rotating cylinder 530 against the reaction surface of an opposing fourth rotating cylinder 540, which has an (e.g., wettable) outer surface 540'. The applicator of liquid material (e.g., flavoring agent) is represented by arrow 560, and the collector of particles (e.g., flavoring agent) is represented by container 570, which is arbitrarily drawn downstream of nip 500c, but can be located anywhere along the path of rotating surfaces 510', 520', 530', and is preferably collected by rotating surface 540'. Figure 5-7 As shown, multiple collectors can be used in multiple roller groups if desired. Although the example in this figure uses four cylinders of similar size, with each pair of cylinders rotating in opposite directions, this linear arrangement is not necessary. A linear arrangement of rollers can be achieved by using three or more rollers (the rollers can be the same or different, rotate in the same or different directions, and / or rotate at the same or different speeds). In a linear arrangement of rollers, each pair of rollers can be separated from the adjacent pair of rollers if a single compression system and / or a single motor can be used to push and / or rotate any two pairs of rollers into rolling contact.

[0180] In some cases, a series of rollers (whether or not Figure 5-7 The roller assembly (shown in FIG. 1 ) includes a sufficient number of rollers to meet the operating conditions required for preparing a tablet (e.g., a taste agent), thereby allowing for the presence of multiple applicators (e.g., metering devices) capable of delivering a liquid material (e.g., a tastant) to one of the outer surfaces of the plurality of cylinders comprising the roller assembly. The liquid material delivered by all applicators can be the same, and this configuration is suitable for continuously applying the liquid material and collecting the resulting tablets.

[0181] Figure 6 Schematically, a plurality of radially aligned nip rollers 600a, 600b, 600c, and 600d are shown, facing a common central rotating cylinder 610 having an (e.g., wettable) outer surface 610' (not shown). The nip roller 600a is formed by the opposing surfaces of the first rotating cylinder 610 and a second rotating cylinder 620, which has an (e.g., wettable) outer surface 620' (not shown). The nip 600b is formed by the opposing surfaces of the first rotating cylinder 610 and a third rotating cylinder 630, which has an (e.g., wettable) outer surface 630' (not shown). The nip 600c is formed by the reaction surfaces of the first rotating cylinder 610 and the fourth rotating cylinder 640, which has an outer surface 640' (e.g., wettable) (not shown). The indentation 600d is formed by the reaction surfaces of the first rotating cylinder 610 and the fifth rotating cylinder 650, which has an outer surface 650' (e.g., wettable) (not shown). The applicator of the liquid material (e.g., a flavoring agent) is indicated by arrow 660, and the collector of the (e.g., flavoring agent) particles is indicated by container 670, which is arbitrarily drawn downstream of the indentation 600c but can also be located on rotating surfaces 610', 620', 630', 640', and preferably on rotating surface 650'. For example, the collector 670 can be located downstream of the pressing roller 600d. While this figure illustrates radial alignment of the nip with four similarly sized cylinders arranged diametrically on either side of a common central cylinder, with each outer cylinder counter-rotating relative to the central cylinder, this is not a requirement. Radial alignment of the nip can be achieved with any other number of outer cylinders, three or more, with the same or different cylinders, rotating in the same or different directions, and / or rotating at the same or different speeds.

[0182] It is worth noting that in Figure 6 In the embodiment, rotating cylinders 620, 630, 640, and 650 are arranged to contact the outer surface of central rotating cylinder 610, to which the liquid feedstock is applied for processing by the present method. Alternatively, they may face the cylindrical wall of 610 from the inside. In this case, rotating cylinder 610 should be a hollow cylinder or drum, and the liquid feedstock should be applied to the inner surface of the hollow cylinder. Similarly, collector 670 should be located within the hollow chamber of 610.

[0183] Whether located inside or outside of the central rotating cylinder 610, multiple cylinders (e.g., 620, 630, 640, and 650) can be positioned and rotated in contact with 610 to achieve different ways of applying the liquid feedstock. Specifically, instead of spraying the liquid feedstock onto the first nip in the series through one or more nozzles parallel to the nip, the liquid feedstock can be applied by partially immersing the cylinders in the first nip in a bath filled with the liquid feedstock. In the latter case, the appropriate metering of the liquid feedstock applied to the surface is determined by the surface energy of the cylinder surface immersed in the bath and the surface tension of the liquid feedstock, with excess liquid typically dripping back into the bath by gravity before the remaining film enters the downstream nip.

[0184] Figure 7 A schematic depicts a nip array configuration combining the principles of linear and radial nip alignment. The nips between rotating cylinders 710, 720, 730, 740, and 74B form a linear alignment, while the nip rollers between 71A, 71B, and 710, or 72A, 72B, and 720, or 73A, 73B, and 730, or 74A, 74B, and 740 are considered to be radially aligned with rotating cylinders 710, 720, 730, and 740, respectively. An applicator for liquid material (e.g., a test substance) is represented by arrow 760, while a collector for the test substance (e.g., a test substance) is represented by container 770, which is arbitrarily drawn downstream of the nip formed by rotating cylinders 740 and 74C.

[0185] In some of the above configurations, especially those including a series of nips, necessary or optional devices not shown in the figures for clarity may be repeated. For example, each rotating cylinder may be independently driven by a different motor. When considering level adjustment and / or separation devices, they do not need to be located only on the first and last cylinders, but may be repeated along the series of nips. Figure 6 For example, a first flattening device can be located downstream of the liquid feed at roller 610 and upstream of roller 620; a second flattening device can be located adjacent to roller 620, or again adjacent to roller 610 but downstream of nip 600a. Similarly, a final stripping device can be used to strip flakes from the surface of roller 650, but a stripping device can be located upstream of it, for example, to remove flakes (e.g., flavoring agents) from the surface of roller 610 (between nips 600c and 600d). Additional collectors may be required in addition to 670, depending on their specific structure and mode of operation, as well as the precise relative positioning of the stripping devices.

[0186] In certain embodiments, regardless of the alignment employed by the series of rollers (e.g., linear and / or radial), the number of rollers and the rotating cylinders comprising the rollers are selected to ensure continuous application of the (e.g., reagent) liquid feedstock and collection of the (e.g., reagent) sheet material upon completion of the process under the established operating conditions.

[0187] According to another aspect of the present invention, there is provided an apparatus for preparing a sheet from a material dissolved or dispersed in a liquid, the apparatus comprising:

[0188] a) a supporting frame,

[0189] b) at least two cylinders mounted on a frame, at least one of which is movable relative to the support frame,

[0190] c) a mechanical device for applying a force to bring the cylinders into contact with each other to form at least one clamping area, and

[0191] d) a drive motor for rotating at least one cylinder,

[0192] It is characterized by

[0193] e) a metering device for applying liquid raw material to at least one cylinder so as to form a thin film only on the surface of the cylinder, wherein the concentration of solid material in the film increases as the film passes through the at least one nip multiple times, thereby forming a sheet of material, and

[0194] f) a controller for adjusting the rate at which liquid stock is applied to the at least one roller to match the rate at which liquid is lost from the film as the film continues through the at least one nip.

[0195] Because the two or more rotatable rollers of the present apparatus are pressed into contact during operation of the sheet forming system, the nip formed between any two adjacent rollers may vary in spacing during the process. Even if the force mechanism pushes the rollers into contact with a constant force, when the material to be sheeted is being conveyed, the nip gap (separation distance) may be larger than under similar conditions without the supply of liquid raw material (e.g., before the supply of raw material or after sheeting is completed).

[0196] In certain embodiments, the apparatus further comprises a flattening device for evenly distributing the (e.g., flavoring) liquid material into a thin film before the material passes through the nip. Unlike the preferred nip of the present invention, the flattening device can be positioned at a fixed distance from the surface of the liquid to be flattened.

[0197] In certain embodiments, the apparatus further comprises at least one heating device for heating the liquid material (eg, taste agent) dispensed by the metering device and any surface of the two or more rotating cylinders.

[0198] In certain embodiments, the apparatus further comprises a separating device for separating the flakes (e.g., of the flavoring agent) from the film of removed liquid, i.e., from the thin layer or flakes of solid material formed by precipitation, agglomeration, and compaction, for collection by a collector.

[0199] In some embodiments, the apparatus further comprises a controller for continuously or periodically controlling at least one of the following:

[0200] a-the amount of liquid material dispensed by the metering device and / or the dispensing cycle or rate of the liquid material;

[0201] b-force or pressure applied by the force mechanism (also called compression mechanism);

[0202] c-the rotational speed of at least one rotating cylinder; and

[0203] d- The temperature of the liquid feed and / or the temperature of any surface of the two or more rotating cylinders.

[0204] Such control systems are well known and require no further explanation. They can be based on feedforward active control, setting predetermined target values ​​to meet requirements, and / or feedback control, responding to signals related to the controlled parameter. For example, the inventors have discovered that when the material in sheet form contacts a rotary cylinder, the motor torque of the rotary cylinder can predict when the next dose of material can be applied during a discontinuity in the sheet material processing process. Thus, a liquid applicator or metering device (e.g., as indicated by arrows 260, 360, 460, 560, 660, and 760 in the previously described figures) can be controlled by such a feedback mechanism to release a new dose of liquid at each (e.g., first) nip (e.g., rollers 200, 300, 400, 500a, 600a, and between rotary cylinders 710 and 720). When the motor torque (measured by a torque measuring device) reaches a minimum value (corresponding to the lowest proportion of liquid in the sheet), another suitable controller can monitor the progress of the sheeting process and adjust the metering device accordingly. Other types of control may involve the force or forces applied by the compression mechanism, which may be monitored, for example, by strain gauges located near the controlled nip and adjacent to the compression mechanism.

[0205] In certain embodiments, the outer surfaces of two or more rotatable cylinders in the device are made of or coated with a material that is wettable by a liquid feedstock (eg, a substance to be tested).

[0206] In certain embodiments, the outer surfaces of two or more rotatable cylinders in the apparatus are made of or coated with a material having an average surface roughness (Ra) of 500 nm or less, 400 nm or less, or 300 nm or less.

[0207] In certain embodiments, the outer surfaces of two or more rotatable cylinders in the apparatus are made of, or coated with, a material having a Vickers hardness between 50 HV and 10,000 HV, between 100 HV and 5,000 HV, between 150 HV and 3,500 HV, or between 200 HV and 2,000 HV.

[0208] According to another aspect of the present disclosure, a product (also referred to as a manufactured product) is provided, which includes a sheet of water-soluble or water-insoluble material as disclosed in the present disclosure, and / or is prepared by the present method, and / or is prepared using the present device.

[0209] According to another aspect of the present disclosure, there is provided a food product comprising the taste tablet as described above, and / or prepared by the method, and / or prepared using the device.

[0210] According to another aspect of the present disclosure, a method for improving an article of manufacture is provided, comprising incorporating into an article of manufacture a sheet disclosed herein, and / or a sheet prepared by the present method, and / or a sheet prepared using the present apparatus, wherein the sheet comprises or consists of at least one active or inactive ingredient. The improvement in the article of manufacture can be reflected in its chemical efficacy, physical efficacy, biological efficacy, quality, ease of preparation, storage, or transportation, or cost of preparation, storage, or transportation, to name a few areas in which an article of manufacture can be improved by the sheet of the present invention.

[0211] According to another aspect of the present disclosure, a method for improving food is provided, comprising adding a sheet as described herein, and / or a sheet prepared by the present method, and / or a sheet prepared using the present device, to a food or beverage, wherein the sheet optionally has a flavor. The improvement in food may be reflected in its taste, smell, freshness, texture, appearance, or ease of preparation, all of which are areas where food improvement may be desirable and can be achieved using the sheet of the present invention.

[0212] Food enhancement can also be manifested in extending the duration of properties exhibited by food after fresh preparation, or delaying the degradation of these properties over time, properties that consumers desire using all the senses commonly used to evaluate the sensory properties of food products. Therefore, in a broader sense, flavor enhancers do not necessarily need to provide taste, but rather assist in the perception of the quality of food products, such as emulsifiers, thickeners, binders, gelling agents, texture modifiers, hardeners, fermentation agents, stabilizers, preservatives, anti-caking agents, humectants, pH adjusters, colorants, flavor enhancers, vitamins, mineral nutrients, and any food additives that are intended to have a positive effect on the properties of food, whether for consumption, production, processing, handling, packaging, transportation or storage.

[0213] According to another aspect of the present disclosure, a method for reducing the amount of a certain material used in a manufacturing process or a manufactured product is provided, the method comprising replacing at least a portion of the material in the process or product with a sheet disclosed in the present disclosure, and / or a sheet prepared by the present method, and / or a sheet prepared by the present device.

[0214] According to another aspect of the present disclosure, there is provided a method for reducing the amount of taste substances used to impart a desired taste to a food, the method comprising replacing at least a portion of the taste substances in the food or beverage with a taste substance tablet disclosed in the present disclosure, and / or a taste substance tablet prepared by the present method, and / or a taste substance tablet prepared by the present device.

[0215] For the sake of brevity, the methods and apparatus of the present invention are primarily described as being suitable for preparing taste enhancer tablets suitable for use in the food industry or other industries that rely on oral administration or the use of products that have flavor and / or contribute to product quality (e.g., foods). However, they can also be used to prepare tablets of any other active or inactive ingredient for any other purpose. The raw material to be formed into a tablet need not have a flavor, nor need it be suitable for animal consumption or use, nor need it be designed specifically for the food industry. For example, the product to be formed into a tablet can be any product as long as this particular form is beneficial to it, such as promoting dissolution, dispersion, decomposition, release into the surrounding environment, absorption by relevant organisms, or any other process in which the relatively increased specific surface area is beneficial to the product's efficiency.

[0216] Example

[0217] Example 1: Drying and flaking of taste substances

[0218] In this example, commercially available sugar, salt, and ground coffee were selected as flavor substances and fed in the form of dry powder for flaking. Sugar and salt are water-soluble materials, while coffee, although it contains water-soluble components, is considered a water-insoluble material. The dry sample is fed into a Figure 5 The clamping device shown in FIG. 1 is composed of three rotating cylinders. The two rotating cylinders 510 and 530 are composed of Made of stainless steel (Vickers hardness 240HV, average surface roughness R aLess than 1,600nm) and a diameter of 30cm. The rotating cylinder 520 located between cylinders 510 and 530 is made of tungsten carbide and has a diameter of 1 cm. The axial length of the three cylinders is 25 cm. They rotate in opposite directions at a similar speed (20 revolutions per minute, rpm) and are squeezed into contact under the action of a calculated Hertzian contact pressure (up to 750MPa), which is applied by a compression mechanism that provides a force of 1.5 tons, in this case a hydraulic cylinder. Granular sugar is fed into the pressure zone and the surface temperature of the rotating cylinder is about 23°C. After a single application of 1 gram of sugar and passing through the pressure roller 6 times (reported as the number of cycles below), the flaky sugar is collected using a scraper coated with ceramic material, which is appropriately positioned and oriented to peel the flakes from its bottom surface. The experiment and the resulting flakes are named DF-1. The particles to be examined were placed on an aluminum pin-shaped SEM stage covered with double-sided adhesive carbon tape. SEM-FIB microscopic images were acquired using a Zeiss Crossbeam 340 microscope at x100 magnification, 1.2 kV electron high voltage (EHT), and a 30 μm aperture size. Samples were measured at the beginning and end of the exfoliation process, and their average size was assessed based on at least 10 individual particles or flakes detectable in the field of view. Typically, 20–30 discrete particles were selected from one or more fields of view. All initial particles were approximately spherical, even if slightly cubic in shape, to express the initial size of the sample as an average diameter. Figure 8A is a photo of sugar particles before entering the device, and Figure 8B This is a photo of the sugar sheet obtained under the above conditions.

[0219] The conditions and results of the dry flaking method described in detail above and similar methods are summarized in Table 1 according to the preparation method and feed rate of all tested particles. In this table and the following tables, SS stands for stainless steel. WC stands for tungsten carbide, Represents the average diameter of the feed particles or the diameter of the rotating cylinder.

[0220] Table 1

[0221]

[0222] Example 2: Paste peeling of sample

[0223] In this example, coffee granules with an average diameter of about 500 μm are dispersed as a dry powder in a viscous medium and fed into a Figure 4 The first and second rotating cylinders 410 and 420 have the same structure and are both made of Made of stainless steel (Vickers hardness 240HV, average surface roughness R aLess than 1,600nm), a diameter of 30cm, an axial length of 25cm. They rotate in opposite directions at a similar speed (60rpm), and are squeezed into contact under a pressure of 370MPa when the calculated pressure is calculated, and the pressure is produced by a compression mechanism providing 7.5 tons of force, and a hydraulic cylinder is adopted in this example. Granular coffee is mixed into a viscous medium made of a 20wt.% xanthan gum aqueous solution in a mass ratio of 1:10, and the medium is measured at room temperature using a suitable rheometer (Thermo Scientific (Germany) Haake Mars III), which is equipped with a C20 / 1 ° rotor, a 0.052mm gap, a 0.04ml volume, and a shear rate-oscillation frequency sweep range of 0.1-100Hz, with a gamma value of 1%. The resulting paste is fed into a press roller, and the surface of the rotating cylinder is in room temperature. After a single coating of 0.5 gram of paste and passing through a press roller 20 times, the adapted scraper described in detail previously is used to collect the flake coffee at least partially wrapped with a viscous medium from the cylinder surface. This experiment and the resulting flakes were designated PF-1. As previously described, SEM-FIB micrographs were taken at the beginning and end of the flake formation process, and the average size of at least 10 individual particles or flakes detectable within the field of view was evaluated. Figure 9A is a photo of coffee particles before entering the device, and Figure 9B These are photos of coffee flakes obtained under the above conditions, both magnified 100 times.

[0224] The conditions and results of the above-mentioned flaking method are summarized in Table 2.

[0225] Table 2

[0226]

[0227] Example 3: Liquid tableting of flavoring material

[0228] In this case, whether the material is water-soluble or water-insoluble, it is delivered in the form of a solution or dispersion in a non-viscous liquid to a device having a pressing roller (such as Figure 4 or Figure 5 The materials tested, which can be used as taste substances and / or for other applications in other industries, include: A: salt, citric acid, potassium chloride, sodium bicarbonate, and disodium hydrogen phosphate (monohydrate and dihydrate), which are considered water-soluble materials; and B: calcium carbonate, dyes, magnesium stearate, silicon dioxide, and zinc oxide, which are considered water-insoluble materials.

[0229] Regarding the non-limiting potential uses of the water-soluble materials prepared in this example, salt and citric acid (E330) are both well-known for their dual roles as flavor enhancers and food preservatives, but both can also perform a variety of additional functions in other industries. Potassium chloride can be used as a substitute for sodium chloride in the food industry and as a thickener, flavoring agent, and pH regulator. It can also be used as an electrolyte supplement in medicine, a fertilizer in agriculture, and as a water softener in related industries. Although sodium bicarbonate (E500) has a slightly bitter and salty taste, it is more widely known for its use as a leavening agent for baked goods. It is also widely used in other industries (for example: as an antacid in medicine to relieve heartburn and indigestion, as a detergent in personal care or cleaning products, etc.). Disodium hydrogen phosphate (E339(i)) and disodium dihydrogen phosphate (E339(ii)), also known as monosodium phosphate (MSP) and disodium phosphate (DSP), are considered relatively tasteless but can be used in food as emulsifiers, thickeners, leavening agents, anti-caking agents or pH adjusters. In other industries, they are used in detergents and cleaning products, while in medicine they are used as laxatives (for example before colonoscopies).

[0230] Regarding the non-limiting potential uses of the water-insoluble material (in flake form) described in this example, silicon dioxide (also known as silicon) can be used in a variety of applications, such as in the production of concrete in the construction industry, in hydraulic fracturing (when it is in crystalline form), glass production, sedatives, elemental silicon production, an anti-caking agent for powdered foods (such as spices), a clarifier for juices, beer and wine, in the pharmaceutical industry for tablet production, and in toothpaste to remove plaque. Zinc oxide is widely used as a filler or filler and as a white pigment. It is found in certain rubber, glass and ceramic products and is used as a catalyst in the chemical industry. It is also used in coatings as a preservative and mildew inhibitor. Because zinc is an essential trace element, zinc oxide is also added to fertilizers, animal feed and vitamin supplements. It is also used in cosmetics and medical products for its antibacterial and deodorizing properties. Its strong absorption properties for ultraviolet (UV) light lead to its use in sunscreen products. Near-infrared (NIR) dyes, such as QCR Solutions Corp's NIR983A, can be used to create images that can be read by specialized infrared detectors, for example in security solutions ranging from QR codes to semi-disappearing images, or as research tools or diagnostic imaging in chemical biology or medicine. The use of NIR dyes for tumor-specific imaging may open up new avenues for photothermal therapy and photodynamic therapy. Magnesium stearate can be used in the food and pharmaceutical industries, typically as an emulsifier, binder, thickener, as well as an anti-caking agent, lubricant, release agent, and defoaming agent. The various uses of calcium carbonate have been described previously and will not be repeated here.

[0231] Regarding the preparation method, ordinary table salt (sodium chloride, NaCl) is first briefly ground in a coffee grinder to a particle size of about 500 μm, and then fine salt with a particle size of about 50 μm is prepared. The ultrafine salt is mixed with water in a mass ratio of 1:3 at room temperature until it is completely dissolved. For reference, the solution is considered to be nearly saturated, where the mass percentage concentration of sodium chloride is 25 wt.%, while a saturated solution at the same temperature contains about 35 grams of sodium chloride per 100 grams of pure water (that is, the mass percentage of salt in the total weight of the solution is about 26.5 wt.%). The resulting liquid raw material is fed into a Figure 4 The two rotating cylinders 410 and 420 are composed of Made of stainless steel (Vickers hardness 240HV, average surface roughness R a Less than 1,600 nm), with a diameter of 30 cm and an axial length of 25 cm. The two cylinders rotated in opposite directions at the same speed (60 rpm) while being forced into contact with a calculated Hertzian contact pressure (370 MPa) by a hydraulic piston providing a force of 7.5 tons, while the cylinder surfaces were at ambient temperature. 0.5 ml of liquid was applied to the middle of the cylinders, extending parallel to the axis along the indentation direction, and after 38 indentations, the salt crystals were collected using an adapted scraper as previously described in detail. This experiment and the resulting salt crystals were designated LF-1. As previously described, SEM-FIB micrographs were taken at the beginning and end of the peeling process, and the average size of at least 10 individual particles or crystals detectable within the field of view was evaluated. Figure 10A This is an X100 magnified photo of the salt particles before they are dissolved and fed into the device. Figure 10B This is a photo of a salt flake obtained under the above conditions at a magnification of X1,000.

[0232] The conditions and results obtained using the liquid stripping method described in detail above and similar methods are summarized in Table 3A and subsequent paragraphs when the material is water-soluble, and in Table 3B when the material is water-insoluble. In the table and in each example, water refers to pure double distilled water and Citric Ac. refers to citric acid. For LF-2 and LF-3, the surface of the rotating cylinders 410 and 420 is preheated to the desired temperature by blowing hot air onto the rotating surface. In addition, the liquid raw materials of the salt solution and the salt dispersion are applied at the same temperature (obtained by stirring the liquid raw materials on a hot plate). For LF-4 and LF-5, the apparatus includes a series of clamping devices, such as Figure 5As shown. For LF-4, rotating cylinders 510, 520, and 530 are identical to those described in Example 1. For LF-5, a series of six identical cylinders are used, arranged linearly, allowing the liquid material to pass through any nip and continuously coating the liquid material on the first cylinder while continuously collecting the taste particles on the sixth cylinder. For LF-6, the configuration is similar to that described for LF-1, but the nearly saturated solution of the taste substance is made of citric acid (HOC(CO2H)(CH2CO2H)2).

[0233] Table 3A

[0234]

[0235]

[0236] Figure 11A This is an X100 magnified image of the salt particles before they are dispersed and fed into the device. Figure 11B This is a X1,000 magnified image of the salt flakes in the LF-3 sample obtained under the above conditions.

[0237] For LF-1 to LF-6, in subsequent experiments not reported in the previous tables, 0.5 ml of liquid stock solution was applied as a single dose near the center of the cylinder length to promote uniform distribution of the liquid in the nip along the length.

[0238] In the LF-7, the configuration is similar to that described for the LF-1, but instead of a solution feed, the liquid feedstock is fed as a dispersion. The feedstock is prepared by dispersing the salt in a liquid in which it is insoluble. Fine salt with an average diameter of approximately 50 μm was dispersed in 100 ml of isopropyl alcohol at a concentration of 3 g. Experimental results show that after 10 nip passes, the sodium chloride flakes had an average thickness t of approximately 3 μm, an average longest planar dimension L of approximately 400 μm, and an aspect ratio ASP of approximately 133. This thickness is comparable to that of the LF-1, but the flakes' planar dimensions (and aspect ratio) are larger. Notably, because isopropyl alcohol is more volatile than water, salt flakes were obtained more quickly from the isopropyl alcohol dispersion than from an aqueous solution, especially at room temperature, where the experiments were conducted. Figure 12A and 12B The following are pictures of the salt taken at X100 magnification, showing the state of the salt in the form of particles before dispersion in a liquid that is not suitable for its dissolution, and the flakes obtained under the above-mentioned LF-7 conditions.

[0239] For LF-8 to LF-10, the configuration was similar to that described for LF-1, but the cylinder was rotated at 120 rpm instead of 60 rpm at room temperature.

[0240] In the LF-8, a nearly saturated solution of the water-soluble material is prepared by dissolving sodium bicarbonate (NaHCO3) in water at a mass ratio of 1:10. Experimental results show that after 40 roller presses, the sodium bicarbonate, which was originally spherical and had an average diameter of approximately 70 μm, becomes a sheet with an average thickness t of approximately 1.5 μm, an average longest planar dimension L of approximately 40 μm, and an aspect ratio ASP of approximately 27.

[0241] In LF-9, a nearly saturated water-soluble material solution was prepared by dissolving sodium dihydrogen phosphate (Na2HPO1) in water at a mass ratio of 1:10. Testing showed that after 10 tableting cycles, the sodium dihydrogen phosphate, which was spherical and had an average diameter of approximately 200 μm before dissolution, produced tablets with an average thickness t of approximately 4 μm, an average longest planar dimension L of approximately 60 μm, and an aspect ratio ASP of approximately 15.

[0242] In LF-10, the mother liquor of the water-soluble material is prepared by dissolving disodium hydrogen phosphate (NaH2PO4) in water at a mass ratio of 1:14. Experimental results show that after 10 extrusions, the sodium hydrogen phosphate, which was spherical and had an average diameter of approximately 400 μm before dissolution, produces flakes with an average thickness t of approximately 6 μm, an average longest planar dimension L of approximately 150 μm, and an aspect ratio ASP of approximately 25. Figure 13A and 13B They are respectively an X100 magnified photograph of the sodium phosphate particles in a dispersed state before entering the device, and a photograph of the flakes prepared under the above LF-10 conditions.

[0243] In LF-11, the cylinder is made of zirconium oxide (Vickers hardness 1300HV, average surface roughness R a The zirconia cylinders were made of stainless steel (approximately 250 nm), with a diameter of 6 cm (rather than 30 cm) and an axial length of 6 cm. A liquid slurry made from an ultrafine salt solution prepared according to the method described in LF-1 was applied to the cylinders while rotating at 300 rpm at room temperature. A calculated Hertzian contact pressure of 350 MPa was applied by a suitably configured compression mechanism (in this case, a pneumatic piston) to bring the zirconia cylinders into contact with each other. After 150 passes through the nip, the resulting sheet had an average thickness t of approximately 5 μm, an average longest planar dimension L of approximately 400 μm, and an aspect ratio ASP of approximately 80.

[0244] In the LF-12, the cylinders are made of zirconium dioxide, each with an 11 cm diameter and an axial length of 25 cm. A liquid feedstock consisting of a 25 wt.% potassium chloride (KCl) aqueous solution with an initial particle size of approximately 500 μm is applied to a cylinder heated to 70°C and rotating at 100 rpm. A suitably configured pneumatic compression mechanism presses the zirconium dioxide cylinder into contact with a calculated Hertzian contact pressure of 225 MPa. After 35 roller rolls, the resulting sheet has an average thickness, t, of approximately 25 μm, an average longest planar dimension, L, of approximately 450 μm, and an aspect ratio, ASP, of approximately 18.

[0245] LF-13 salt flakes are produced in a similar apparatus to LF-12, except that the cylinder rotates at 250 rpm at 65°C. Furthermore, unlike LF-1 to LF-12, the liquid feedstock is no longer applied as a single 0.5 ml dose at a single point in the center of the nip. Instead, it is applied in larger doses at multiple points to promote uniform distribution of the liquid feedstock within the nip. In LF-13, a 25 wt.% aqueous sodium chloride solution with an initial particle size of approximately 500 μm is applied simultaneously at three locations along the nip, with approximately 1.2 ml applied to each location. After 40 nip cycles, the resulting flakes have an average thickness, t, of approximately 25 μm, an average longest planar dimension, L, of approximately 800 μm, and an aspect ratio, ASP, of approximately 32.

[0246] The materials and conditions for the preparation of LF-14 to LF-18 (involving the flake processing of water-insoluble materials, whether in dispersed or dissolved state) and the flakes obtained therefrom are summarized in Table 3B, where Mg Ste. represents magnesium stearate. For all samples, the roller configuration was as follows Figure 4 As shown, two stainless steel cylinders, each 30 cm in diameter and 25 cm in axial length, rotated at 60 rpm. The liquid feedstock and the surface were both at room temperature. Furthermore, because the hydraulic piston pressure applied to each sample in this series was 370 MPa, this information is omitted from the following tables. In all cases, a single 0.5 ml dose of liquid sample was applied to the center of the nip.

[0247] Table 3B

[0248]

[0249]

[0250] LF-14 through LF-17 represent dispersion systems in which the water-insoluble material is insoluble in water at the added concentration, while LF-18 utilizes a non-aqueous solvent (i.e., acetone) to dissolve the near-infrared dye. The flake sizes obtained in this series of experiments suggest that flakes are typically formed by compaction of solid particles by circulating through rollers in the current process. Furthermore, given the planar dimensions of the flakes, it is expected that particle agglomeration is also occurring. This hypothesis was confirmed using liquid solutions containing even smaller dispersed particles, where flakes formed that, in some cases, exceeded the size of individual particles, and certainly exceeded the size of individual compacted particles, under appropriate operating conditions. For example, ZnO particles with an initial diameter of approximately 0.5 μm (i.e., one-tenth the original particle size), formed flakes greater than 2 μm in thickness.

[0251] Figure 14A and 14B The pictures are of calcium carbonate at X1,000 and X100 magnifications, respectively. The former shows the state of the particles before being dispersed and fed into the device, and the latter shows the flakes obtained under the above LF-14 conditions.

[0252] Figure 15A and 15B The following are photos of particles (before dissolution) taken with near-infrared dye NIR983A at X1,000 magnification and photos of flakes prepared under the above LF-18 conditions.

[0253] Example 4: Improvement of tablet dissolution rate

[0254] In this example, the dissolution rate of flakes prepared according to Example 3 in water was tested at room temperature and compared to the dissolution rate of various types of unflaked reference materials. Unless otherwise noted, all experiments in this and subsequent examples were conducted on flakes that were actively peeled from the surface of a rotating cylinder using an appropriately guided scraper.

[0255] The dissolution rate of salt flakes was determined by measuring the conductivity of the solution after dissolving different salt components in water. Salt dissolution changes the ionic conductivity of the solution. A 40 mg sample of salt was dried at 120°C for at least two hours and then stored in a desiccator at room temperature. The sample was then added to 80 ml of double-distilled water at room temperature and mixed with stirring at 400 rpm. Conductivity was measured using a Keithley 2750 multimeter. An alternating voltage was applied through electrodes immersed in the solution sample, and the resulting current was measured. The conductivity (i.e., the measured current) increased with salt dissolution until it reached a plateau value. The time from salt addition to the current reaching the plateau value was recorded. Each conductivity measurement was repeated at least three times, and the time (in seconds) required for the current to stabilize at the plateau value after dissolution is reported in Table 4 as the average of all replicates.

[0256] Table 4

[0257]

[0258] Dissolution rates were also assessed qualitatively: a sample of known mass was placed on a glass slide, and a known volume of solvent was added at a distance from it—enough to dissolve the solid by capillary action after the operator formed a liquid bridge. The results were then observed under a confocal microscope at x228 magnification. For each material, two samples were tested: first, the uncomminuted original material, and then a comminuted version of the same material. The observations were repeated for all samples. This method revealed that sodium phosphate and sodium hydrogen phosphate dissolved significantly faster in water when the materials were comminuted as described in LF-10 and LF-9.

[0259] Example 5: Density of Taste Agents

[0260] In this example, the bulk density and tap density of the sodium chloride or potassium chloride taste agent flake samples prepared according to Example 3 were compared with the unflaked standard powder used to prepare the standard powder.

[0261] The flake samples of sodium chloride and potassium chloride were prepared according to the methods described in LF-11 and LF-12, respectively. The bulk density of each sample is B Fill to a known volume V by weighing a pre-dried sample B The mass of the container is then measured (measured with a fine graduated cylinder). The container is then tapped repeatedly until the volume no longer shrinks, and the final constant value is used to estimate the tapping volume V T , and then calculate the tapping density ρ T Typically, the tapping lasted no longer than one minute, with a frequency of two taps per second. Flakes were collected from two sources: first, flakes that spontaneously detached from the surface of the rotating cylinder, and second, flakes that were actively peeled off by placing a blade on the surface of the rotating cylinder in the direction of the peeling. The results are shown in Table 5, where spontaneously detached flakes are marked with a superscript S and actively peeled flakes are marked with a superscript A. Additional information and factors for the relevant calculations are also presented in the table.

[0262] Table 5

[0263]

[0264]

[0265] As shown in the table above, the bulk density of the sheet sample prepared by the present invention is B and tap density ρ T are lower than the corresponding reference (unflaked) material values. In addition, the F2 ratio (F2 = ρ T / ρ B) is greater than the same ratio of its corresponding reference material, which indicates that the flake samples have better stacking properties.

[0266] Taking into account the aspect ratios of the flake sample and the particle source, the factors calculated based on the above measurements lead to a greater difference between the flakes prepared by the present invention and their source materials. For example, the F3 ratio of the flake sample (F3 = ASP / ρ B ) at least 60cm 3 / g, while the values ​​for particle sources are between 0.85 and 1.25 cm 3 / g; F4 ratio of the flake sample (F4=ASP / ρ T ) at least 40cm 3 / g, while the values ​​for particle sources range from 0.74 to 0.79 cm 3 / g.

[0267] Example 6: Crystallographic Analysis of Crystallizing Reagents

[0268] The crystal structure of the salt flakes prepared by tableting was analyzed by X-ray powder diffraction (XRPD). The data were obtained using a Panalytical Empyrean III multifunctional diffractometer (K α radiation, ) were acquired in 1D line detector mode with X-ray tube parameters of v = 45 kV, I = 40 mA. Each sample was directly mounted in a stainless steel ring sample holder and fixed with backing filler. During the measurement, the sample was rotated at a speed of 8 rpm, and the measurement range was 5-140° 2θ. Phase identification and size-strain analysis were performed by Reitveld refinement using the HighScore Plus powder diffraction data analysis software package (version 5.1) in combination with the ICDD (International Center for Diffraction Data) Powder Diffraction File (PDF-4+) database (2022 edition).

[0269] Sample 1 is made of standard table salt particles with an average particle size of about 500 μm (used to prepare ultrafine salt after grinding), sample 2 is made of ultrafine salt particles with an average particle size of about 50 μm (used to prepare LF-1 wafers after dissolution), and sample 3 is made of LF-1 salt wafers prepared in Example 3.

[0270] The diffraction peaks obtained for the analyzed samples were relatively similar in position and included known characteristic peaks for sodium chloride, such as those detected at approximately 31.7°, 45.4°, 66.2°, and 75.3°, to name a few. The diffraction peaks for the flake samples were slightly broader than those for the reference granular samples. Phase analysis indicated that the NaCl content in all samples exceeded 99.5 wt.%. The microstrain values ​​(expressed as percentages) and grain sizes for each sample are shown in Table 6.

[0271] Table 6

[0272]

[0273]

[0274] As shown in the table above, the grain size of the flakes prepared using this method is approximately 1 / 4 of the original material, and the microstrain value is at least 3 times that of the original material. Similar results were observed for other salt flake samples prepared using the method of this invention, that is, the grain size is smaller than the original material. To clarify whether these significant changes are due to the flake morphology of the prepared material or the preparation method, a commercial salt flake sample produced by Cargill was tested. A similar analysis was performed on conventionally prepared salt flakes sold under the trademark Fine Flake Salt. The crystal size of this control sample was The microstrain, 0.017%, is closer to the results of Pellet 1 than to those of Pellet 3. Therefore, the values ​​monitored in freshly prepared flake samples using this method are believed to arise from repeated compaction during the manufacturing process, rather than simply from the material's flake morphology. Therefore, when flakes made from crystalline materials exhibit smaller grain sizes and / or larger microstrain values ​​than conventionally prepared flakes of the same material, crystallographic analysis indicates that these flakes were produced using this method. This identification is easier to make when the flakes have not been exposed to environmental conditions that could be detrimental to the crystal structure. For example, if the material is hygroscopic, such as salt, exposure to humidity could affect the flakes. Therefore, it is recommended that such analyses be performed on freshly prepared flakes or those that have been properly stored to avoid affecting the crystal behavior.

[0275] Example 7: Tablets prepared from mixed materials containing taste substances

[0276] The tablets can be prepared from a liquid raw material comprising two or more materials, for example, two or more taste substances can be mixed. The following mixtures were prepared according to the steps of Example 3 with the following modifications, and some of the results are summarized in Table 7.

[0277] In the first series of experiments, the materials used to form the flakes were individually provided taste substances. The first taste substance was table salt with a particle size of about 500 μm, dissolved in water at a mass ratio of 1:3 (i.e., 25 wt.%). 34 g of this NaCl solution was blended with 16 g of fresh red pepper in a Ninja blender (model Nutri-Blender Plus BN303) at 700 watts for about 20 seconds until a milkshake-like mixture was obtained. The mixture was filtered through a cloth to separate the pulp. The resulting brown liquid mother liquor was then Figure 4As shown, the liquid was fed into a clamping device consisting of two identical stainless steel cylinders. Each cylinder was mounted with a zirconia sleeve, both with an 11 cm diameter and a 20 cm axial length. The cylinders were heated to 65°C and rotated at 250 rpm, while a pneumatic piston applied a calculated Hertzian contact pressure of 365 MPa to press the cylinders together. 1.5 ml of a liquid containing salt and chili extract was added simultaneously at two locations on the rollers, with 0.75 ml added each time. After 45 passes through the rollers, flakes containing the salt and fresh chili flavor mixture were collected by gravity, with the flakes falling off the rollers over time. This experiment and the resulting flakes, designated LF-19, were evaluated by detailed microscopic analysis of 20-30 individual particles. The conditions and results of preparing flakes of mixed materials (e.g., flavored or colored salt) using the liquid flake method described above are summarized in Table 7, although the roller configuration and operating parameters are not repeated.

[0278] Table 7

[0279]

[0280] As shown in the figure, all prepared flakes achieved an aspect ratio of at least 55. In addition to evaluating their size, they were also tested for flavor and / or color. The LF-19 and LF-20 flakes exhibited a spicy flavor in addition to a salty base. The LF-19 flakes were slightly brown, the LF-20 flakes were light red, and the LF-21 flakes were a deeper red, with no noticeable difference in taste.

[0281] In a second set of experiments, the materials used in the tablets prepared according to the teachings of the present invention were detergents supplied as a mixture. As is known, powdered detergents used for laundry can cause problems if they do not dissolve adequately during the washing process. For example, they can leave behind solid residues that can cause white stains on clothing and / or accumulate in washing machine drains, especially when using cold or hard water. Washing powders typically contain a complex mixture of surfactants (nonionic, anionic, and / or cationic) to remove stains, chelating agents (e.g., to stabilize other ingredients, ensure the detergent is effective under a wide range of conditions, remove odors, etc.), polymers (e.g., to prevent stains from reattaching to already cleaned clothing), builders (e.g., to soften water, buffer pH, promote the emulsification of oily stains, etc.), bleach, oxidants, fabric softeners, pH buffers, enzymes, solvents, pigments, and fragrances, some of which are less water-soluble under certain conditions.

[0282] A commercially available laundry detergent (Ariel, manufactured by Procter & Gamble) with relatively coarse detergent particles, with an average initial diameter of about 500 μm, was suspended in water at a weight ratio of 1:9 (i.e., 10 wt.%). Figure 4 The sandwich shown here consists of two stainless steel cylinders with a diameter of 30 cm and an axial length of 25 cm. The cylinders rotate at 120 rpm and are pressed against each other by a hydraulic piston, applying a calculated Hertzian contact pressure of 370 MPa without heating. After a single application of 1 ml of liquid raw material in the center of the nip, the cylinders are passed through the nip 40 times, and a flake containing the detergent mixture is peeled from the cylinder surface using a suitable scraper. This experiment and the resulting flakes, designated LF-22, were evaluated by microscopic analysis of 20-30 individual particles. The average thickness t of the detergent flakes was approximately 10 μm, and the longest planar dimension L averaged approximately 600 μm, resulting in a calculated aspect ratio of approximately 60.

[0283] In an additional experiment, the "coarse" detergent particles were briefly ground in a coffee grinder to produce fine granules with an average particle size of approximately 50 μm. These fine granules were suspended in water at a 1:1 mass ratio (i.e., 50 wt.%), with all other process parameters consistent with the LF-22 experiment. This experiment and the resulting flakes, designated LF-23, exhibited similar dimensions to those previously measured for LF-22 flakes.

[0284] The dissolution rate of LF-22 and LF-23 detergent tablets in water (relative to directly or indirectly prepared detergent coarse granular powders), measured as the dissolution rate (DT) in seconds, was evaluated according to the method detailed in Example 4. 110 mg of sample (LF-22 or LF-23 tablets, or original coarse granules) was added to 80 ml of water and dissolved under stirring at 970 rpm. While the reference powder required 13.27 seconds to dissolve, the prepared tablets achieved similar solubility in only 1.34 seconds and 1.49 seconds, respectively, dissolving approximately 10 times faster than the reference powder.

[0285] The bulk density and tap density of LF-22 detergent tablets were compared with the corresponding densities of the detergent coarse powder from which they were prepared. B and ρ T The unit is grams per cubic centimeter as measured by the method described in detail in Example 5. The bulk density is 0.80 g / cm 3 Down to 0.40g / cm2 for flakes 3 , while the bulk density increased from 0.93 g / cm 3 Down to 0.64g / cm2 for LF-22 flakes 3 .

[0286] Factors calculated based on these measurements lead to greater differences between the sheets prepared according to the present invention and their reference materials. For example, the sheets of the present invention exhibited an F1 ratio (F1 = ASP / DT) of approximately 44.78 sec. -1 , while the value of the detergent particles is 0.08sec -1 ; F2 ratio (F2 = ρ T / ρ B ) is about 1.60, while the value of the detergent granules is 1.16, which indicates that it has better stacking ability; F3 ratio (F3 = ASP / ρ B ) is 150cm 3 / g, while the original detergent is 1.25cm 3 / g, and F4 ratio (F4=ASP / ρ T ) is 93.75cm 3 / g, while the original detergent is about 1.08cm 3 / g.

[0287] These results further support that materials other than deodorants, as well as mixtures and pure compounds, may benefit from the present invention. In the case of detergents, the significant increase in the dissolution rate of the active ingredient (approximately 10 times the original) is expected to improve its efficacy in finished products (such as laundry detergents) that contain or consist of the same active ingredient. This increase in efficacy may alternatively or additionally allow the amount of active ingredient used in the finished product to be reduced while maintaining similar efficacy to similar products containing the same active ingredient but in a different (e.g., traditional) form.

[0288] Example 8: Effects of various parameters on process and sheet

[0289] As previously mentioned, various operating parameters can be modified according to the methods of the present invention. These variables primarily relate to the volume of material entering the nip (e.g., application volume, number of application points along the rotating cylinder, application frequency, concentration of material per dose, properties of the dissolved / dispersed liquid, etc.) and the operating conditions of the adapting equipment (e.g., area (axial length and diameter) of the rotating cylinder, cylinder speed and temperature, nip length, nip pressure, etc.). This example investigates the effects of these exemplary parameters.

[0290] Unless otherwise stated in the following tables, each experiment was conducted by repeatedly applying a single dose (1 ml) of a liquid stock solution containing 25 wt.% common salt (initial particle size of about 500 μm) dissolved in water every few seconds (e.g., less than once per minute). Each dose was applied to the center of the nip of the rollers (e.g., Figure 4As shown, once the previously applied liquid dose is converted into a sheet that can fall off the surface of the rotating cylinder, its surface becomes available again for the application of a fresh dose to form a new sheet. The interval between each subsequent dose application was recorded in each experiment because it is affected by operating conditions (e.g., drum temperature, size and speed, the volume and material concentration of each dose, ambient humidity, etc.). These observed intervals are then used to calculate the number of doses applied per hour. For example, if the interval between two coatings in a certain experiment is 10 seconds, the coating frequency can be expressed as 360 times / hour.

[0291] The embossing was formed between two identical stainless steel cylinders, each fitted with a zirconia sleeve. The cylinders, including the sleeves, had a diameter of 11 cm and an axial length of 20 cm. The parameters tested included the temperature of the cylinders (25°C, 45°C, 60°C, 75°C and 90°C), their rotation speed (100 rpm, 200 rpm, 250 rpm, 300 rpm and 400 rpm), the calculated Hertzian contact pressure, i.e. the pressure at which the cylinders are pressed into contact (110 MPa, 182 MPa, 258 MPa, 365 MPa and 447 MPa) using a pneumatic piston, the applied volume (0.6 ml, 1 ml, 1.8 ml, 3 ml, 6 ml, 9 ml and 10 ml), the number of points applied along the embossing point (1 and 3), and the final salt concentration in the water (25 wt.% and 59 wt.%). The experiment is terminated 10 minutes after the first dose is applied and the flakes collected at the different settings are weighed to assess productivity or analyzed by any suitable method for their average size or other characteristics of interest (e.g., their moisture content, if any).

[0292] Details of each experiment, including modifications from the master setup and frequency of dose application, and example results are summarized in Tables 8A to 8D below.

[0293] Table 8A - Effect of Temperature

[0294]

[0295] As shown in the table above, the data are derived from a series of experiments in which a single 1 ml dose was applied in each experiment. The tablet yield was improved by increasing the temperature of the rotating cylinder (when required, the temperature was raised to the temperature indicated in the table by an internal electric heating element), as expected, because the evaporation of water from the applied liquid is accelerated, thereby increasing the frequency of the dose applied to the nip of the rotating cylinder.

[0296] Under the conditions of the present study, the temperature did not appear to have a significant effect on the size of the resulting flakes within the higher range. All flakes obtained at elevated temperatures had relatively similar average thicknesses, t, of approximately 25 μm, average longest planar dimension, L, of approximately 1,200 μm, and aspect ratios, ASP, of approximately 48. Flakes obtained at room temperature were thinner and smaller than those obtained at elevated temperatures (t ~10 μm, L ~500 μm), but aspect ratios were similar at all temperatures. Similar behavior was observed with increasing production rate and dosage application frequency as the extrusion point temperature increased at additional rotational speeds of 100 rpm, 300 rpm, and 400 rpm.

[0297] Similar experiments were conducted after preheating the mother liquor to a temperature similar to that of the rotating drum (above ambient temperature). Under the conditions of the current study, preheating the liquid to match the drum surface temperature did not appear to significantly affect the final yield or flake size.

[0298] Table 8B - Effect of Speed

[0299]

[0300] As shown in the table above, data collected through a series of experiments (each applying a single dose of 1 ml) indicate that increasing the rotational speed of the cylinder increases the tablet output, which is consistent with expectations because the number of times the applied liquid feedstock passes through the nip increases in the same amount of time. In addition, the rotational speed itself promotes evaporation, accelerating the removal of liquid from the applied dose, allowing subsequent doses to be applied at a higher frequency. The production rate tends to stabilize at higher rotational speeds. Under the conditions of the current study, when the rotational speed is increased from 100 rpm to 400 rpm, the rotational speed does not appear to have a significant effect on the size of the tablets. The average thickness t of all the resulting tablets is approximately 25 μm, the average longest planar dimension L is approximately 1,200 μm, and the aspect ratio ASP is approximately 48. Similar behavior of increasing productivity with increasing drum speed was observed at additional temperatures of 45°C, 75°C, and 90°C.

[0301] For comparison, an experiment, termed LF-LS, was conducted in a similar nip at a lower speed of 3 rpm, with the roll heated to 90°C and the same applied pressure of 365 MPa. Although the production rate of 60 g / h was comparable to that achieved at approximately 150 rpm and 60°C, the drastic reduction in speed significantly affected the dimensions of the resulting flakes. The LF-LS flakes were approximately five times the volume (L ~ 6,400 μm) and eight times the thickness (t ~ 195 μm) of those produced at higher speeds (100-400 rpm), with a corresponding decrease in aspect ratio from 48 at high speed to 33 at lower speeds. Without being bound by any particular theory, it is believed that the lower speed reduces the number of passes through the nip within a predetermined timeframe (e.g., 10 minutes in this experiment), thereby reducing the contact time between the liquid feedstock, and the resulting films and coatings, and the compact environment of the nip. Furthermore, it is hypothesized that the higher speed increases the relative velocity between the roll outer surface and the surrounding air, thereby facilitating the rapid entrainment of the liquid vapor during its formation.

[0302] Table 8C - Contact Pressure Effect

[0303]

[0304] As shown in the table above, as the calculated Hertzian contact pressure at the nip increases, the frequency of dosing repetitions and the sheet production rate both show a nonlinear growth trend, and both tend to plateau at higher pressures. Notably, before the plateau, the nip pressure also affects the sheet thickness and its longest planar dimension, while its aspect ratio remains relatively stable.

[0305] Although not shown in the above table, it has been demonstrated that increasing the drum surface area by using rollers with larger diameters can relatively increase the production rate and application frequency while keeping other parameters constant (except the achievable sheet size).

[0306] Table 8D - Effect of Dose Size

[0307]

[0308] As shown in the table above, increasing the volume of liquid feedstock applied to the nip per application reduces the frequency of reapplication and increases the sheet production rate in a nonlinear manner, with the production rate tending to plateau at higher doses. The optimal volume of a single dose is expected to depend on factors including, but not limited to, the cylinder size (which determines the nip length and the surface area that can be covered by the liquid film), cylinder temperature, rotational speed, and the force applied to achieve the desired nip contact pressure. It is worth noting that the volume of the applied dose may also affect the wafer thickness, but has less influence on the longest planar dimension of the wafer, thereby affecting the wafer aspect ratio.

[0309] In similar experiments, the effect of material concentration (in this case, sodium chloride) was evaluated using a 1 ml dose at 90°C, 250 rpm, and 365 MPa. Increasing the salt concentration from 25 wt.% to 59 wt.% simultaneously increased the salt flake production rate from 244 g / h to 566 g / h, with application frequencies of 976 and 959 times / h, respectively. Because the 59 wt.% salt solution is not a solution but rather an overloaded dispersion, the sample solutions in this experiment were prepared using ultrafine sodium chloride ground internally to a particle size of less than 5 μm, rather than the 500 μm particle size used previously, regardless of the final solids concentration. Under the conditions investigated, the initial salt concentration in the liquid feedstock did not appear to significantly affect flake size. All flakes had an average thickness, t, of approximately 18 μm, an average longest planar dimension, L, of approximately 1,400 μm, and an aspect ratio, ASP, of approximately 78. Similar positive correlations between salt concentration and production rate were observed at additional temperatures of 45°C and 75°C.

[0310] In similar experiments conducted at 65°C, 250 rpm, and 365 MPa, the effect of the number of application points along the nip was tested, with the total volume per application remaining constant. When the liquid feedstock was applied at a single (central) point along the embossed area (as in the previous procedure) at a dosage of 1.8 ml, the production rate of salt crystals was 132 g / h. When the same liquid feedstock was applied at three equally spaced application points along the embossed area, with a dosage of 0.6 ml per application point (still a total dosage of 1.8 ml), the rate of salt crystal formation increased to 175 g / h. Under the conditions investigated, the number of application points in the embossed area did not appear to have a significant effect on crystal size. All crystals had an average thickness, t, of approximately 20 μm, an average longest planar dimension, L, of approximately 1,200 μm, and an aspect ratio, ASP, of approximately 60.

[0311] The inventors discovered that the motor torque of the rotating cylinder can be used to predict the appropriate time interval between subsequent dose applications, thereby determining the application frequency. It is believed that after the first dose is applied, the liquid diffused along the gap between the rollers will generate resistance during the rotation of the cylinder, and this resistance gradually decreases as the liquid is eliminated. When the tablet formed by the first dose is ready (for example, when it is relatively dry), the motor of the rotating cylinder exhibits the minimum torque value required to maintain a substantially constant speed. At this stage of the cycle, the tablet can be removed (or fall off on its own) and a new dose is applied upstream of the roller to start the next preparation cycle. Therefore, as time passes and fresh material to be tableted is repeatedly added, the motor torque value shows a sinusoidal curve. This characteristic can be used in a feedback mechanism: the motor torque of the rotating cylinder is monitored, and when the monitored torque reaches a minimum value under operating conditions, a signal is sent to the liquid reservoir dispenser to release a new dose of material.

[0312] In all the experiments described above, productivity, expressed in grams per hour, was assessed by weighing all flakes produced during a 10-minute operating cycle and calculating the expected weight within 60 minutes. The flakes were also sampled to determine their moisture content. To do this, approximately 1 gram of each flake produced under the above conditions was placed in an aluminum crucible, its precise weight was measured, and the crucible was then dried in a 120°C oven for 2 hours to remove any residual moisture. The weight of the dried sample was measured, and its moisture content was calculated. All flakes produced in this example had a moisture content of less than 1 wt.%.

[0313] Example 9: Comparison of the sheet of the present invention with commercial samples

[0314] Flakes prepared according to the present teachings and the preceding examples were compared with commercial samples of the same material, some of which were in granular form and others in "flake" form. All test samples in this example were made from sodium chloride. Four flakes, designated LF-24 through LF-27, were prepared using a liquid feedstock containing 25 wt.% salt (with an initial particle diameter of 500 μm). Their preparation conditions and average measured dimensions are shown in Table 9.

[0315] Table 9

[0316]

[0317] Nine commercially available sodium chloride samples, designated CS-1 through CS-9, were independently sized using the same microscopy method as the flake samples. Table 10 presents the average values ​​of their measured dimensions, with one dimension omitted and marked with a negative sign to indicate samples with an aspect ratio of approximately 1 and a distinctly granular appearance.

[0318] Table 10

[0319]

[0320] As shown in the table above, the aspect ratios of all comparative salt samples (although some of them are commercially sold in the form of "flakes") do not exceed 10, among which the aspect ratio of CS-1 flake salt is the highest at 7.2, and CS-3 Diamond The aspect ratio is 6.9. CS-3Diamond It has a distinct hollow pyramid crystal structure and is claimed to provide a superior sensory experience, rapid solubility, strong adhesion, and a lower bulk density. For reference, the flake samples listed in Table 9 were all prepared using this method, with an aspect ratio of no less than 35.

[0321] LF-24 to LF-27 and CS-1 to CS-9 were subjected to head-to-head comparison tests: a) their dissolution rates DT (in seconds) were determined using the same method as described in detail in Example 4, except that the sample stirring speed was set at 970 rpm instead of 400 rpm; b) their bulk densities ρ B and tap density ρ T (in grams per cubic centimeter), the test method being the same as described in detail in Example 5.

[0322] The results of these comparative studies and the factors calculated therefrom, as described below, are summarized in Table 11.

[0323] Table 11

[0324]

[0325] As shown in the table above, and further confirmed by another series of experiments, the tablets of the present invention exhibit rapid dissolution, with nearly all dissolving within approximately 2 seconds, and most dissolving within 1 second. By comparison, CS-5, used to prepare the tablets of the present invention, dissolved in 8.95 seconds in the same series of experiments (consistent with a previously measured 8.7 seconds). Furthermore, the closest commercially available materials to the tablets of the present invention, CS-1 and CS-3, dissolve in at least 3 seconds. This suggests that the tablets of the present invention may dissolve more rapidly than existing, considered similar products.

[0326] It is worth noting that when calculating the ratio of the sample aspect ratio ASP to the dissolution rate DT (which can be mathematically expressed as F1 = ASP / DT, in seconds - 1 ), the difference between the present invention's sheets and commercially comparable samples was significant. On average, the comparative samples had an F1 factor of approximately 0.76, with CS-1 and CS-3 having the highest values ​​of 1.59 and 2.32, respectively. The average for the present invention's sheets was approximately 60 times greater, with the lowest F1 factor value in the group exceeding 15.

[0327] With respect to the bulk density and tap density of the samples, it can be seen that the flakes prepared according to the present invention generally have a lower density than the commercially available comparative samples. The tap density ρ of each sample was calculated by T and volume density ρ B The dimensionless ratio F2 between the two groups can further highlight the difference between the two groups. This ratio can be mathematically expressed as F2 = ρ T / ρ BWhile the bulk density of the control samples was, on average, approximately 20% higher than their bulk density (i.e., F2-1.19), the difference between the two densities increased to 96% when the sheets prepared according to the present invention were considered (i.e., F2-1.96). This suggests that the sheets prepared according to the present invention may have better bulking properties than existing products, which may facilitate their packaging, storage, and transportation, and therefore have commercial advantages.

[0328] It is worth noting that when calculating the aspect ratio ASP and volume density ρ of the sample B The ratio F3 (mathematically expressed as F3 = ASP / ρ B When the weight of the tablets prepared according to the present invention is measured in grams per cubic centimeter, the difference between the tablets prepared according to the present invention and the commercially available comparative samples is significant. On average, the comparative samples have an F3 factor of approximately 4.61, with the highest values ​​of 16.7 and 11.8 for CS-1 and CS-3, respectively. The tablets prepared according to the present invention exhibit an average F3 factor exceeding 40 times that of the comparative samples, with the lowest F3 factor in the group exceeding 90.

[0329] When calculating the sample aspect ratio ASP and volume density ρ T Similar results are observed when the ratio F4 is used, which can be expressed by F4 = ASP / ρ T (Units are cubic centimeters per gram) mathematically expressed. While the average F4 factor of the comparative samples was approximately 3.96, with CS-1 and CS-3 having the highest values ​​of 14.18 and 10.58, respectively, the flakes prepared by the method of the present invention exhibited an average F4 factor approximately 25 times that, with the lowest F4 factor in the group exceeding 60.

[0330] In summary, the comparisons conducted in this example demonstrate that the sheets prepared according to the present invention differ significantly from existing products that are considered equivalent. Distinguishing characteristics of the sheets of the present invention can be reflected in directly measurable values, such as a relatively thin sheet and / or a relatively large longest dimension, and / or in parameters derived from these measurements, such as a relatively higher calculated aspect ratio between characteristic dimensions compared to a standard sheet. These distinguishing characteristics and the range of possible values ​​for each measurement parameter have been discussed previously and will not be repeated here.

[0331] The calculable parameters used to highlight the unique characteristics of the tablets of the present invention include factors F1 through F4. While the constraints described below may be used to characterize these factors in certain circumstances, these constraints are primarily based on tablets made from salt. However, as illustrated by the detergent described in Example 7, the following lower limits, upper limits, and / or ranges therebetween are not limited to this specific material.

[0332] In some cases, the ratio F1 of the aspect ratio ASP of the tablet to the dissolution rate DT of the tablet in the present invention, expressed as F1 = ASP / DT, is 5 or greater, 10 or greater, 15 or greater, 25 or greater, 50 or greater, 75 or greater, or 100 or greater. In certain embodiments, F1 is equal to or less than 500, less than 400, less than 300, less than 200, or less than 150. In particular cases, F1 is between 5 and 500, between 10 and 300, or between 10 and 150.

[0333] In some cases, the bulk density of the flakes in the invention is T and volume density ρ B The ratio F2 between them is expressed as F2 = ρ T / ρ B , is 1.25 or greater, 1.50 or greater, 1.75 or greater, 2.00 or greater, 2.25 or greater, 2.50 or greater, or 2.75 or greater. In certain embodiments, F2 is equal to or less than 5.0, less than 4.5, less than 4.0, or less than 3.5. In particular instances, F2 is between 1.25 and 5.0, between 1.35 and 4.0, between 1.45 and 3.5, or between 1.55 and 3.0.

[0334] In some cases, the aspect ratio ASP of the sheet material of the invention is equal to its bulk density ρ B The ratio F3 is expressed mathematically as F3 = ASP / ρ B , is 25 or greater, 50 or greater, 75 or greater, 100 or greater, 150 or greater, 200 or greater, 250 or greater, 300 or greater, or 350 or greater. In certain embodiments, F3 is equal to or less than 1,000, less than 750, less than 500, or less than 400. In particular instances, F3 is between 25 and 1,000, between 50 and 750, between 75 and 500, or between 100 and 400.

[0335] In some cases, the aspect ratio ASP of the sheet material of the invention is equal to its bulk density ρ T The ratio F4 between them is mathematically expressed as F4=ASP / ρ T In some cases, F4 is 20 or more, 40 or more, 60 or more, 80 or more, 100 or more, 120 or more, 140 or more, 160 or more, or 180 or more. In certain embodiments, F4 is equal to or less than 500, less than 400, less than 300, or less than 200. In particular cases, F4 is between 20 and 500, between 40 and 400, between 60 and 300, or between 80 and 200.

[0336] Figures 16A to 16EThis is a picture of commercially available salt prepared according to the prior art at a magnification of X100, wherein the aspect ratio of the salt is at least 2, and the picture was taken by SEM-FIB microscopy, consistent with the method previously described for the flakes of the present invention. Figure 16A The flakes showing CS-1 (Asp~7.2) Figure 16B Diamond of CS-3 (Asp~6.9) is shown hollow particles, Figure 16C The top plate crystals of CS-4 (Asp ~ 2.4) are shown. Figure 16D The coarse plate-like crystals of CS-6 (Asp ~ 2.7) are shown. Figure 16E Fine plate-like crystals of CS-7 (Asp ~ 2.4) are shown. Figure 16F LF-26 flakes (Asp-53) are shown nearby for comparison. As shown, while most of the particles in the comparative sample are commercialized as flakes by the supplier, their observed shape is closer to flat blocks than flakes, as evidenced by their relatively low aspect ratios (ranging from 2.4 to 7.2). As shown in the figure, the higher aspect ratio of the flakes of the present invention gives them a unique shape, and their planar surfaces appear smoother than the corresponding edges of the comparative sample at the same magnification.

[0337] Example 10: Compressibility of flaky particles

[0338] The flaky particles prepared according to the present invention were compared with commercial samples of the same material (as shown in Example 9), and it was found that the density (ρ T and / or ρ B ) is usually lower than the commercial comparison sample, and / or its apparent density ρ T and bulk density ρ B The dimensionless ratio F2 between the two is higher. This suggests that the tablets of the present invention may have better stacking properties than existing products. The purpose of this example is to verify the above findings by evaluating the compressibility of the tablets and their ability to recover to their original bulk density after compression.

[0339] Tablets designated LF-28 were prepared according to the present invention by continuously adding a 25 wt.% sodium chloride liquid feedstock in 1.5 ml increments into an extrusion gap formed by two cylinders with an 11 cm diameter and 20 cm axial length, each with a zirconia outer surface. The cylinders were heated to 65°C, rotated at 250 rpm, and pressed into contact under a pressure of 365 MPa generated by a pneumatic piston. The resulting tablets had an average thickness, t, of approximately 16 μm, an average longest planar dimension, L, of approximately 1,100 μm, and an aspect ratio, ASP, of approximately 69. These tablets were tested and compared with previously described commercial samples.

[0340] First, weigh a syringe with a 50 ml injection volume and then gently fill it with the material to be tested until the volume reaches 50 ml. Weigh the filled syringe to determine the initial density of the sample and calculate its bulk density ρ B (Units are grams per cubic centimeter). The piston is then pressed until the test material can no longer be compressed. The volume of the compressed material is measured and used to calculate the compressed density ρ of the sample. C The samples were placed in a compressed state for approximately 18 hours, after which the piston was removed, the samples were taken out of the syringe barrel and returned to an uncompressed state. The unconstrained samples were gently re-filled into their respective syringes to check whether they had recovered their original volume of 50 ml or if the volume had changed after decompression due to modification. The decompressed density ρ was calculated based on the volume recovered by the sample after overnight compression. DC .

[0341] By calculating the compression density ρ of each sample C and the initial volume density ρ B The dimensionless ratio F5 between them (mathematically expressed as F5 = ρ C / ρ B ), to assess the degree of compressibility that the sample may exhibit. The calculation results and related factors are summarized in Table 12.

[0342] Table 12

[0343]

[0344] As shown in the table above, although the average compressed density of the comparative samples is about 30% higher than their bulk density (i.e., F5 ~ 1.29), when the sheet samples prepared according to the method of the present invention are considered, the difference between the two densities increases dramatically, reaching 3 times (i.e., F5 ~ 3.33). All commercial samples return to their original shape after decompression, and their density after decompression is ρ DC and the initial volume density ρ B The density of the sheet sample after decompression is slightly higher than its original bulk density.

[0345] Without being bound by any particular theory, it is believed that the sheet material of the present invention may have partially broken down during the experimental compression process because the aspect ratio of the sheet material of the present invention (ASP ~ 68) is at least an order of magnitude higher than the average aspect ratio of the compared materials (ASP ~ 3.4, with a peak of about ~ 7 for CS-1 and CS-3). However, even after breaking up, the sheet material still maintains a relatively low decompressed density ρ DC About 0.4g / cm 3 , while the average value of the comparative samples is about 0.8g / cm 3Because a material's brittleness (i.e., its tendency to deform under compression) depends in part on its initial aspect ratio, a dimensionless factor, F6, was calculated to establish a relationship between a material's initial aspect ratio, ASP, and its compressibility, estimated by F5. F6 can be expressed mathematically as F6 = ASP / F5, and was found to highlight the differences between the current sheet material and the comparative sample.

[0346] This example demonstrates that the current sheet material with excellent F2, F5 and F6 values ​​has better stacking ability than existing products, which is expected to simplify its packaging, storage and transportation.

[0347] Furthermore, this example provides additional parameters, F5 and F6, that can be calculated to emphasize the unique characteristics of the flake material studied. While the following limitations may apply to these parameters in certain circumstances, these limitations are based on salt-based flake materials. However, the following lower and upper limits, as well as the ranges, are not limited to this specific material.

[0348] In some cases, the compressed density of the sheet material of the present invention is C and the initial volume density ρ B The ratio F5, the mathematical expression is F5=ρ C / ρ B , having a value of 1.6 or greater, 1.8 or greater, 2.0 or greater, 2.2 or greater, 2.4 or greater, 2.6 or greater, 2.8 or greater, 3.0 or greater, or 3.2 or greater. In certain embodiments, F5 is equal to or less than 10.0, less than 7.5, less than 5.0, or less than 4.0. In particular instances, F5 is between 1.6 and 10.0, between 1.8 and 7.5, between 2.0 and 5.0, between 2.2 and 4.5, or between 2.4 and 4.0.

[0349] In some cases, the ratio of the aspect ratio ASP of the sheet material of the present invention to its compressibility as estimated by F5, mathematically expressed as F6 = ASP / F5, is 6 or greater, 10 or greater, 15 or greater, 20 or greater, 25 or greater, 30 or greater, 35 or greater, or 40 or greater. In certain embodiments, F6 is equal to or less than 200, less than 150, less than 100, less than 75, or less than 50. In particular cases, F6 is between 6 and 200, between 10 and 150, between 20 and 100, between 20 and 75, or between 20 and 50.

[0350] Example 11: Sensory testing of taste tablets

[0351] The effect of the form of a taste substance on the corresponding perceived taste can be tested using human volunteers. The taste substance can be tested directly before and after the tablet treatment described in the present invention, or it can be applied to or mixed into a food that does not contain the taste substance and tested. For example, the taste substance can be applied to the surface of popcorn or mixed into a relatively tasteless edible gel. The same ratio of the reference taste substance or the tablet taste substance is applied to or mixed into the food to determine how much stronger the taste intensity provided by the taste substance tablet is compared to the reference taste substance. Conversely, once the content of the reference taste agent is set to provide a satisfactory taste, food samples with gradually reduced amounts of the taste agent tablet can be prepared until a similar satisfactory taste is achieved. Through this method, it can be determined how much the amount of taste agent can be reduced when using the tablet taste agent instead of the standard reference taste agent.

[0352] This study evaluated the ability of sodium chloride tablets prepared according to the LF-26 process to impart a desirable salty taste to unflavored fried potato chips. The effect of the inventive flavor tablets on the saltiness of potato chips coated with them was compared with that of commercially available CS-8 tablets. One gram of the test tablets was mixed with 100 grams of unflavored fried potato chips in a seasoning drum to ensure uniform coating and evaluated by at least five trained panelists.

[0353] Trained tasters rinsed their mouths with mineral water between ratings, consumed the same portion of the food samples, and assigned a taste intensity value to each sample, ranging from 0 (no taste change compared to a control food coated with CS-8 taste enhancer) to 10 (highest intensity above baseline). Each judge repeated the sensory test four times, with a 5-minute break between each test. The food samples were randomly assigned to either the reference sample CS-8 or the currently used LF-26 flavoring tablet in each round of evaluation.

[0354] The taste scores of each food sample were summed for each panelist and divided by the total number of tests to obtain a calculated average taste score for each food sample. In the first round of experiments, LF-26 salt flakes were found to provide a significantly stronger saltiness intensity than the commercial CS-8 salt flakes used as a reference, when the weight of salt flakes in the potato chips was the same. In the second round of experiments, the relative amount of LF-26 crystals on the bare potato chips was gradually reduced (for example: -30%, -50%, -75%) until the taste was similar to that obtained by sprinkling 1 gram of CS-8 crystals on 100 grams of potato chips. The results showed that the amount of LF-26 could be reduced by approximately 30-40% (i.e., to 0.6-0.7 grams of salt per 100 grams of potato chips) while maintaining a flavor similar to the reference sample.

[0355] The experiment was repeated using sodium chloride flakes prepared identically to LF-13 and compared to commercially available CS-8. All trained panelists, eight in total, agreed that the relative dosage of LF-13 flake salt applied to bare potato chips could be reduced by at least approximately 30-35% (i.e., to 0.65-0.70 grams of salt per 100 grams of potato crisp) while maintaining a flavor profile similar to that of the CS-8 reference sample (applied at 1 gram of salt per 100 grams of potato crisp). This estimate was based on the observation that when the flake dosage according to the present invention was reduced to 75% of the reference flake weight, none of the panelists could distinguish the test sample from the reference. When the LF-13 dosage was reduced to 50% of the CS-8 reference, a quarter of the panelists rated the potato chips containing the test flakes as "less salty." When the test flake dosage was further reduced to 25% of the reference, half of the panelists could perceive a flavor difference.

[0356] It is important to note that the reference salt used in this sensory testing is itself reported to provide a reduction in sodium compared to regular table salt. Cargill reports that consumer sensory testing indicates that Fine Flake Salt (CS-8) ​​achieves the same taste as table salt using less product, resulting in a 30% reduction in sodium. In other words, 1 gram of CS-8 provides the same salty taste as approximately 1.4 grams of regular table salt. Since this experiment showed that less than approximately 0.65-0.7 grams of flake salt (used per 100 grams of potato chips) according to the present teachings has a mouthfeel equivalent to 1 gram of CS-8, it can be inferred that 0.65-0.7 grams of LF-13 or LF-26 flakes, or less, has a mouthfeel equivalent to approximately 1.4 grams of table salt. Therefore, the sodium chloride flakes of the present invention can achieve at least a 50% reduction in sodium compared to conventional table salt.

[0357] Example 12: Pretreatment of raw materials

[0358] As described in the previous examples, the raw material to be made into sheets and / or the liquid raw material prepared therefrom can be pretreated before use in the present method or apparatus. For example, in Example 3, the raw material with an average diameter of about 500 μm was ground to an average diameter of about 50 μm to facilitate the preparation of the mother liquid; in Example 8, the raw material with an average diameter of about 500 μm was ground to an average diameter of about 5 μm to facilitate the preparation of the raw material solution and the raw material dispersion, and in the same example, the raw material solution was preheated to the same temperature as the surface of the rotating cylinder. These pretreatment steps are performed as independent steps before the liquid raw material is applied to the outer surface of the rotating cylinder. In this example, the pretreatment is performed simultaneously with the subsequent steps of the sheeting process.

[0359] The structure of the pretreatment apparatus is similar to that of the previously described sheeting apparatus. The apparatus consists of two cylinders with zirconia outer surfaces, each mounted with a zirconia sleeve with a diameter of 11 cm and an axial length of 20 cm. The cylinders are heated to 65°C, rotated at 250 rpm, and pressed into contact by a pneumatic piston at a calculated Hertzian contact pressure of 365 MPa. The rotational axes of the two cylinders in the pretreatment apparatus are slightly tilted relative to the horizontal, so that one end of the nip is higher than the other. Compared to the previously described peeling experiments, liquid feedstock (a 25 wt.% aqueous NaCl solution) is continuously supplied to the upper end of the nip at a sufficiently high flow rate (~33 ml / min) to form a liquid feedstock reservoir along the nip and overflow at the lower end. This feed rate would be too high for sheeting under similar conditions, resulting in shearing of the material upstream of the nip as it moves along the nip, ultimately overflowing from the lower end. The feed at the top of the squeeze point was a clear solution, while the discharge at the bottom was a white slurry, indicating at least a preliminary material concentration effect. This result was confirmed by weight loss analysis, which showed that the salt concentration of the sludge was at least 50 wt.%, so the calculated flow rate at the discharge point did not exceed approximately 16 ml / min. The dynamic viscosity of the concentrated liquid was measured at room temperature in 100s -1 The shear rate was measured to be approximately 1,500 mPa.s.

[0360] Without being bound by any particular theory, it is believed that a portion of the water in the liquid feed is removed as it passes through the nip, and any non-volatile matter that passes through the nip is recycled back to the upstream pool. Despite continued addition of liquid feed upstream, the concentration of solids in the pool gradually increases. As the solution transforms into a dispersed system (as evidenced by increasing turbidity), the solidified particles are exposed to the shear forces generated by the rotating cylinder. This produces a secondary effect: particle size reduction. In this experiment, salt with an initial diameter of 500 μm (dissolved in liquid applied to the upper end of the nip) was sheared into cubic particles with an average side length of approximately 2.5 μm. Notably, this dramatic particle size reduction was achieved in just seconds (less than 10 seconds in this experimental setup), compared to 1.5 hours for a similar particle size reduction using standard ball milling. Because this pretreatment process both concentrates the material and reduces the size of the dispersed particles, it can be fed directly into the nip of the flaking equipment, such as the 59 wt.% salt feed described previously in Example 8.

[0361] Example 13: Specific surface area of ​​flakes

[0362] The specific surface area (SSA) of the material flakes prepared using this method can be measured and compared with the specific surface area of ​​the corresponding material before flake formation (serving as a reference value) using the following method. The surface area of ​​the sample was measured using a Micromeritics Instrument Corporation ASAP 2020 Accelerated Surface Area and Porosity Measurement System using gas adsorption techniques according to standard methods. The following steps are briefly described: The sample was weighed and placed in a measuring glass tube with a known free space. A filler rod was inserted into the tube, and the tube mouth was sealed with a suitable frit to allow gas flow during analysis. The sample was dried overnight under vacuum. The dried sample was then subjected to a heated vacuum stage with a target temperature of 30°C and a heating rate of 1°C / min. The vacuum was applied at a rate of 5 mmHg / s until a vacuum of 10 μmHg was achieved. The measuring glass tube was then transferred to liquid nitrogen for a nitrogen infusion stage lasting 10 minutes to allow molecules to physically adsorb onto the dried sample surface. Excess nitrogen was then vented under a vacuum of 100 mmHg, and measurements were performed for 120 minutes, with an analysis interval of 5 seconds. Each measurement was repeated at least three times, and the specific surface area of ​​the samples was calculated by the BET method.

[0363] Example 14: Flowability of sheet materials The effect of material form on flowability can be determined by any suitable method. For example, a sample mass can be weighed and timed to flow through a calibrated orifice in a flowmeter funnel, as described in ASTM B213 (Hall flowmeter) or ASTM B964 (Carney flowmeter). If flakes or reference particles of the water-soluble material do not flow freely at a regular and constant rate in the former instrument, the latter method should be used.

[0364] The experiment is best carried out in a temperature and humidity controlled laboratory to ensure low relative humidity and stable temperature. Fix the dry and clean flow meter funnel on a stable workbench and support it with a bracket to ensure that the flow measurement is not disturbed. When the discharge port of the funnel is blocked, carefully place the sample that has been dried at 120°C for 2 hours into the funnel with a predetermined weight, avoiding knocking, vibration or any human operation that may cause sample accumulation. When the discharge port is opened, start the timing device at the same time to record the time required for the last part of the sample to flow out of the discharge port. Multiple flow tests can be performed, each time using a fresh dry sample, and the flow time corresponding to the same sample can be averaged. The flow time of different samples, or the average value of repeated tests on different samples, can be compared. The flow rate can be calculated and normalized based on the funnel dependency factor.

[0365] Worked Example Summary

[0366] As shown in the table above and the results reported therein, the methods of the present invention and exemplary apparatus for implementing the methods are suitable for rapidly producing microscopic flakes, with some experiments achieving a sufficiently high proportion of submicron flakes to permit their separation. All flakes, regardless of their average thickness range (approximately 0.5 to 200 μm as shown), exhibited dimensionless aspect ratios of at least approximately 5 (see LF-6), with the majority exceeding 30. The flakes obtained in accordance with the present invention are believed to be composed of at least compacted solid particles, and in most cases, these particles also agglomerated due to the pressure-induced gradual separation of the particle aggregates during liquid removal.

[0367] Although the feasibility of the sheeting method and apparatus of the present invention has been primarily demonstrated with taste substances (alone or in mixture), its scope of application is not limited to such compounds. In addition, a variety of water-soluble and water-insoluble materials with other industrial uses have also been successfully made into sheets. Considering the preparation of sheets of water-soluble material by applying a relatively non-viscous liquid to a movable surface (forming a compacted gap with an opposing surface), sheets can be prepared whether the material is fed in the form of a solution (see, for example, LF-1 to LF-6, and LF-8 to LF-13) or in the form of a dispersion (see LF-7). Similarly, for water-insoluble materials, sheets can be prepared whether they are prepared from a dispersion (see LF-14 to LF-17) or from a solution (see LF-18).

[0368] Advantageously, the flakes prepared by the present method exhibited an improved dissolution rate compared to corresponding reference materials (e.g., taste substances). This improvement was demonstrated by an approximately 10-fold increase in the dissolution rate of salt or detergent mixtures (see LF-1 and LF-22), with similar increases in dissolution rate observed for sodium dihydrogen phosphate and disodium hydrogen phosphate monohydrate (see LF-9 and LF-10). Notably, the bulk density and tap density of the active exfoliated salt flakes exhibiting accelerated dissolution were approximately 10% of the bulk density or tap density of the control salt, respectively. Surprisingly, when the material was a crystalline taste substance, the microstrain in the structure of the flake taste substance was at least approximately three times greater than that of the control taste substance crystals that were originally dissolved to form the flake. The crystallite size was also found to be at least approximately 36 times smaller than that of the reference granular taste substance, further supporting the idea that the flakes (e.g., taste substances), when prepared as described herein, were subject to constraints not typically present in naturally grown crystals (e.g., compressive forces perceived during embossing). The flakes of the present invention also exhibited good compressibility suitable for standard commercial processes.

[0369] Taking sodium chloride flakes as an example, as a taste test agent, they have been shown in sensory studies to have the same taste as reference salt, but with a relatively lower content. Current experiments show that the sodium content may be reduced by at least 50% compared to ordinary table salt.

[0370] This method has been demonstrated to be applicable to a variety of materials, providing a wide range of activities for tablets, not limited to taste or the food industry. Importantly, tablets prepared using the methods or apparatus of the present invention exhibit unique characteristics with respect to measurable properties and their calculated values, as demonstrated by the ASP and ratios such as F1 to F6, as defined herein. In some cases, tablets of the present invention can be distinguished by one or more of these characteristics.

[0371] In addition to the features described in this disclosure and claimed in the appended claims, the features listed in the following clauses are considered independently inventive in nature to provide a fair basis for filing one or more divisional patent applications in the future.

[0372] 1. A method for manufacturing a sheet, the method comprising: a) providing a raw material comprising at least one material; b) applying the raw material to a first movable surface so as to form a uniform layer of the raw material on the surface; and c) periodically passing the raw material through at least one pressing zone formed by pressing the first movable surface against an opposing surface so as to gradually form solid particles of the raw material, wherein the particles are compacted and agglomerated in step c) to form a sheet of a sheet made of the raw material.

[0373] 2. The method according to claim 1, wherein the raw material is applied in a dry state.

[0374] 3. The method of claim 1, wherein the raw material is applied in a paste form, the paste raw material having a dynamic viscosity of 5,000 millipascal seconds (mPa·s) or more, the method further comprising gradually removing any liquid present in the paste raw material.

[0375] 4. The method of claim 1 , wherein the feedstock is applied in liquid form, optionally having a viscosity not exceeding 5,000 mPa·s, the method further comprising gradually removing any liquid from the liquid feedstock.

[0376] 5. A method according to paragraph 3 or 4, wherein the liquid in the paste or liquid feed is selected to react with one or more materials in the feed so that the chemical composition of the tablets is different from the chemical composition of the one or more materials in the feed.

[0377] 6. A method according to any one of paragraphs 3 to 5, wherein the liquid is removed from the slurry or liquid in one or more cycles by evaporating the liquid.

[0378] 7. A method according to any one of clauses 1 to 6, wherein the average thickness t of the sheet is not more than 200 μm.

[0379] 8. A method according to any one of clauses 1 to 7, wherein the average aspect ratio ASP of the sheet (the ratio of the longest planar dimension L to the maximum thickness t of the sheet) is not less than 10:1 on average.

[0380] 9. A method according to any one of clauses 1 to 8, wherein the tablets of compacted and agglomerated particles of solid material contain less than 5 wt.% liquid.

[0381] 10. A method according to any one of clauses 1 to 9, wherein the relative surface separation distance of the roller gap formed between each roller is dynamically variable, the separation distance being reduced to 1 micron or less in the absence of the raw material or its derivatives, and optionally not exceeding 400 microns in the presence of the raw material.

[0382] 11. An apparatus for preparing a sheet from a raw material of at least one material, the apparatus comprising: a) a support frame, b) two cylinders mounted within the frame, at least one of the cylinders being movable relative to the support frame, c) a force mechanism for applying force to bring the cylinders into contact with each other to form a nip, and d) a drive motor for rotating at least one of the cylinders, characterized in that e) a metering device for applying the raw material to at least one of the cylinders to form a film containing solid particles of the material on the surfaces of the two cylinders, wherein during use, the number or concentration of the solid particles increases as the film repeatedly passes through the nip, and f) a controller for adjusting the material supply rate of the metering device according to an empirically prepared table which predicts the relationship between the rate and at least one of the following factors: the speed of the motor-driven cylinder, the force at the nip, the temperature of the cylinder surface, and the composition of the material.

[0383] 12. Apparatus according to claim 11 wherein the metering means is adapted to apply the slurry in the form of a paste or liquid, the amount or concentration of solid particles increasing during use as the film is passed repeatedly through the nip.

[0384] 13. The apparatus according to clause 12, further comprising a heating device for facilitating the removal of liquid from the slurry or liquid feedstock.

[0385] 14. An apparatus for preparing a sheet from a raw material of at least one material, the apparatus comprising: a) a support frame, b) two rollers mounted on the frame, at least one of the rollers being movable relative to the support frame, c) a mechanical device for applying a force to bring the two rollers into contact with each other to form a pressing roller, and d) a drive motor for rotating at least one of the two rollers, characterized in that e) a metering device for applying the raw material to at least one of the rollers to form a film, the film comprising solid particles of the material, the number or concentration of the solid particles increasing as the film repeatedly passes through the pressing roller during use, f) a torque measuring device for determining the torque applied by the drive motor, the torque varying with the proportion of solid particles in the film, and g) a controller for adjusting the material supply rate of the metering device based on the measured torque.

[0386] 15. An apparatus for preparing a sheet from a liquid feedstock, the feedstock being a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame, b) two cylinders mounted on the frame, at least one of the cylinders being movable relative to the support frame, c) a force mechanism for applying a force to bring the cylinders into contact with each other to form a pressure zone, and d) a drive motor for rotating at least one of the cylinders, characterized in that: e) a metering device for applying the liquid feedstock to at least one cylinder so as to form a thin film only on the surface of the cylinder, the concentration of solid material in the film increasing as the film repeatedly passes through an extrusion gap, thereby forming a sheet of the material, and f) a controller for adjusting the rate at which the liquid feedstock is applied to the cylinder to match the rate at which liquid is lost from the film as the film continues to pass through the extrusion gap.

[0387] 16. An apparatus for preparing a sheet from a liquid raw material, wherein the liquid raw material is a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame, b) two rollers mounted on the frame, at least one of the rollers being movable relative to the support frame, c) a force mechanism for applying a force to bring the rollers into contact with each other to form a pressure zone, d) a drive motor for rotating at least one of the two cylinders, and e) an apparatus for applying a film of the liquid raw material to the cylinder as the cylinder rotates, characterized in that the interior of at least one cylinder is heated so that the concentration of solid material in the film increases as the film repeatedly passes through the pressure zone, thereby forming a sheet of material on the cylinder.

[0388] 17. A sheet composed of sodium chloride, said material having at least one of the following crystallographic characteristics:

[0389] A- The grain size of the sodium chloride in the flakes is at least 20%, 30%, 40% or 50% smaller than the grain size of a reference unflaked sodium chloride, and the grain size in the flakes is optionally at least 2, 3 or 4 times the reference grain size; and

[0390] The microstrain percentage value of the B-flaked sodium chloride is at least 20%, 30%, 40% or 50% greater than the microstrain percentage value of the reference unflaked sodium chloride, and the microstrain percentage value in the flake is optionally at least 2 times, 3 times or 4 times the reference microstrain percentage value.

[0391] 18. A sheet made of at least one material, the sheet having a thin planar dimension, wherein each sheet has a longest dimension and the plurality of sheet have an average longest dimension (L) within the plane, each sheet has a maximum thickness and the plurality of sheet have an average maximum thickness (t) from one side of the plane to the other, and wherein the sheet has a dimensionless aspect ratio between the longest dimension and the maximum thickness such that the average aspect ratio (Asp=L / t) of the plurality of sheet is at least 10:1; the sheet having at least three of the structural features described in a) to j) below, and further having at least one, at least two, or at least three of the features described in k) to y) below:

[0392] a) t is at most 200 μm, 150 μm, 100 μm, 80 μm, 60 μm or 40 μm;

[0393] b) t is at most 20 μm, 18 μm, 16 μm, 14 μm, 12 μm or 10 μm;

[0394] c) t is at most 9 μm, 8 μm, 7 μm, 6 μm, 5 μm, 4 μm, 3 μm or 2 μm;

[0395] d) t is a maximum of 1μm, 0.9μm, 0.8μm, 0.7μm, 0.6μm, 0.5μm, 0.4μm or 0.3μm;

[0396] e) t is at least 50 nm, 100 nm, 150 nm or 200 nm;

[0397] f) L is at most 10,000 μm, at most 7,500 μm, at most 5,000 μm, at most 4,000 μm, at most 3,000 μm, at most 2,000 μm, at most 1,500 μm, or at most 1,000 μm;

[0398] g) L is at most 500 μm, at most 400 μm, at most 300 μm, at most 200 μm, at most 100 μm, or at most 50 μm;

[0399] h) L is at least 5 μm, at least 7.5 μm, at least 10 μm, at least 12.5 μm, or at least 15 μm;

[0400] i) Asp is at least 20:1, at least 30:1, at least 40:1, or at least 50:1;

[0401] j) Asp is a maximum of 150:1, a maximum of 125:1, a maximum of 100:1, or a maximum of 75:1;

[0402] k) The specific surface area (SSA) of the flakes is at least 0.001 m 2 / g, at least 0.005m 2 / g, at least 0.01m 2 / g, at least 0.05m 2 / g, at least 0.1m 2 / g, at least 0.2m 2 / g, at least 0.3m 2 / g, at least 0.4m 2 / g, or at least 0.5m 2 / g;

[0403] l) The specific surface area (SSA) of the flakes does not exceed 10m 2 / g, not exceeding 8m 2 / g, not exceeding 6m 2 / g, not exceeding 4m 2 / g, or not more than 2m 2 / g;

[0404] m) the dissolution rate DT of the tablet (which can be measured in water at 23°C) and its ratio F1 = ASP / DT are not less than 5, not less than 10, not less than 15, not less than 25, not less than 50, not less than 75 or not less than 100;

[0405] n) the dissolution rate DT of the tablet (measured in water at 23°C) and its ratio F1 = ASP / DT do not exceed 500, 400, 300, 200 or 150;

[0406] o) The flake has a bulk density ρ T and bulk density ρ B , and the ratio of the two is F2=ρ T / ρ B not less than 1.25, not less than 1.5, not less than 1.75, not less than 2, not less than 2.25, not less than 2.5 or not less than 2.75;

[0407] p) The flake particles have a bulk density ρ T and bulk density ρ B , and the ratio of the two is F2=ρ T / ρ B Maximum is 5, Maximum is 4.5, Maximum is 4, or Maximum is 3.5;

[0408] q) The flake has a bulk density ρ B , and F3=ASP / ρ B The ratio is not less than 25, 50, 75, 100, 150, 200, 250, 300 or 350;

[0409] r) Bulk density of the flakes ρ B and ratio F3 = ASP / ρ B The value of is up to 1,000, up to 750, up to 500, or up to 400;

[0410] s) Tap density of flakes ρ T and F4 = ASP / ρ T The ratio is not less than 20, 40, 60, 80, 100, 120, 140, 160 or 180;

[0411] t) Bulk density of the sheet ρ T and F4 = ASP / ρ T The ratio is at most 500, at most 400, at most 300, or at most 200;

[0412] u) The sheet has a compressed density ρ C and bulk density ρ B , the ratio of the two is F5 = ρ C / ρ B not less than 1.6, not less than 1.8, not less than 2.0, not less than 2.2, not less than 2.4, not less than 2.6, not less than 2.8, not less than 3.0 or not less than 3.2;

[0413] v) The sheet has a compressed density ρ C and bulk density ρ B , and the ratio of the two is F5=ρ C / ρ B Maximum is 10, Maximum is 7.5, Maximum is 5, or Maximum is 4;

[0414] w) The sheet has a compressed density ρ C and bulk density ρ B , and the ratio of the two is F6=(ASP×ρ B ) / ρ C Not less than 6, not less than 10, not less than 15, not less than 20, not less than 25, not less than 30, not less than 35 or not less than 40;

[0415] x) The sheet has a compressed density ρ C and bulk density ρ B , and F6=(ASP×ρ B ) / ρ C The ratio is at most 200, at most 150, at most 100, at most 75, or at most 50; and

[0416] y) The material of the platelet is a crystalline material.

[0417] 19. A sheet as described in clause 17 or 18, prepared by any method and / or any apparatus described and claimed in this specification.

[0418] 20. A tablet according to clause 18 or 19, wherein at least one material comprising the tablet is a taste substance suitable for imparting taste to a product containing or consisting of the same.

[0419] 21. The sheet as described in any one of Items 18 to 20, wherein the material is sodium chloride, and the crystalline material has at least one of the following crystallographic characteristics:

[0420] A- the grain size of the sodium chloride in the flakes is at least 20%, 30%, 40% or 50% smaller than the grain size of a reference unflaked sodium chloride, the grain size in the flakes optionally being at least 2, 3 or 4 times the reference grain size; and

[0421] The microstrain percentage value of the B-flaked sodium chloride is at least 20%, 30%, 40% or 50% of the microstrain percentage value of the reference unflaked sodium chloride, and the microstrain percentage value in the flake is optionally at least 2 times, 3 times or 4 times the reference microstrain percentage value.

[0422] 22. A sheet as claimed in claim 18 or 19, wherein at least one material comprising the sheet is an active or inactive ingredient suitable for providing efficacy and / or manufacturing advantages to a finished product containing or made therefrom.

[0423] 23. A food product comprising a flake according to any one of clauses 17 to 20, said flake being distributed on and / or in said food product and optionally being insoluble therein.

[0424] 24. A manufactured article comprising the sheet of any one of clauses 18, 19 or 22.

[0425] 25. A method of improving a food product, the method comprising adding a tablet as claimed in any one of clauses 20 to 22 to the food product.

[0426] 26. A method of improving the performance of an article of manufacture, the method comprising incorporating the tablet of any one of clauses 19, 22 or 24 into the article of manufacture.

[0427] 27. A method of reducing the amount of a taste substance that provides a desired taste in a food, the method comprising replacing at least a portion of the taste substance in the food with a tablet according to clause 20 or 21, optionally replacing all of the taste substance.

[0428] 28. A method of reducing the content of an active or inactive ingredient used to provide a desired effect in a manufactured product, the method comprising replacing at least a portion of the ingredients in the manufactured product, optionally replacing all of the ingredients, with the tablet according to clause 22.

[0429] Those skilled in the art will appreciate that certain features described in this disclosure for clarity in the context of separate embodiments may also be provided in combination in a single embodiment. Conversely, certain features described in this disclosure for brevity in the context of a single embodiment may also be provided individually or in any suitable subcombination, or in any suitable manner in any other described embodiment of the disclosure. Certain features described in various embodiments should not be considered essential features of that embodiment unless the embodiment would not function properly without those elements.

[0430] Although the present disclosure has been described with respect to various specific embodiments, for illustrative purposes only, the embodiments specifically disclosed should not be considered restrictive. Based on the disclosure of the present application, those skilled in the art will recognize many other alternatives, modifications, and variations. Therefore, the present application is intended to encompass all such alternatives, modifications, and variations, and is limited only by the disclosure of the present application and its equivalents.

[0431] In the description and claims of this disclosure, the verbs "comprise," "include," and "have," and their variants, are used to indicate that the object of the verb referent is not a complete list of the features, members, steps, components, elements, or parts of the subject matter of the verb referent. However, the compositions taught by the present invention may also consist essentially of or consist of the recited components, the methods taught by the present invention may also consist essentially of or consist of the recited process steps, and the devices taught by the present invention may also consist essentially of or consist of the recited devices.

[0432] Positional or motion terms such as "upper," "lower," "right," "left," "bottom," "below," "lower," "top," "above," "raised," "high," "vertical," "horizontal," "front," "rear," "backward," "forward," "upstream," and "downstream," and grammatical variations thereof, are used for exemplary purposes only to describe the relative position, arrangement, or displacement of certain components, to indicate first and second components in the present schematic, or both. Such terms do not necessarily mean, for example, that the "bottom" component is below the "top" component, as such orientations, components, or both may be flipped, rotated, shifted in space, positioned diagonally, horizontally or vertically, or similarly modified.

[0433] In this specification, the singular forms "a," "an," and "the" include plural meanings and mean "at least one" or "one or more" unless the context clearly requires otherwise. In this specification, the term "at least one of A and B" means A or B, and in some embodiments may mean A and B.

[0434] Unless otherwise stated, "and / or" between the last two options in a list means that one or more of the listed options can be selected.

[0435] The word “exemplary” is used in this document to mean “serving as an example, instance, or illustration.” Any embodiment described as “exemplary” should not be construed as preferred over other embodiments, nor should it exclude the possibility of incorporating features from other embodiments.

[0436] Unless otherwise indicated, when adjectives such as "substantially," "approximately," and "about" are used in this document to modify a condition or relationship characteristic of a feature or combination of features in an embodiment of the present disclosure, it should be understood that the definition of the condition or characteristic is within an acceptable tolerance range to ensure that the embodiment can function properly in the intended application, or within the range of variation allowed by the measurement process and / or the measuring instrument used. For example, when the word "about" or "approximately" appears before a numerical value, it may mean ±15%, ±10%, or even only ±5%, or any other suitable ± deviation within the above range, and in some cases may mean the exact value. In addition, unless otherwise indicated, the terms (such as numbers) used in the embodiments of the present disclosure, even if not accompanied by such adjectives, should be understood to have tolerances that may deviate from the precise meaning of the relevant terms but still enable the embodiment or its relevant parts to operate and function as described and / or as understood by those skilled in the art.

Claims

1. A method for manufacturing a sheet, the method comprising: a) providing a liquid raw material, wherein the liquid raw material comprises at least one solid material dissolved or dispersed in the liquid; b) applying the liquid raw material to a first movable surface to form a thin film of the liquid raw material on the surface; c) cyclically i) evaporating at least a portion of the liquid in the film of the liquid feedstock to increase the concentration of solid particles in the film, and ii) applying pressure to the film by passing the film through at least one nip formed by pressing nip-forming surfaces facing each other, thereby gradually forming a layer of a sheet of agglomerated and compacted solid particles until the liquid content in the sheet is less than 5% by weight. 2 . The method according to claim 1 , wherein the average maximum thickness t of the sheet is not more than 200 μm.

3. The method according to claim 1 or 2, wherein the average aspect ratio ASP of the sheet, that is, the ratio of the longest planar dimension L to the maximum thickness t of the sheet, is not less than 10:

1.

4. The method according to any one of claims 1 to 3, wherein the liquid raw material is applied by a glue applicator, the first movable surface and the glue applicator move relative to each other during the gluing step, and at least one of the formation of the film of the liquid raw material, the concentration of the solid particles in the film, and the acquisition of the sheet is caused by passing through the nip.

5. The method according to any one of claims 1 to 4, further comprising forming the film of the liquid feedstock before passing through at least one of the nip zones.

6. A method according to any one of claims 1 to 5, wherein the first movable surface is the outer surface of a first rotating cylinder forming one of the opposing nip forming surfaces, the other nip forming surface of the nip being optionally formed by the outer surface of a second rotating cylinder.

7. The method of any one of claims 1 to 6, wherein the temperature of the liquid feedstock on the first movable surface is above ambient temperature and at least 5°C below the boiling point of the liquid.

8. A method according to any one of claims 1 to 7, wherein at least one of the nip forming surfaces is heated to a temperature above ambient temperature.

9. A method according to any one of claims 1 to 8, wherein the pressure applied in the or each nip is independently from 10 MPa to 1,500 MPa, from 50 MPa to 1,250 MPa or from 100 MPa to 1,000 MPa.

10. The method according to any one of claims 1 to 9, further comprising collecting the sheet downstream of at least one nip forming surface.

11. The method according to any one of claims 1 to 10, wherein the liquid raw material is supplied continuously and the obtained flakes are collected continuously.

12. The method according to any one of claims 1 to 11, wherein The opposing nip forming surfaces have a dynamically variable spacing in each or said nip, said spacing being reduced to 1 μm or less in the absence of said liquid material, said film, said layer or said sheet derived therefrom, and said spacing optionally not exceeding 400 μm in the presence of said liquid material.

13. The method of any one of claims 1 to 12, wherein the material is a crystalline material.

14. The method according to any one of claims 1 to 13, wherein at least one of the one or more materials is a taste substance.

15. An apparatus for preparing a sheet from a liquid feedstock comprising at least one material dissolved or dispersed in the liquid, the apparatus comprising: Support frame, two cylinders mounted on the frame, at least one of which is movable relative to the support frame, a force applying mechanism for applying force to bring the cylinders into contact with each other to form a pressing zone, a drive motor for rotating at least one of the two cylinders, It is characterized by a metering device for applying the liquid raw material to at least one of the cylinders to form a thin film on the surfaces of both cylinders, wherein during use, as the film repeatedly passes through the nip, the concentration of the solid particles in the material gradually increases, a torque measuring device for determining the torque applied by the drive motor, said torque varying with the proportion of liquid in the membrane, and A controller is configured to adjust a rate at which the metering device applies the liquid feedstock based on the measured torque.

16. The apparatus of claim 15, wherein the metering device is adapted to apply discrete amounts of the liquid feedstock, the controller regulating the dosage and / or repetition rate of the discrete applications.

17. The apparatus of claim 15, wherein the metering device is adapted to apply a continuous flow of the liquid feedstock, the controller regulating the flow rate of the continuous flow.

18. Apparatus according to any one of claims 15 to 17, wherein at least one cylinder is heated during use, at least one heating means being located inside and / or outside the heated cylinder.

19. The device of any one of claims 15 to 18, wherein the force applying mechanism comprises a pneumatic piston or a hydraulic piston, the hydraulic piston comprising an accumulator.

20. The apparatus according to any one of claims 15 to 19, further comprising a collector for collecting the flakes.

21. The apparatus of claim 20, further comprising separation means for separating the flakes from the surface of the cylinder, said separation being dependent on a low liquid fraction in the film.

22. The apparatus according to claim 21, wherein said separating means is retractably contacted with a surface of at least one of said cylinders and positioned so that said separated sheets are collected in said collector, said separating means being selected from the group consisting of a scraper and a blade.

23. The apparatus according to any one of claims 15 to 22, further comprising a leveling device for leveling the liquid level of the liquid material before the liquid material passes through the nip.

24. The device according to any one of claims 15 to 23, further comprising at least one of the following: a) a pre-treatment station adapted to (i) heat the liquid feedstock, (ii) reduce the particle size of material dispersed therein, and / or (iii) increase the concentration of dissolved or dispersed material therein, said pre-treatment station being located upstream of and in fluid communication with said metering device; and b) a post-flaking station adapted for (i) drying and / or (ii) sorting the collected flakes, and / or for (iii) recycling the flakes that do not meet the required size to the metering device.

25. The device according to any one of claims 15 to 24, wherein The rotation axis of the cylinder is not horizontal, the metering device is located at the upper end of the cylinder to apply the liquid raw material, and the flakes are collected at the lower end of the cylinder.

26. The apparatus according to any one of claims 15 to 25, further comprising at least one cylinder urged into contact with one of the two cylinders to form at least one additional nip, three or more cylinders being arranged linearly or radially with respect to each other.

27. The device according to any one of claims 15 to 26, wherein During use, the opposing nip forming surfaces have a dynamically variable spacing in each or said nip, said spacing being reduced to 1 micron or less in the absence of said liquid material, said film or said sheet derived therefrom, and optionally not exceeding 400 microns in the presence of said liquid material.

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