Method and apparatus for preparing flakes

Abstract

A method for producing flakes is disclosed. The method comprises the following steps: a) providing a liquid raw material comprising at least one solid material dissolved or dispersed in a liquid; b) coating the liquid raw material onto a first movable surface to form a thin film of the liquid raw material on the surface; c) periodically applying pressure to the thin film by i) evaporating at least a portion of the liquid from the thin film to increase the concentration of solid particles, and ii) passing it through at least one nip formed by pressing opposing surfaces together, thereby gradually forming a layer of relatively dry flakes consisting of aggregated and / or compressed solid particles. Flakes produced by the above method and apparatus for producing them, as well as the uses and advantages of such flakes, are also disclosed.

Description

Cross-reference of related applications

[0001] This application claims priority under the Paris Convention from UK Patent Application No. GB ​​2302788.1, filed on 27 February 2023, and GB 2316241.5, filed on 24 October 2023. The contents of these applications are incorporated herein by reference as if they were fully described herein. [Technical Field]

[0002] This disclosure relates to a method for producing flakes from a material placed in a liquid, and an apparatus that enables the carrying out of this method. [Background technology]

[0003] It has long been known that altering the form of a material affects its properties or behavior in a wide variety of ways, too numerous to list comprehensively. One of the many properties that can be affected by changing the dimensions and shape of a material, particularly its specific surface area (SSA), is its solubility in any given liquid. Increasing the specific surface area and dissolution rate of a material has applications in a wide range of fields, such as agriculture, cosmetics, manufacturing, water treatment, firefighting, pharmaceuticals, and food.

[0004] The latter area is easier to understand because it ultimately involves the consumption of products by living subjects; therefore, the merits of the following disclosures will be explained in particular with respect to the components of such products.

[0005] Flavor perception is a complex process involving smell, taste, and chemical sensations (e.g., spiciness, astringency, and irritation). Taste is perceived through dedicated taste receptors located in taste buds on the tongue, sides of the mouth, soft palate, cheeks, back of the throat, and esophagus. The five perceptible basic tastes are sweet, sour, salty, bitter, and umami, which can be felt when eating sugar, vinegar, salt, caffeine, and monosodium glutamate, respectively. Compounds or compositions that can induce or trigger the perception of one or more tastes within a taste category or other tastes are called flavoring agents. Flavoring agents can be added to food to improve the overall taste, which is one reason why animals secrete saliva. When flavoring agent molecules dissolve in saliva, they can properly contact the taste receptor nerves within each taste bud, stimulating the nerves and transmitting the perception of taste to the brain.

[0006] The importance of taste is not limited to the food that humans consume; it can similarly influence compliance in other animals, for example, when they take pharmaceuticals. However, the current issue may be easier to understand if discussed in the former context. For example, consider table salt (sodium chloride, often simply called salt) and sugar (glucose, fructose, sucrose, lactose, etc.). Both are important components of the foods we eat and drink, and relatively high levels are listed on the packaging as a health concern, considering the long-term effects. Excessive salt intake can cause diseases such as high blood pressure, heart disease, and stroke through the sodium portion. Excessive sugar intake, if accompanied by insufficient endogenous insulin secretion, can cause weight gain, damage to the eyes, kidneys, and nerves, and diabetes. On the other hand, too little of these is also undesirable. Insufficient salt concentration can cause, for example, weakness, nausea, and muscle cramps, while insufficient sugar concentration (e.g., hypoglycemia) can cause headaches, dizziness, and confusion. If the concentration of salt or sugar is too low or too high for an extended period, medical consequences can worsen, and in some cases, it can be fatal if left untreated. For some individuals, consuming foods with reduced levels of certain flavorings may be medically justifiable.

[0007] In recent years, the food industry has strived to reduce the salt and sugar content in products, but such reductions are sometimes compensated for by the addition of substances that enhance taste. Other approaches include replacing these representative taste substances with substances that provide similar tastes while being considered less harmful to health, or manufacturing them as hollow structures (e.g., spheres, cubes, pyramids) or as thin coatings on edible cores, which provide an increased surface area and enhanced perceived taste. Simply grinding taste substances into smaller granular particles can achieve increased specific surface area, some degree of improved adhesion to dry foods, and improved taste, but this method has been ruled out as a viable solution. This method introduces a new problem of fluidity, as the fine particles tend to stick together and form clumpy aggregates. This clogging and clumping leads to difficulties in handling, transport, and storage, or to unfavorable dustability as the fine particles become airborne during processing. Furthermore, small granular particles tend to sink in the oil layer, slowing down their dissolution and reducing the intensity of the flavor.

[0008] Consumer health, consumer compliance with ingesting materials in a favorable form, the benefits that such a form may offer to the effectiveness of the material during the manufacturing process of a product containing it, and / or the effectiveness of said product after administration are not the only improvements that can be sought. A suitably improved material allows for a reduction in its relative amount in the intended product, leading to cost savings.

[0009] The need remains to modify the form of the material to improve at least one of its properties that may be desirable for future intended uses. In the context of ingested articles such as food or pharmaceuticals, improvements arising from such forms may be exemplified by maintaining a satisfactory organic sensory sensation associated with flavoring and odor-masking agents, or achieving the desired solubility of active ingredients, while favorably reducing their presence in articles manufactured using them, respectively. [Overview of the project]

[0010] This disclosure is directed to address at least some of the aforementioned needs for materials having forms that are advantageously adapted to overcome the limitations currently observed in the art, for example, to reduce the presence of such materials and / or increase their effectiveness for their respective intended applications.

[0011] In a first embodiment, the present disclosure provides a method for producing flakes as described in detail below, as described in claim 1 and any dependent claims of the appended claims.

[0012] In a second embodiment, the present disclosure provides an apparatus for manufacturing flakes, as described in more detail below, as claimed in claim 15 of the appended claims and as claimed in the claims dependent thereon.

[0013] Further aspects of this disclosure are described in the following sections that follow the description of the embodiments.

[0014] These aspects of the present disclosure, as well as additional advantages and features, will be better understood by referring to the following detailed description, which is taken in conjunction with the figures and non-limiting embodiments. [Brief explanation of the drawing]

[0015] Next, some embodiments of the present disclosure will be described further as examples with reference to the accompanying drawings, where similar reference numerals or letters (or their last digits) indicate corresponding or similar components. This specification, together with the drawings, will make it clear to those skilled in the art how some embodiments of the present disclosure may be carried out. The drawings are for illustrative purposes only and do not attempt to show structural details of the embodiments in more detail than necessary for a basic understanding of the present disclosure. For clarity and convenience of presentation, some objects depicted in the drawings are not necessarily shown to scale. In the diagram [Figure 1]Figure 1 shows a flowchart of a method for preparing (e.g., taste) flakes according to an embodiment of this instruction. [Figure 2] A schematic representation of a nip or a series of nips that may be used according to one embodiment of the method or apparatus described herein is shown. [Figure 3] A schematic representation of a nip or a series of nips that may be used according to one embodiment of the method or apparatus described herein is shown. [Figure 4] A schematic representation of a nip or a series of nips that may be used according to one embodiment of the method or apparatus described herein is shown. [Figure 5] A schematic representation of a nip or a series of nips that may be used according to one embodiment of the method or apparatus described herein is shown. [Figure 6] A schematic representation of a nip or a series of nips that may be used according to one embodiment of the method or apparatus described herein is shown. [Figure 7] A schematic representation of a nip or a series of nips that may be used according to one embodiment of the method or apparatus described herein is shown. [Figure 8] Figures 8A and 8B are photographs captured by a scanning electron microscope (SEM) with further focused ion beam (FIB) capabilities. Figure 8A shows the flavoring substance before processing using the method or apparatus according to one embodiment of this teaching, while Figure 8B shows the same flavoring substance after processing therewith. In this particular case, the flavoring agent is supplied to the nip as a dry powder. [Figure 9] Figures 9A and 9B are similarly photographs taken with a SEM-FIB microscope. Figure 9A shows the flavoring agent before processing using the method or apparatus according to another embodiment of this teaching, while Figure 9B shows the same flavoring agent after processing therewith. In this particular case, the flavoring agent is supplied to the nip as a paste consisting of a dry powder dispersed in a viscous medium. [Figure 10]Figures 10A and 10B are similarly taken with a SEM-FIB microscope. Figure 10A shows the taster before being treated using the method or apparatus according to further embodiments of this teaching, while Figure 10B shows the same taster after being treated therewith. In this particular case, the taster is supplied to the nip as a solution. [Figure 11] Figures 11A and 11B are photographs similarly taken by a SEM-FIB microscope. Figure 11A is identical to Figure 10A and shows the taster before being treated with a method or apparatus according to another further embodiment of this teaching, while Figure 11B shows the same taster after being treated therewith. In this particular case, the taster is supplied to the nip as a dispersion in a liquid that is soluble at low concentrations. [Figure 12] Figures 12A and 12B are photographs similarly taken by a SEM-FIB microscope. Figure 12A is identical to Figures 10A and 11A, but shows the taste substance before treatment using the method or apparatus according to an additional embodiment of this teaching, while Figure 12B shows the same taste substance after treatment therewith. In this particular case, the material is supplied to the nip as a dispersion in an insoluble liquid. [Figure 13] Figures 13A and 13B are photographs similarly taken by SEM-FIB microscopy. Figure 13A shows a water-soluble material before treatment using a method or apparatus according to yet another embodiment of this teaching, and Figure 13B shows the same material after treatment therewith. In this particular case, a water-soluble material, which may be an active ingredient in various products, is supplied to the nip as a solution. [Figure 14] Figures 14A and 14B are similarly taken with a SEM-FIB microscope. Figure 14A shows a water-insoluble material before treatment using a method or apparatus according to further embodiments of this teaching, and Figure 14B shows the same material after treatment therewith. In this particular case, the water-insoluble material, which may be an active ingredient in various products, is supplied to the nip as a dispersion. [Figure 15]Figures 15A and 15B are similarly taken with a SEM-FIB microscope. Figure 15A shows the water-insoluble material before treatment using the method or apparatus described herein, and Figure 15B shows the same material after treatment therewith. In this particular case, the material is supplied to the nip as a solution in a non-aqueous solvent. [Figure 16] Figures 16A to 16F are similarly taken with a SEM-FIB microscope. Figures 16A to 16E show different commercially available sodium chloride particles that have been prepared conventionally, while Figure 16F shows flakes of the same material prepared according to this instruction. [Modes for carrying out the invention]

[0016] To address some of the shortcomings of the prior art, the present invention seeks to modify the form of a material to obtain flakes, whether they be inert components or active components such as flavoring and odor-masking agents. Methods and apparatus designed for this purpose may accordingly be called “flaking” processes and apparatus.

[0017] The disclosed invention is not limited to flavoring agents and may also apply to additional water-soluble or water-insoluble materials (e.g., detergents or any other active ingredients) that, once flaked as described herein, may induce advantages derived from different forms. However, for the sake of simplicity, the technique is primarily illustrated with these particular types of materials that can improve the taste of food. Accordingly, any reference to flavoring substances (singular or plural) below for the sake of brevity should be understood more generally as referring to any material that can be similarly treated as demonstrated herein in a non-limiting manner.

[0018] Before describing at least some embodiments in detail, let me give a general introduction.

[0019] Water-soluble materials can dissolve in water (for example, to form a clear solution). Water-soluble materials dissolve in water at a concentration of at least 10 g / l (in other words, 1 wt.%), and in some embodiments, the water-soluble materials used in the preparation of flakes of this composition have a water solubility of 2 wt.% or more, 4 wt.% or more, 6 wt.% or more, 8 wt.% or more, or 10 wt.% or more. Water solubility is usually evaluated at room temperature (between 20°C and 25°C), but materials suitable for this method may, alternatively or additionally, be water-soluble at high temperatures (e.g., temperatures at which flake processing can be performed). While solubility often refers to water, similar rules may apply to the solubility of materials in any other solvent. Solubility (or lack thereof) in any liquid can be evaluated visually; compositions in which the material dissolves at a certain concentration (and / or temperature) are generally clear, while insoluble materials form a cloudy dispersion.

[0020] While many flavoring substances are water-soluble, this is not essential for carrying out this teaching. Several components, including those known to provide flavor and containing water-insoluble components (e.g., cocoa, coffee), can also be made into flakes. To avoid misunderstanding, the method of the present invention is suitable for both water-soluble and water-insoluble materials, regardless of their intended use. Furthermore, materials can be successfully flakeped by dissolving them in a single phase in a liquid (forming a solution) or by suspending them as a solid in different phases (forming a suspension or dispersion).

[0021] For example, even if a substance is water-soluble, it can be flakebed at a higher concentration than its solubility in an aqueous liquid carrier, or dispersed in a liquid carrier other than pure water that may be insoluble (i.e., soluble at less than 1 wt.%). In such cases, the water-soluble substance will be suspended rather than dissolved. Alternatively, even if a substance is water-insoluble, it can be flakebed in a liquid carrier other than pure water. In such cases, the water-insoluble substance will dissolve rather than be suspended in the liquid acting as the solvent.

[0022] While this instruction does not necessarily alter the absolute water solubility of a material (e.g., converting a water-insoluble material to a water-soluble version), it can nevertheless significantly improve the dissolution rate to obtain a practically significant and detectable upgrade. For example, a semi-insoluble substance (e.g., soluble in water at less than 100 ppm) may not become highly soluble, but thanks to this instruction, it can become sparingly soluble. Furthermore, solubility may not be a property that needs to be changed due to a change in the material's morphology.

[0023] In some embodiments, the dissolution rate of flakes made from flaked material is at least 20%, at least 30%, at least 40%, at least 50%, or at least 60% higher than the dissolution rate of the non-flaked counterpart. The improvement in dissolution rate between the non-flaked and flaked versions of the same material can also be more than 2, 3, 4, 5, or 6 in some embodiments. In certain embodiments, the improvement in dissolution rate conveyed by the implementation of the method can be measured on the order of magnitude and can be more than 10.

[0024] The material is characterized by its solubility (or lack thereof) in water, but this does not have to be the only liquid relevant to the evaluation of the improved dissolution rate. For example, if the material is used in a manufacturing process where the reaction solution is alcohol, the improvement in dissolution rate can be evaluated in that alcohol. Furthermore, the liquid of interest for dissolution evaluation can be a blend of liquids and / or a liquid to which any agent (e.g., pH adjusters) relevant to the conditions under which solubilization is required has been added. The dissolution rate of the material can be evaluated by routine experiments using standard methods known to those skilled in the art.

[0025] Since the dissolution rate can be evaluated by the time (e.g., in seconds) required to dissolve a predetermined amount (e.g., 100 mg) of a substance in a specific volume (e.g., 100 ml) of the liquid of interest at any suitable temperature and / or pressure, under any specific stirring conditions, and / or in any apparatus suitable for such measurement, an increase in the dissolution rate corresponds to a decrease in the time required to achieve complete solubilization of the test sample under the test conditions. For example, if a flaky substance is said to have twice the dissolution rate of its non-flaky precursor, this corresponds to halving the time required for complete dissolution under similar test conditions.

[0026] Due to their size and form, conventionally prepared flavorings only partially dissolve in the mouth during consumption, meaning that the majority of the flavoring is swallowed without contributing to the perceived taste of the product. While we do not wish to be bound by any particular theory, the form described in this instruction is thought to promote the dissolution of the flavoring substance and, accordingly, increase the perceived taste compared to the same amount of a less soluble corresponding flavoring substance. In other words, for the same taste, taste intensity, and duration of taste perception, a smaller amount of the flavoring in the form described in this instruction is required than for the same flavoring in the conventional form.

[0027] Flavoring agents can conventionally be provided in various forms, shapes, and dimensions. They are typically available as small granules with particle sizes of 2–5 mm, or up to approximately 10 mm if coarse and / or flaky. Particle sizes are typically in the range of 1–2 mm, and some flavoring agents are available as fine powders of 0.2–1 mm, or even smaller for specific applications (e.g., sugar powder). Some flavoring agents, where consumption reduction is important enough to warrant substantial research, have been developed down to the micrometer (μm) range, generally with at least one dimension of 20 μm or larger, 30 μm or larger, or 40 μm or larger. Such very small particles are generally difficult to flow and cannot be applied with conventional equipment, so many remain of anecdotal interest. Materials other than flavoring agents can exist as much larger pellets in the centimeter (cm) range, or as small granules in the millimeter (mm) range, with particle sizes up to 10 mm. However, to implement this method, it would be advantageous to use smaller elements as starting materials.

[0028] The dimensions of particles (e.g., before or after processing as disclosed herein) can be estimated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), focused ion beam (FIB), confocal laser scanning microscopy, and / or optical microscopy. For example, optical microscopy can be used for particles of a few microns or up to an estimated dimension of about 200 nm, scanning electron microscopy can be used to evaluate the planar dimensions of particles having dimensions less than 200 nm, and the thickness or length of particles can be determined by focused ion beam FIB technique. Such dimensions can be evaluated, for example, by image analysis of at least one instrument field of view obtained by appropriate microscopy technique and magnification, repeating microscopic measurements on multiple particles to obtain statistical significance, with representative particles in one or more fields of view. Certain microscopes have built-in image analysis devices that can easily provide metrics relevant to a population of particles captured in the relevant field of view. Depending on the microscopy technique, magnification, and the size of the particles being investigated, a field of view may contain at least 5 particles, at least 10 particles, or at least 20 particles, and optionally, at most 200 particles, at most 100 particles, or at most 50 particles. In some embodiments, a field of view may contain particle numbers in the range of 5–200, 10–100, or 20–50. In some embodiments, two or more separate fields of view are considered to reach a particle number considered sufficient to reasonably represent the population. As used herein, mean dimensions reflect the average of such dimensions estimated for at least 10 particles, at least 20 particles, at least 30 particles, at least 40 particles, or at least 50 particles. Selecting representative particles, or representative groups of particles, that characterize the population with sufficient accuracy (e.g., by diameter, longest dimension, thickness, aspect ratio, and similar measures characterizing particles, or their average values) may be within the scope of a trained operator's skill.

[0029] According to one aspect of the present disclosure, a material having the form of thin flakes is provided (e.g., a taster or any other compound having a desired activity and / or providing any manufacturing advantages), which may be referred to herein as flakes or taster flakes. A taster flake can be defined by its thickness (or average thickness over its planar dimensions; t) and its longest dimension in that plane (L), and further characterized by the dimensionless aspect ratio between the two (Asp = L / t). Taking a taster as an example of an active ingredient that contributes to the efficacy of the final product (e.g., the taste of food), in stark contrast to conventional tasters, the flakes of the present invention have a thickness of at least in the low micrometer range (e.g., less than 200 μm, less than μm), the thickness of the taster flakes may optionally be in the submicron range (e.g., less than 1 μm), or in the nanometer (nm) range (e.g., less than 200 nm, 150 nm, or 100 nm). Flakes (of a flavoring substance) with an average thickness between 1 and 200 μm may also be called microflakes (of a flavoring substance), flakes (of a flavoring substance) with an average thickness between 0.2 and 1 μm may also be called submicroflakes (of a flavoring substance), and flakes (of a flavoring substance) with an average thickness less than 0.2 μm may also be called nanoflakes (of a flavoring substance).

[0030] In some embodiments, the average flake thickness t (for example, Tastant) is up to 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 some embodiments, the average flake thickness t is at most 20 μm, 18 μm, 16 μm, 14 μm, 12 μm, or 10 μm. In some embodiments, the average flake thickness t is at most 9 μm, 8 μm, 7 μm, 6 μm, 5 μm, 4 μm, 3 μm, or 2 μm. In some embodiments, the average flake thickness t is at most 1 μm, 0.9 μm, 0.8 μm, 0.7 μm, 0.6 μm, 0.5 μm, 0.4 μm, or 0.3 μm.

[0031] In some embodiments, the average thickness t of the (e.g., taster) flakes is at least 50 nm, at least 100 nm, at least 150 nm, or at least 175 nm.

[0032] In some embodiments, the average thickness t of the (e.g., tastent) flakes is 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.

[0033] In some embodiments, the longest planar dimension of the (e.g., taste) flake L is, on average, 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.

[0034] In some embodiments, the longest planar dimension of the flake L (e.g., flavoring agent) 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.

[0035] In some embodiments, the longest planar dimension of the (e.g., taste) flake 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, between 7.5 μm and 4,000 μm, between 7.5 μm and 300 μm, between 10 μm and 2,000 μm, between 10 μm and 1,000 μm, between 10 μm and 200 μm, or between 10 μm and 100 μm.

[0036] The ranges of thickness and longest planar dimension to which each flake of the present invention may correspond are generally correlated and can therefore be additionally or alternatively characterized by their relationship, which can be determined by calculating the dimensionless aspect ratio between them. In some embodiments, the aspect ratio (Asp=L / t) between the longest planar dimension of a (e.g., tastent) flake and its thickness is, on average, 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 some embodiments, the aspect ratio Asp is, on average, at most 200, at most 150, at most 125, at most 100, or at most 75. In some embodiments, the aspect ratio Asp is, on average, 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.

[0037] As will be further detailed below, the method and apparatus of the present invention make it possible to control to some extent the dimensions of the flakes obtained thereby. Typically, the majority of the flakes have the aforementioned size and aspect ratio that fit within a specified range, but in some embodiments, it may be desirable to achieve specific values ​​(e.g., a narrower size distribution) that may be required for a particular intended application. In such cases, the flakes obtained can be further sorted by a suitable separation process or apparatus (e.g., sieving) into smaller groups, each having sizes that fit or do not fit within the desired range. In such cases, the non-conforming particles can, if desired, be recycled back into the process (e.g., dissolved or dispersed to become part of a liquid stock to be subsequently coated). Such recycling can be carried out at a post-flaking station following flake recovery and desired sorting.

[0038] Advantageously, tasty flakes having the aforementioned dimensions are expected to exhibit good compatibility with food, good adhesion to food surfaces (and thus more uniform surface coverage), and less dust generation than conventional equivalents. While the above can be considered manufacturing advantages of the flakes, the term further encompasses stages preceding and / or following the actual production of the product (e.g., storage, transport, packaging, etc.). Furthermore, the dimensions of the flakes that can be prepared may be selected to provide other benefits depending on the desired texture (e.g., crunchiness) or appearance (e.g., the visual aspect of a topping), or the size of the flakes and the properties derived therefrom (e.g., dissolution rate). Such effects are more directly linked to the activity expected from the tasty or its flakes in the first place and are considered efficient advantages; the usefulness of tasty flakes may, in some cases, encompass both types of advantages, which are not mutually exclusive.

[0039] Tasting flakes have a higher specific surface area than standard equivalents, allowing them to dissolve faster, provide a stronger flavor with the same amount of tasting agent, or provide the same flavor with a smaller amount, thus reducing the amount of tasting agent in the food. Foods can have any conventional consistency, for example, liquid, semi-solid (e.g., spread, paste, gel) or solid at normal storage or serving temperatures. Tasting flakes can be attached to the outer surface of food (e.g., salt in snacks, sugar in cereal, spices in biscuits or croutons), dispersed within it, or attached to both. When consumed dispersed within food, materials that are less soluble or insoluble in food are usually used. For example, water-soluble flavoring agents (e.g., salt) can be dispersed as flakes in hydrophobic liquids (e.g., oil), semi-solid emulsions (e.g., mayonnaise or oil-containing sauces), or any product that is relatively solid under normal storage conditions (e.g., butter). Similar considerations regarding the relative viscosity of the product and the localization of the flakes on and / or in the product also apply to other commodities that may benefit from the presence of flakes prepared as taught herein.

[0040] Having a higher specific surface area can not only accelerate the dissolution rate of any particular material in any particular liquid, but also potentially increase any other desirable intermolecular interactions. Taking chemical reactions as an example, materials acting as catalysts in such reactions are expected to stimulate the rate of the chemical reactions they typically promote more rapidly if the catalyst has a relatively high surface area than if its counterpart has a relatively small surface area.

[0041] Tasting flakes can impart sweetness, saltiness, sourness, bitterness, or umami, and any tastings known or developed, or combinations thereof, can be used to provide such flavors. In some embodiments, the tasty flakes are acetic acid, citric acid, lactic acid, malic acid, ascorbic acid, tartaric acid, succinic acid, hydrochloric acid, sulfuric acid phosphate, sucrose, arabinose, ribose, xylose, glucose, galactose, mannose, fructose, lactose, maltose, raffinose, stachyose, sucralose, trehalose, glycerol, erythritol, arabitol, xylitol, sorbitol, mannitol, lactitol, malitol, corn syrup, aspartame, low molecular weight maltodextrin, bitter peptides, amino acids, alkaloids, amides, thiourea, polyphenols, sodium bicarbonate, sodium glutamate, disodium 5'-inosinate, and disodium 5'-guanylate, sodium chloride, sodium iodide, calcium chloride, potassium chloride, potassium iodide, or mixtures thereof; the above list is an example and non-limiting list of materials that can provide flavor.

[0042] Because this approach does not rely on the presence of taste-modulating compounds that alter the perception of the taste provided by the taste substance, the flavor flakes (which can consist of pure compounds or blends of natural taste substances) have no aftertaste. This also has the potential to increase customer compliance when seeking clean alternatives that are as close as possible to the source of natural taste substances. This would certainly be the case if the flavor flakes were made from a single ingredient (e.g., salt).

[0043] However, the flavoring substances are provided only as examples, and additional materials can be made into flakes as taught herein. Such materials are generally selected in terms of the efficacy they may provide to products containing or consisting of them, and the flakes made possible by this teaching offer improvements over conventional forms (e.g., increased efficacy (optionally, allowing for a reduction in the presence of materials required to achieve a particular effect), ease of manufacture, cost reduction, etc.). When materials contribute to or produce the chemical, physical and / or biological effects of a manufactured article, they can generally be defined as “active ingredients,” with catalysts, reinforcing materials, and pharmaceutical active ingredients being examples of such effects, respectively. However, the improvements provided by flaked materials are not limited to the chemical, physical, and / or biological effects to which they contribute, and thus also include “inert ingredients” that “simply” facilitate the manufacture of the article in any way. Inert ingredients may also be said to provide manufacturing advantages, and this term encompasses all technical aspects of processes preceding or following the manufacture. The efficacy of the active ingredients prepared in accordance with these instructions relates at least to the efficacy normally desired in the as-is or final product, but optionally includes further manufacturing advantages.

[0044] Suitable materials (active or inactive components) can be water-soluble or water-insoluble, organic (e.g., plastics or other nonpolar compounds) or inorganic (e.g., ceramics, minerals, metal-based, etc.), and can be found in a variety of chemical families useful in a wide range of industries.

[0045] For example, sodium chloride (NaCl), commonly known as table salt used in food seasonings, can also be used as a de-icing agent, reagent, and catalyst in the manufacture of chemicals. A non-exclusive list of water-soluble substances includes: ammonium nitrate (NH4NO3), which can be used in the manufacture of fertilizers, explosives, and nitric acid; and calcium carbonate (CaCO3). はIt can be used as a nutritional supplement in human and animal food, as an antacid in medicine, agriculture, and industry, as a filler in the manufacture of adhesives, sealants, paints, coatings, paper, and plastics, and in the manufacture of cement and concrete; calcium chloride (CaCl2) は In addition to its use in food processing, copper sulfate (CuSO4) can be used as a de-icing agent and in the manufacture of cement and concrete. In addition to being a catalyst, copper sulfate (MgSO4) can be used as an algaecide, fungicide, mycicide, herbicide, mollusk repellent, and root killer; magnesium sulfate (MgSO4) can be used as a fertilizer in agriculture, as a laxative in pharmaceuticals, in the manufacture of paper and textiles, and as a catalyst; manganese sulfate (MnSO4) can be used as a fertilizer, as a supplement for livestock when manganese is deficient in the soil, and also in some glazes, varnishes, ceramics, and fungicides. g. Potassium chloride (KCl) is used as a fertilizer, and potassium hydroxide (KOH) is used in the manufacture of soaps and detergents; potassium hydroxide ( ) can be used as a pH adjuster in food processing, as well as in the manufacture of soaps and detergents and biodiesel; potassium iodide (KI) can be used as a nutritional supplement, a treatment for hyperthyroidism, a drug to protect the thyroid during radiation emergencies and the use of certain radiopharmaceuticals, and as a catalyst; potassium hydroxide ( ) can be used as a pH adjuster in food processing, as well as in the manufacture of soaps and detergents and biodiesel; potassium iodide (KI) can be used as a nutritional supplement, a treatment for hyperthyroidism, a drug to protect the thyroid during radiation emergencies and the use of certain radiopharmaceuticals, and as a catalyst; potassium nitrate (KNO3) is used in food preservation, as well as in the manufacture of fertilizers and explosives. Sodium bicarbonate (NaHCO3) is used in food processing, as an antacid in pharmaceuticals, in combination with organic acids such as citric acid and tartaric acid to impart a foaming effect to the active ingredients in pharmaceuticals, and as a fire extinguishing agent; sodium hydroxide (NaOH) can be used in the manufacture of soaps and detergents, drain cleaners, and paper. Zinc chloride (ZnCl2) can be used in dry cell batteries as an electrolyte, catalyst, condensant, dehydrator, deodorant, disinfectant, and wood preservative.

[0046] Water-insoluble substances that can benefit from the methods of the present invention consist of carbonates, phosphates, sulfides, and oxides, and it is known or readily apparent that this chemical family also includes relatively soluble exceptions. For example, taking materials containing metals such as calcium as an example, calcium carbonate (CaCO3), calcium phosphate (Ca3(PO4)2) , calcium sulfate (CaSO 4) Bone meal ((Ca(PO4)2)3CaF2) and rock phosphate (Ca3(PO4)2CaF2) are widely used water-insoluble materials. Other examples include barium carbonate (BaCO3), barium sulfate (BaSO4), copper carbonate (CuCO3), iron oxide (Fe2O3), and 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).

[0047] As can be easily understood from the aforementioned non-exclusive list of exemplary materials, many are salts existing in various forms of hydrates and / or crystals, some of which have different roles, but all forms support the fact that a wide variety of industries can benefit from this teaching, and all forms are included as materials (e.g., active ingredients) that are suitable for the flakeping method of the present invention.

[0048] Regardless of the type of material that makes up the flake, if this material constitutes at least 95% by weight of the flake, the flake can be considered to be made of pure material, and the degree of purity, as assessed by weight content, is favorably 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 the material (or blend of materials) in the flake can be determined by any analytical method suitable for measuring the distinct properties (e.g., elemental composition, physicochemical properties, etc.) of the material(s) under consideration.

[0049] As already mentioned, the method is suitable for the preparation of flakes consisting of two or more types of materials. This can be advantageous when the blend materials can act additively or synergistically with other materials when in proximity and / or when the desired effects on the materials can benefit from their overall distribution being relatively uniform. For example, taking a food coated with different flakes, each flake provides a different taste (e.g., salt and pepper), but if the flakes are not distributed relatively uniformly on the surface of the food, a subject eating the food may experience different tastes in different regions (e.g., a bite) of the product. Although not essential for all products, in some cases, it can be beneficial to have flakes made of two or more materials in order to impart an even effect (e.g., a similar taste profile, aroma, color, etc.) to each part of the product (e.g., food) on which the flakes are applied or incorporated.

[0050] As a non-limiting example, when one of the materials is a flavoring agent (e.g., a salt such as sodium chloride or a sugar such as sucrose), additional materials that can be combined with it in the flakes prepared according to the present teachings can be selected from the group consisting of flavoring agents, seasonings, fragrances, spices (e.g., basil, cardamom, chili, cinnamon, coriander, cumin, garlic, ginger, nutmeg, oregano, paprika, pepper, rosemary, sage, thyme, turmeric), 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 the other material.

[0051] In some embodiments, the flakes (e.g., flavoring agents) are at least 0.001 m 2 / g, at least 0.005 m2 / g, at least 0.01 m 2 / g, at least 0.05 m 2 / g, at least 0.1 m 2 / g, at least 0.2 m 2 / g, at least 0.3 m 2 / g, at least 0.4 m 2 / g, or at least 0.5 m 2 It has a specific surface area of ​​10 m² / g. Generally, tasty flakes have a specific surface area of ​​10 m² / g. 2 It has a specific surface area not exceeding / g, and that specific surface area is usually at most 8m². 2 / g, at most 6m 2 / g, at most 4m 2 / g, or at most 2m 2 It is / g.

[0052] Therefore, in some cases, the specific surface area of ​​the flakes of the present invention is 0.001 m². 2 / g and 10m 2 Between / g, 0.01m 2 / g and 8m 2 Between / g, 0.1m 2 / g and 6m 2 Between / g, 0.2m 2 / g and 4m 2 Between / g, or 0.5m 2 / g and 2m 2 It is between / g.

[0053] For reference, a material (e.g., a taste substance) with the same density but a granular shape that can approximate a sphere and an average diameter of 50 μm would be approximately 0.2 m 2 It may have a specific surface area of ​​less than / g. The surface area of ​​a material can be routinely measured by any suitable method, such as nitrogen sorption, which can be analyzed using any suitable instrument by the Brunauer-Emmett-Teller (BET) method or the Langmuir method, and the specific surface area is calculated based on the weight of the measured sample.

[0054] (For example, flavoring and odor-masking agents) Flakes may have their bulk density (ρ) also called their apparent density, either additionally or alternatively. B ) That is, the bulk volume (V) of the unused (and therefore interparticle void volume) powder sample. B The ratio of mass to volume can be characterized as being relatively lower than the bulk density of their standard counterparts. In other words, for the same volume of flavoring particle (e.g., one tablespoon), flaking the flavoring as disclosed herein reduces the weight of the flavoring. If the flavor provided to the food is not impaired by the reduced bulk density, this allows for a corresponding reduction in the weight content of the flavoring. However, if the flavor provided by the flavoring flakes is affected by the reduction in bulk density, the reduction in the weight of the flavoring added to the food will no longer coincide with the reduction in bulk density.

[0055] In some embodiments, the bulk density of the (e.g., taster) flakes is at least 20%, at least 30%, at least 40%, or at least 50% lower than the bulk density of the standard counterpart. Taking table salt as an example, standard granular salt is generally about 1.25 g / cm³. 3の It has a bulk density, and in this case, the reduced bulk density of the tasty flakes is at most 1.00 g / cm³. 3 (1.25g / cm 3) 80% of that, at most 0.88 g / cm³ 3 At most 0.75 g / cm³ 3 , or at most 0.62 g / cm³ 3 The bulk density of the tasty flakes should be at most 0.50 g / cm³, if desired. 3 at most 0.40 g / cm³ 3 , or at most 0.30 g / cm³ 3 It can be lowered even further, but generally it does not need to be lower than 1% or even 5% of the original bulk density of the conventional taster. Therefore, in some embodiments, the bulk density of the taster flakes is 0.01 g / cm³. 3 and 1.00 g / cm³ 3 の between 0.01 g / cm 3 and 0.80 g / cm³ (3)の between, 0.05g / cm3 and 0.50 g / cm³ 3 , 0.10 g / cm³ 3 ~0.75g / cm 3 , 0.10 g / cm³ 3 ~0.70g / cm 3 , 0.05 g / cm³ 3 ~0.65g / cm 3 , or 0.20 g / cm³ 3 ~0.62 g / cm³ 3 の The apparent bulk density of particulate matter can be assessed by routine experiments using standard methods such as those described in ASTMB527.

[0056] When using flakes (e.g., flavoring and deodorizing agents) in mixture with other dry powders (e.g., other flakes), it may be advantageous for all powders to have relatively similar bulk densities in order to reduce powder separation and maintain a homogeneous mixture. Bulk densities are considered relatively similar if the bulk densities of the individual components of the mixture deviate from the bulk densities of the mixture by no more than 20%.

[0057] (For example, flavoring and odor-modifying agents) Flakes may have their tap density (ρ) added or replaced. T ) can be characterized by being relatively lower than the tap density of a standard counterpart. In contrast to bulk density, tap density measurement evaluates the packing capacity of a powder by tapping the sample to reduce the voids between particles. For a defined mass of powder, bulk density is the bulk volume V occupied by the mass of the powder. (B)を The tapping density is calculated by measurement, and the tapping volume V is normally reduced by the rearrangement of the powder during the application of tapping. (T)を It is calculated by measurement. Generally, unless the powder is completely fluid, the tap density of the powder will be higher than the bulk density, but the difference between the two values ​​depends on the intrinsic properties of the particles (size, shape, porosity, etc.), particle size distribution (homogeneity, segregation ability, etc.), interparticle interactions, and environmental factors (moisture, temperature, etc.).

[0058] In some embodiments, the tap density of the (e.g., taster) flakes is at least 20%, at least 30%, at least 40%, or at least 50% lower than the tap density of the standard counterpart, but generally does not need to be lower than 5% of the original tap density of the conventional material. Taking a taster, specifically salt, as an example, the tap density of standard granular salt is typically about 1.45 g / cm³. 3 In this case, the reduced tap density of the flavoring flakes is at most 1.16 g / cm³. 3 (1.45 g / cm³) 3 80% of that, with a maximum of 1.02 g / cm³ 3 The maximum is 0.87 g / cm³. 3 , or at most 0.73 g / cm³ 3 The tap density of Tasting Flakes is up to 0.50 g / cm³. 3 , max. 0.40g / cm 3 , or up to 0.30 g / cm³ 3 While it can be further reduced as desired, it is generally not necessary to reduce it below 5% of the original tap density of the conventional taster. Therefore, in some embodiments, the tap density of the taster flakes is 0.07 g / cm³. 3 ~1.02 g / cm³ 3 , 0.07 g / cm³ 3 ~0.87 g / cm³ 3 , 0.10 g / cm³ 3 ~0.73g / cm 3 , 0.07 g / cm³ 3 ~0.50g / cm 3 , or 0.20 g / cm³ 3 ~0.73g / cm 3 の It is in between.

[0059] The relatively low bulk density and / or tap density that the taster flakes of the present invention can exhibit is considered advantageous, particularly when the taster is applied to the surface of dry snack foods such as chips or nuts. In the case of such foods, conventionally applied tasters generally suffer relatively high losses during processing, as they peel off and fall off the food before consumption due to their relatively poor adhesion and / or relatively high tendency. Such phenomena lead to unnecessary waste of the taster.

[0060] Having flavorings formed as flakes may, in itself, increase the likelihood of sufficient contact to promote adhesion during the application of flavorings to food, compared to flavorings in a more granular form, but this is only a primary requirement. The flavoring flakes should also remain on the product during the remaining processing steps and subsequent handling of the food, such as packaging, transport, and storage. Flavorings with relatively low bulk density have been reported to be less likely to detach from food surfaces than flavorings with relatively high bulk density. This can be partially explained by the fact that particles with lower bulk density and, accordingly, smaller mass are less affected by gravity than particles with higher bulk density / larger mass, and therefore such flavoring flakes can maintain better adhesion to food until ingested.

[0061] In some cases, the dimensions of the flakes and their relatively high aspect ratio compared to conventional products result in relatively high compressibility of the particles, which can facilitate packaging, storage, or transportation. The compressibility of the flakes can be determined by calculating the dimensionless ratio between the density of the particles after compression and the density of the particles before compression. This ratio is further useful in evaluating the correlation between the aspect ratio of the flakes and their compressibility. Such factors (e.g., F5 and F6) and the measurements taken to estimate them can be determined, for example, as illustrated in Example 10 herein, which also provides a range of values ​​that can characterize the flakes of the present invention, either alone or in combination with other features.

[0062] In some embodiments, (e.g., taste) flakes may be made from water-soluble or water-insoluble materials having a crystalline structure. In such cases, the flakes may be additionally or alternatively characterized by a specific crystalline structure detectable by X-ray diffraction (XRD), depending on the material, the XRD-detectable structure may be selected from the group consisting of the position of the diffraction peak, the ratio between any two diffraction peaks at one particular position, the diffraction peak width, the crystallite size, the minute strain value, and the dislocation density at any particular diffraction peak or across the scanning spectrum, and similar parameters indicating the crystalline structure.

[0063] In some embodiments, at least one of the aforementioned crystallographic parameters measurable by XRD or other suitable method on (e.g., tasten) flakes deviates by at least 20% compared to the same parameter measured in a reference (e.g., unflaked or alternatively prepared) crystalline material. In some cases, the parameter values ​​measured on the flakes may diverge by at least 20% lower or at least 20% higher than the same parameter measured in a standard grown / prepared crystal. In some embodiments, at least one of these crystallographic parameters measurable on the flakes diverges by at least 30%, at least 40%, or at least 50% compared to the corresponding parameter in a reference standard crystal without flakes. For some crystallographic parameters, the difference between measurements made on the flakes and measurements made on the reference crystal can be at least 2x, at least 3x, or even at least 4x.

[0064] For example, the relatively high compression perceived during crystal growth, and the compression and aggregation of precipitates due to passing through the nip, can be observed in crystallite size and minute strain values, which can be at least twice as large or twice as large in tasty flakes made from the salt compared to standard salts.

[0065] The XRD structure detectable in the original, unflaked material (e.g., a flavoring substance) before processing according to this method and / or using an apparatus as taught herein can be referred to as the first XRD-detectable structure, while the corresponding structure detectable in the prepared flakes (e.g., a flavoring substance) can be referred to as the second XRD-detectable structure. Since it is understood that changes in the crystalline structure of crystalline materials, which may occur in some embodiments, can themselves cause minute shifts in diffraction peaks, the structures of the original material (e.g., unflaked) and the flaked version are considered corresponding if they relate to similar parameters analyzed along similar positions or similar spectral spans. Thus, the corresponding structures do not need to be identical, but the parameters claimed should be of essentially the same kind.

[0066] In the foregoing, (for example, flavoring agent) flakes were characterized by one parameter at a time, such as i) their thickness, ii) their length, iii) their aspect ratio, iv) their specific surface area, v) their bulk density, their tap density, or any ratio between the two densities, or vi) if crystalline, any crystallographic specifications suitable for the material. However, those skilled in the art will readily understand that flakes, such as those that can be produced by the present method, can be characterized by any combination of two or more of these parameters. For illustrative purposes, taster flakes may have both the bulk density and crystallographic behavior disclosed herein. In some embodiments, taster flakes exhibiting the aforementioned characteristic parameters may further be produced from pure taster (e.g., constituting 95% by weight or more of the flakes).

[0067] For example, the tasty flakes produced according to this instruction are a) made from pure salt containing, for example, more than 95% by weight of sodium chloride; and b) 0.60 g / cm³. 3 , optionally up to 0.55 g / cm³ 3 , max. 0.50g / cm 3, maximum 0.45 g / cm 3 , maximum 0.40 g / cm 3 , maximum 0.35 g / cm 3 , maximum 0.30 g / cm 3 , maximum 0.25 g / cm 3 , at most 0.20 g / cm 3 , at most 0.15 g / cm 3 , or at most 0.10 g / cm 3 ; and c) i) 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) at most 1,000 Å (angstrom), at most 750 Å, at most 625 Å, or at most 500 Å crystallite size.

[0068] In this specification, when the term salt is used to refer to sodium chloride, the raw materials that can be used in the preparation of salt flakes include all available salt sources, whether they are naturally available salts (e.g., sea salt, ocean salt, mineral salt, etc.) or further processed salts (e.g., smoked salt, flavored salt, supplemented salts such as iodized salt, etc.), and the flakes produced therefrom can have a similar designation.

[0069] The flakes of the present invention can be characterized by additional features, as a result of which the relationship between two or more structural features can be calculated. The aspect ratio of the flakes is an example of a method in which the ratio between two measurable features (the longest planar dimension and the thickness) can provide complementary valuable and characteristic information. Alternative or additional calculated ratios are exemplified by coefficients F1 to F6 as described in Examples 7, 9 and 10.

[0070] For the sake of brevity, only the mathematical expressions of the foregoing exemplary factors are incorporated into the following paragraphs. F1 is the ratio of the aspect ratio ASP of the flakes to their dissolution rate (DT), and can be mathematically expressed as F1 = ASP / DT (the unit is seconds -1 ). F2 is the tapped density ρ T of the flakes and the bulk density ρ(B)の is a ratio without units between them, which can be mathematically expressed as F2 = ρ T / ρ B and can be expressed as such. F3 is the aspect ratio ASP of the flakes and the bulk density ρ (B)の ratio, which can be mathematically expressed as F3 = ASP / ρ B (the unit is cubic centimeters per gram) and can be expressed as such. F4 is the aspect ratio ASP of the flakes and the tap density ρ (T)の ratio, and F4 = ASP / ρ T (the unit is cubic centimeters per gram) and can be mathematically expressed as such. F5 is the ratio between the compression density ρ C and the initial bulk density ρ B of the flakes before compression, and F5 = ρ C / ρ B and can be mathematically expressed as such. F六亲は、フレークのアスペクト比ASPとF5によって推定される圧縮性との比であり、F6 = ASP / F5によって数学的に表すことができる。Regarding measurable characteristics, the factors of the present invention, among themselves and / or in combination with the measured characteristics (e.g., i) thickness t, ii) longest planar 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.), can characterize and distinguish the flakes of the present invention.

[0071] For the sake of explanation, the flakes of the present invention can have at least two, at least three, at least four, or at least five of the following characteristics, and these are exemplified in this paragraph by only one of the various limitations that each can satisfy as set forth in detail below in this specification for the sake of brevity: 1) an average thickness t not exceeding 200 μm; 2) an aspect ratio ASP of at least 10; 3) an F1 coefficient of at least 5; 4) an F2 coefficient of at least 1.25; 5) an F3 coefficient of at least 25; 6) an F4 coefficient of at least 20; 7) an F5 coefficient of at least 1.6; and 8) an F6 coefficient of at least 6.

[0072] In some embodiments, two or more features characterizing the flakes of the present invention include any of the above-listed items 1) and 2), 2) and 3), 2) and 4), 2) and 5), 2) and 6), 2) and 7), as well as 2) and 8), and their respective limitations as described herein. In some embodiments, three or more features include, to give some combinations, any of the above-listed items 1), 2) and 3); 2), 3) and 4); 3), 4) and 5); 3), 5) and 7); 3), 5) and 8), and their respective limitations as described herein. In some embodiments, four or more features include, to give some combinations, any of 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), and their respective limitations as described herein.

[0073] Another aspect of this disclosure provides a method for producing flakes (e.g., flavor flakes), the method including: a) A process of providing a liquid stock comprising at least one solid material dissolved or dispersed in a liquid. b) The step of applying the liquid stock to the first movable surface so as to form a thin film of liquid stock. c) Cyclically i) A step of removing at least a portion of the liquid from a thin film of liquid stock to increase the concentration of solid particles in the thin film, and ii) Apply pressure to the film by passing it through at least one nip formed by biasing opposing nip-forming surfaces toward each other, thereby gradually forming a layer containing flakes made of compressed and / or aggregated solid particles. The cycle is repeated until the flakes contain less than 5% by weight of liquid.

[0074] The flakes produced by the above method may have an average thickness t of up to 200 μm, not exceeding the thickness of the layer, and in a further embodiment, may have an average aspect ratio ASP between at least 10 longest planar dimensions L and the thickness t of the (e.g., taster) flakes.

[0075] The values ​​described in the above introduction to this method are illustrative and may be replaced in this specification by any additional values ​​relating to the features monitored to determine the end of the flakening method.

[0076] As used herein, the layer in which the flakes are ultimately formed does not have to be a continuous layer, but can refer to discrete clusters of otherwise scattered particles that can be aggregated and held together by any suitable force. While we do not wish to be bound to any particular theory, in this method, it is conceivable that particles of solid material that gradually separate from the liquid stock as the liquid is removed can be aggregated by pressure agglomeration, partial sintering or fusion, and / or accumulation crystallization, depending on the material considered.

[0077] Since aggregation does not require a clear pattern for particles to gather into a solid mass, such aggregates can take on any shape and size if they form spontaneously. Because the solid particles in this method aggregate under periodic compression, the minimum thickness of the layer, once substantially dry (e.g., containing less than 5 wt.% liquid), can be predetermined (e.g., empirically) according to the size of the solid particles that may be present in or gradually separated from the liquid stock, their hardness, and the forces they experience at the nip(s). Since flakes can be considered part of the layer that initially constitutes them, separated gradually or at the end from adjacent flakes and / or the underlying surface, they can also be considered aggregates of solid particles. Because the process also involves compression, the particles forming the flakes (or the layers from which they separate) can be described as agglomerating and compressing, or vice versa, and both effects likely occur simultaneously, with their order in any particular sentence not signifying any particular order of events concerning the particles. As is easily understood, a layer consisting of flakes made up of aggregated and compressed particles does not have to be the thickness of a single particle, and the number of particle layers can be stacked one by one depending on the material and operating conditions. Taking crystals of a solid material that can be gradually separated from a liquid stock as an example, the aggregated layer of crystals can be formed from multiple crystals adjacent to each other in all three dimensions.

[0078] Two cylinders biased to contact (e.g., by a pneumatic or hydraulic piston, the latter optionally including an accumulator which may be a spring-loaded or gas-loaded accumulator to compensate for the lack of compressibility of the hydraulic fluid in order to provide the piston with some spring-like behavior) are at an essentially null distance (e.g., less than 1 μm) from the other when no material is supplied to the nip, but it is understood that this distance may increase when material is present. The extent of the actual distance between the two cylinders in the nip portion may depend on the volume and / or size of the supplied material, its concentration, rotational speed, the pressure applied to achieve contact, the time elapsed since the initial application, and similar factors. In some embodiments, the initial gap in the nip formed between two rotating cylinders when the material to be flaked is applied can be up to 400 μm, up to 300 μm, up to 200 μm, up to 100 μm, up to 80 μm, up to 60 μm, up to 40 μm, up to 20 μm, up to 10 μm, or up to 5 μm, and this distance is required to gradually decrease as the liquid is removed while the cylinders are encouraged to come into contact in the presence of the material to be flaked (for example, as the concentration of solid particles increases, allowing the aggregation and compression of the particles to become flaky).

[0079] The dynamic adjustment of the nip gap dimensions, depending on process conditions and the degree of completion of each step or cycle, occurs naturally as the flakes progress, and no dedicated device is used to directly and controllably adjust the nip spacing (e.g., by fixing cylinders at a predetermined distance from each other). Thus, the periodic closing of the gap as the liquid stock material is flakened (and the liquid is removed) and the widening of the gap as new liquid stock is presented to the nip is considered a spontaneous, spring-like process. The gap in the nip or between the opposing nip-forming surfaces in the nip can be called "dynamic" to reflect this continuous phenomenon.

[0080] If a hydraulic system is employed to bring the cylinders into contact, it may include an accumulator to provide desired spacing variations in the absence or presence of material to be thinned. At the start of the process, rotating cylinders that are temporarily separated by less than 400 μm at the nip are considered to have been prompted to come into contact with each other, even if the "contact" is mediated by the presence of material or liquid stock between them.

[0081] The dried flakes obtained from such initial nip gaps are thin, typically having a thickness at best corresponding to the solid content of the liquid stock being applied, and sometimes even thinner. For example, considering a stock consisting of 25% by weight sodium chloride, under operating conditions where the initial gap between cylinders encouraged to contact at the nip is 400 μm, the resulting flakes will have a maximum thickness of approximately 100 μm.

[0082] In some embodiments, the recycling of the material, which is gradually thinned into recoverable flakes, is performed in the same nip from which the material was initially supplied. In other embodiments, recycling may be performed in one or more nips different from the nip from which the material was initially supplied, and these may be referred to as the first nip. In the case of multiple nips, each nip may consist of a pair of cylinders that do not come into contact with any of the cylinders of the other nips, although in some embodiments it is preferable for multiple nips to share a common cylinder. The rotating cylinders of each nip, and the rotating cylinders of different nips, do not necessarily have to be the same. For efficiency, they generally have similar axial lengths but may have different diameters and / or be made of different materials and / or be coated with different materials and / or be heated or cooled to different temperatures, etc.

[0083] In one embodiment, the material (e.g., a flavoring substance) is provided in the form of dry microparticles. This method is suitable for any flavoring substance that exists in a dry form (e.g., plant spices derived from roots, stems, bark, leaves, flowers, or seeds), but is particularly applicable to flavoring substances that cannot be dispersed or dissolved in a medium that can be relatively easily and efficiently isolated. This “dry method” typically allows for the thinning of the reagent by at least 5 to 1 / 2 times from the initial dimensions (e.g., diameter, edges, thickness) to the final thickness, followed by final reuse of the thinned reagent via a nip. This method is generally suitable for the preparation of microflakes.

[0084] In one embodiment, the material (e.g., a flavoring agent) is provided as a relatively viscous paste (e.g., having a dynamic viscosity greater than 5,000 millipascal seconds (mPa·s) at room temperature around 23°C). The viscosity of the paste can be achieved by dispersing a relatively large amount of flavoring substance in a relatively small amount of liquid and / or by using a liquid that is relatively viscous in itself. The dispersion medium should preferably be compatible with the material to be flaked (e.g., not affecting the taste of the flavoring agent) and, if necessary or desired, should be separable from it. The dispersion medium may be relatively viscous in itself but can be selected according to the future use of the flakes (e.g., flavoring agent). For example, the taster is cocoa, and the viscous medium can be cocoa butter (both water-insoluble) or sugar and molasses (both water-soluble), and at least one of the rotating cylinders is optionally heated or cooled to maintain the desired viscosity of the paste. This example is non-limiting, and the dispersion (e.g., viscous) medium does not have to be from the same source or of the same kind as the flavoring substance. This “paste method” typically allows for diluting the flavoring substance at least tenfold, from its initial dimensions (before forming the paste) to its final thickness, followed by the reuse of the diluted flavoring substance through the nip. This method is generally suitable for the preparation of microflakes and submicroflakes.

[0085] A dispersion medium adapted to form a relatively viscous paste with the materials can be an inherently viscous product, such as honey for flavoring, or prepared by increasing the viscosity of a non-viscous liquid. Such an increase in viscosity, which allows the paste to exhibit a dynamic viscosity of at least 5,000 mPa·s at room temperature, can be achieved by using a relatively large amount of material (e.g., a flavoring) and / or by incorporating a thickener into the dispersion medium. If the material to be flaked is intended to provide flavor or be used in a product to be consumed, the thickener should preferably be tasteless itself and, advantageously, should be edible to the extent that the residue is not removed from the surface of the flavoring flakes, although this is not necessarily required. Such thickeners may be natural or synthetic, are well known, and can be selected from the group consisting of alginic acid (E400), sodium alginate (E401), potassium alginate (E402), ammonium alginate (E403), calcium alginate (E404), propylene glycol alginate (E405), agar (E406), carrageenan (E407), furceran (E408), locust bean gum (E410), oat gum (E411), guar gum (E412), tragacanth (E413), Gum arabic (E414), xanthan gum (E415), karaya gum (E416), tara gum (E417), gellan gum (E418), pectin (E440), gelatin (E441), cellulose (E460), methylcellulose (E461), ethylcellulose (E462), hydroxypropylcellulose (E463), hydroxypropylmethylcellulose (E464), methylethylcellulose (E465), carboxymethylcellulose (E466), natural or modified starches (E1400 series), and combinations thereof.

[0086] In one embodiment, the material (e.g., a flavoring agent) is provided dispersed or dissolved in a relatively non-viscous liquid (e.g., water) having a dynamic viscosity of 1,000 mPa·s or less, 100 mPa·s or less, or 10 mPa·s or less at room temperature. This liquid must be compatible with the material (e.g., not affecting its taste in the case of a flavoring agent) and, if necessary or desired, separable from it. Tasting agents suitable for such a method are generally soluble in the liquid even when supplied at concentrations higher than their solubility limit, although not necessarily so, and the tasting agent is dispersed in the liquid accordingly rather than completely dissolved. This “liquid method” typically allows for dilution by at least 15 times from the initial dimensions (before mixing in the liquid) to the final thickness, after which the diluted tasting agent is finally reused through a nip. This method is generally suitable for the preparation of microflakes, submicroflakes, and nanoflakes.

[0087] As mentioned above, the selection of liquid carriers, their additives, and substances

[0088] As stated above, it is emphasized that, with respect to any material to be flaked by this method and / or the apparatus described herein, the selection of the liquid carrier, its additives, and which parts of the apparatus are made or coated is guided by the principle of compatibility. Materials should be chemically compatible with one another. Basically, a material or chemical composition is compatible with another (or, if desired, inert with respect to it) if it does not interfere with its activity or reduce it to an extent that significantly affects its intended purpose. For example, a liquid carrier is incompatible if it affects the taste of a material that is a flavoring agent intended for consumption, or if it affects the potency or reactivity of a material intended for a manufacturing process. Materials must also be physically compatible with one another. For example, a liquid carrier should preferably be sufficiently volatile at a temperature that does not affect the material being flaked. Thus, materials must also be compatible with the manufacturing method and its operating conditions, and vice versa. For example, the liquid stock in which the material to be flaked is dissolved or dispersed should not be corrosive to the surface to which it is applied, or the surface should be inert to the stock and the flakes produced therefrom. Such general considerations are known to those skilled in the art of chemical manufacturing and will not be elaborated further herein.

[0089] However, in some embodiments, the liquid may be selected to intentionally induce a reaction with the material being flaked. In such cases, the chemical composition of the material before and after flaking may differ. Therefore, the term “flakes produced from the material” encompasses both flakes that retain the original chemical composition of the material treated by the flaking method of the present invention, and flakes that include improved versions of the material. For example, if calcium carbonate is flaked with neutral water, the resulting flakes will consist of calcium carbonate. However, if calcium carbonate is flaked with acetic acid, the resulting flakes may consist of calcium acetate, and water and carbon dioxide will also be produced by the reaction of the carbonate with acetic acid.

[0090] Regardless of the form in which the material (e.g., flavoring agent) is supplied to one or both sides forming a particular nip (e.g., in a dry form, paste form, or dissolved or dispersed in a liquid), its application can be continuous or intermittent.

[0091] In a particular embodiment, considering the production of flakes from a material supplied dispersed or dissolved in a non-viscous liquid, in one embodiment, this method comprises the following steps: a) A step of supplying at least one material (e.g., a flavoring agent or any other active or inactive component) dispersed or dissolved in a liquid to form a liquid stock (e.g., a flavoring agent); b) The process of applying a liquid (e.g., taster(pl)) stock to a movable surface so as to form a thin film of the liquid (e.g., taster(pl)) stock. c) a step of removing at least a portion of the liquid from a thin film of liquid (e.g., taster(s)) stock to form a thin film of solid particles (e.g., precipitated taster(s)), wherein the thin film optionally has a thickness of 400 μm or less; and d) The particles of the thin coating are aggregated and compressed to obtain substantially dry flakes (e.g., containing less than 5 wt.% liquid, optionally with a thickness of 200 μm or less and an average aspect ratio of at least 10:1 between the longest planar dimension and the thickness).

[0092] Theoretically, liquid stock can be applied at any initial thickness, although a relatively thick film is expected to require a longer processing time than a relatively thin film under other similar conditions. However, in some embodiments, the liquid stock has a thin film with an initial thickness of 400 μm or less, 325 μm or less, or 250 μm or less, and the material(s) are preferably homogeneously dispersed or dissolved (or both) in the liquid at the time of application. A liquid stock in which the material to be flaked is dissolved can also be called a stock solution. A liquid stock in which the material to be flaked is dispersed can also be called a stock dispersion.

[0093] For similar reasons, theoretically, liquid stocks can be applied to any initial concentration of the material, but otherwise, it may be advantageous to use a relatively high concentration, which is expected to require a shorter processing time than a relatively dilute stock under similar conditions. It should be understood that a relatively high proportion of material in the liquid can affect its viscosity. Therefore, it is emphasized that while the liquid carrier used to form the liquid stock may itself be nonviscous (e.g., having a dynamic viscosity of less than 1,000 mPa.s), the liquid stock may conversely be slightly viscous. Thus, while the liquid stock may also be nonviscous, in some embodiments, the liquid stock may have a dynamic viscosity of up to 5,000 mPa.s, up to 4,000 mPa.s, up to 3,000 mPa.s, up to 2,000 mPa.s, up to 1,500 mPa.s, or up to 1,250 mPa.s, measured at room temperature. As anyone skilled in evaluating the rheological properties of materials will understand, the dynamic viscosity of a liquid stock can also depend on the probe of the instrument used for analysis, and, if operating in continuous rotation, its frequency and / or shear rate. These parameters need to be adjusted according to the behavior of the substance being tested; typically, the oscillation frequency used for more viscous materials is in the range of 0.1–100 Hz, while the shear rate for relatively less viscous products is 1–1,000 s. (-1)の For more viscous paste-like products, the shear rate is typically around 1-100 seconds. -1Screen for an appropriate setting within the range. The viscosity values ​​reported herein can be measured within the aforementioned operating range suitable for the measurement using an appropriate rheometer, its components, and operating conditions. In some embodiments, the dynamic viscosity (e.g., of a liquid carrier or a liquid stock prepared therefrom) is approximately 10 to 250 s. -1 The range is approximately 50-150 seconds. -1 It is determined by the shear rate within the specified range.

[0094] In some cases, it may be desirable to pre-treat the liquid stock and / or its components before applying it to the target nip-forming surface. Pre-treatment can be at least one of the following: a) reducing the size of the particles of the material to be dispersed, b) heating the liquid to promote the dissolution or dispersion of the material, c) homogenizing the stock dispersion, and d) heating the liquid stock before application. From an apparatus standpoint, an apparatus configured to provide such pre-treatment can be called a pre-treatment station.

[0095] In some embodiments, the surface to which the liquid stock is applied is wettable by the liquid stock, and the liquid can spread uniformly on the surface.

[0096] In some embodiments, a thin film of liquid stock (e.g., a taster) is obtained by intermittently or continuously applying the liquid stock to a surface (e.g., a wetting surface) which is movable, and in particular by passing the applied stock through a nip formed by biasing a movable surface and an opposing surface to contact each other. The portions of the movable surface and the opposing surface that face each other in the nip formed between them can also be called the nip-forming surface. When both opposing surfaces are in motion, for example, when the nip is formed on the contact line between opposing rotating cylinders, all portions of the outer surface of the cylinders may periodically (cyclically) constitute the nip-forming surface.

[0097] An applicator of a liquid stock of a material(s) functioning as a dispensing device and a first movable surface typically move relative to each other. As used herein, the terms “tastant(s) stock,” “liquid stock,” “tastant(s) liquid stock,” or even “stock” may be used interchangeably to refer to a liquid containing a dispersed or dissolved material (e.g., tastant(s)). The liquid carrier of the stock may consist of one or more fluids (and optionally additives therein), the liquid carrier being relatively non-viscous (i.e., having a dynamic viscosity of less than 1,000 mPa·s at room temperature), and the liquid stock therefore having a viscosity not exceeding 5,000 mPa·s when applied to a movable surface.

[0098] In some embodiments, compression of a thin film of precipitated material(s) is achieved by passing the thin film through the same nip or at least one different nip used to level the liquid stock into a thin liquid film, the material(s) gradually precipitate from the liquid in the gradually drying film, and the solid particles aggregate into larger aggregates (e.g., solid particles aggregate into larger aggregates (e.g., aggregates) and the resulting (e.g., tasty) flakes are at most 200 μm. The thickness is at most 150 μm, at most 100 μm, at most 50 μm, at most 20 μm, at most 10 μm, at most 5 μm, or at most 1 μm, and the aspect ratio between the longest planar dimension of a (tasting) flake and its thickness is, on average, at least 10:1, at least 20:1, or at least 30:1 (for brevity, also called at least 10, at least 20, or at least 30). Repeated passage of a thin coating containing solid particles that gradually concentrate as the liquid evaporates eventually forms a layer of flakes, each flake consisting of aggregated and / or compressed solid particles. However, this semantic distinction can sometimes be arbitrary, as areas of the coating may be able to form flakes before they are sufficiently dry as a whole for the solid particles to be compressed into the maximum number of flakes that the process may produce.

[0099] Importantly, the spacing of the nip portions does not need to be constant throughout the flaking process. Rather, the nip may, advantageously, exhibit a dynamic spacing as the steps or cycles progress and / or are completed. The nips of the flaking method of the present invention can more preferably be considered “dynamic nips” having a spacing that is essentially variable in response to process conditions and states, but for the sake of brevity, we shall refer to them as nips.

[0100] As can be understood from the illustrative diagram above, compression of a thin liquid film and a coating of material therefrom by one or more passages through one or more dynamic nips between cylinders urged to contact can also provide a “crushing” step that converts the material precipitated in the coating and the resulting dry layer into flakes. Thus, the crushing step can arise spontaneously from the steps described above and does not require any special action. Crushing may further, or alternatively, require the active separation or destruction of the dry layer containing agglomerated particles into separate flakes of agglomerated precipitates by periodic compression. Crushing or destroying a coating or dry layer containing little to no liquid (e.g., less than 5 wt.%) into flakes of compressed solid particles typically involves the spontaneous detachment of flakes from a thin coating and / or the assisted detachment of a layer consisting of flakes from a movable surface, and the inherent or forced destruction of the relatively dry layer into individual flakes. Since the formation of flakes involves different mechanisms, each of which can be considered as separation from the underlying surface or material, or separation from adjacent portions of the coating that transforms into flakes, the thin coating of precipitated solid particles and the layer to which the majority is aggregated and compressed can be considered to be separable into flakes or to be composed of flakes.

[0101] For efficiency, the material (e.g., a flavoring substance) can be provided with dimensions that facilitate dispersion or dissolution in the liquid, for example, by grinding to have a maximum dimension not exceeding 5 mm (e.g., if the material is soluble and the size reduction is intended to promote dissolution), or to other sizes as desired as a pretreatment for the preparation of the liquid stock to be applied (e.g., if the material is insoluble in the liquid, the size of the material can be reduced to 10 μm or less, 7.5 μm or less, or 5 μm or less, such size reduction is intended to facilitate the initial passage of the dispersion through the nip). Pretreatment of the raw material by grinding can be carried out with standard equipment such as a coffee grinder, mortar and pestle, hammer mill, ball mill, or jet mill. Similarly, the liquid stock can be pretreated before application to the nip with any equipment suitable for the required pretreatment (e.g., a heater for heating the liquid, a sonicator for promoting dissolution, etc.). Alternatively, the equipment for carrying out this method can be modified to allow in-line pretreatment of the material to be flaked.

[0102] If the material is soluble in the stock liquid carrier, the process can be accelerated, either alternatively or additionally, by using a saturated or near-saturated solution. A saturated solution is one in which there is so much solute that any more will not dissolve and will precipitate out of the solution as a solid, for example. The maximum amount of any material (e.g., a flavoring substance) in a saturated solution depends, in particular, on the material, its initial specific surface area, the liquid in which it is dissolved, the temperature of the solution, the pressure applied to it, and other conditions that maintain a uniform concentration of the material in the solution (e.g., stirring). Thus, a solution that can be saturated at a relatively high temperature, for example, may become supersaturated (containing a larger amount of soluble substance than expected) at a relatively low temperature. A near-saturated solution consists of less than the maximum amount of substance that can dissolve under the conditions set for the preparation of the solution. Such an amount (e.g., 70% to 90% of the maximum amount) may be sufficient to saturate the solution under different conditions to which a near-saturated solution may be exposed during the process of preparing the flakes.

[0103] In other words, a solution can be prepared to be nearly saturated, saturated, or supersaturated at the time of its preparation, but such classifications can evolve during the process. For example, a nearly saturated solution may become saturated as liquid is removed from it, and it may even turn into a dispersion as the material (e.g., a flavoring substance) begins to precipitate out of the solution (e.g., by crystallization of the material). In this context, the presence of a soluble material dispersed in a liquid indicates that the material is present at a concentration higher than the concentration allowed for the formation of a supersaturated solution. Alternatively, the material may be dispersed in a liquid in which it does not dissolve. For example, a substance that dissolves in water does not need to dissolve in alcohol.

[0104] As used herein, the terms “precipitate,” “sequester,” and their grammatical variations are not used exclusively to refer to processes that result in the formation of a permanently insoluble substance in the liquid from which it precipitates. Conversely, these terms also include processes in which an insoluble substance is concentrated or formed to such an extent that it can be separated from the liquid as a solid. Thus, a substance precipitated from a liquid may have previously been dissolved or dispersed within it. Crystallization is a specific precipitation process in which the structure of a substance that has lost its solubility and become solid is organized. Certain crystalline substances (e.g., taste substances) can have numerous polymorphs, all of which are encompassed herein.

[0105] In some embodiments, the dispersion or dissolution of a material (e.g., a flavoring agent) in a liquid is carried out at a temperature above room temperature, and this temperature does not exceed the boiling point of the liquid. Considering water as an exemplary liquid, the dispersion or dissolution step can be carried out at temperatures of at least 30°C, at least 40°C, or at least 50°C, and at most 95°C, at most 90°C, or at most 85°C. If the liquid is an alcohol or contains a sufficient amount of alcohol or other substances having a lower boiling point than water, the upper limit of the aforementioned range should be reduced in proportion to the relative proportion of such volatile liquids in the liquid, and the dispersion or dissolution step should be carried out at temperatures between, for example, 30°C and 75°C. The temperature that should not be exceeded during this step should also take into consideration the heat resistance of the material (in the case of multiple materials, the heat resistance of the most sensitive material), and, in the case of a flavoring agent, preferably, it should be lower than the temperature at which the taste of the flavoring agent is detected to be impaired as determined by sensory evaluation.

[0106] Regardless of the temperature at which the dispersion or dissolution step may be performed, it may also be performed at a pressure other than ambient atmospheric pressure. Furthermore, regardless of temperature and / or pressure conditions, the dispersion or dissolution step may be performed under continuous stirring of the liquid while dispersing or dissolving the material therein and / or maintaining the homogeneity of the liquid stock for the formation of a continuous film (i.e., during application to a surface). Regardless of the conditions selected for the preparation of the liquid stock, the liquid stock may be applied to a movable surface at a temperature higher than the ambient temperature. This may occur particularly if the surface itself is heated to the same or a different temperature as the ambient temperature.

[0107] In some embodiments, the removal of at least a portion of the liquid from a liquid stock (e.g., a flavoring agent) that forms a thin, continuous film on a surface is carried out rapidly. While we do not wish to be bound by any particular theory, it is conceivable that, if rapid enough, the removal of the liquid (e.g., evaporation) can occur while the material (e.g., taster) is still relatively homogeneously dispersed or dissolved in the thin film. Rapid removal of the liquid at such a stage allows for the formation of a relatively homogeneous film of the precipitated material (e.g., taster or any other solid particles), which may facilitate the compression of the film (by solid aggregation) and its fragmentation into flakes having a relatively uniform thickness. The liquid film, dry film, collection of flakes, or nanoflakes have a relatively uniform thickness if the ratio between their respective maximum and minimum thicknesses, or between their respective maximum and minimum average thicknesses, is 10 or less, 8 or less, 6 or less, 5 or less, 4 or less, 3 or less, or 2 or less.

[0108] Advantageously, the liquid removal rate in this method is such that the formation of a film of the precipitated material (e.g., a flavoring substance) can occur in less than one minute from the time a thin film of the liquid stock (e.g., the flavoring substance) is formed. In some embodiments, the liquid removal step is performed for 50 seconds or less, 40 seconds or less, or 30 seconds or less. If the liquid removal method alternatively or further includes heating the surface coated with the liquid stock to form a thin film, the liquid removal step may also be called an accelerated evaporation step. In some specific embodiments, the liquid removal or evaporation step requires 20 seconds or less, 15 seconds or less, or 10 seconds or less. The liquid removal or evaporation step can be performed while blowing away or suctioning at least a portion of the liquid or its vapor being removed.

[0109] Any liquid can be used based on its ability to sufficiently dissolve or disperse materials and the relative ease of removal for process efficiency, but selecting a liquid that is also approved for consumption by animals (e.g., humans) may be advantageous in the case of flavoring agents or materials ingested by living subjects. Such liquids are well known and do not need to be described in detail, but for illustrative purposes, they can be selected from the group consisting of water, alcohols, fatty alcohols, glycerol (also called glycerin), propylene glycol, and combinations thereof. If the water-soluble material is not a flavoring agent or is used for ingestion by animals (e.g., nutritional supplements, medicines, etc.), the liquid can be selected from an even broader range of liquids, and nevertheless, the intended use of flake materials may also be considered. For example, if flakes are used in a manufacturing process, the liquid may be suitable for the process (e.g., not inhibiting the intended reaction).

[0110] Advantageously, though not strictly necessary, the liquid selected for the preparation of the liquid stock, whether pure or blended, should be able to dissolve the material (e.g., the material) to a concentration of at least 1 g (1 wt.%) per 100 g of liquid, or at least 5 g (5 wt.%) per 100 g of liquid, at least 10 g (10 wt.%) per 100 g of liquid, or at least 20 g (20 wt.%) per 100 g of liquid, so that it can be measured at room temperature. The liquid should preferably be selected to suit the intended use of the material, to the extent that the flakes may retain residual liquid on their outer surface, and for flavorings, for example, should not exceed a content considered toxic to consumption. In other words, the liquid should preferably be labeled with a Generally Recognized as Safe (GRAS), Food Grade, and / or any other similar indication that it is suitable for oral ingestion where the material is intended to be ingested.

[0111] Alternatively, the liquid, whether pure or blended, should only allow for the dispersion of the material (e.g., flavoring and odor-masking agents), in other words, the material should dissolve at a concentration of less than 1 g (<1 wt.%) per 100 g of dispersion.

[0112] In some embodiments, the movable surface (e.g., wettable by the liquid stock) is the surface of a rotating cylinder. In such cases, assuming a single nip, the liquid removal step, configured to remove at least a portion of the dissolve or dispersion, may preferably occur within 60 cycles or less of the rotating cylinder, and the number of cycles required to allow sufficient removal of at least a portion of the liquid depends on the initial concentration of the material (e.g., flavoring agent) in the liquid, the rotational speed of the cylinder, the temperature of the cylinder surface, the number of nips positioned along the rotating cylinder, and similar factors. In some embodiments, the liquid removal or evaporation step requires 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 requires 8 cycles or less, 6 cycles or less, 4 cycles or less, or 2 cycles or less, ideally 1 cycle or less.

[0113] To avoid misunderstanding, it should be emphasized that the typical gradual removal of liquid from the stock liquid film does not need to be complete for the material(s) to begin precipitation. Consequently, the compression and fragmentation of the precipitated material(s) film into flakes can also begin before complete liquid removal, which may follow one or more cycles of compression. In other words, the removal of the first portion of liquid may cause the precipitation of the first portion of solid particles, and while this first portion is compressed (e.g., leading to particle aggregation), the removal of the second portion of liquid may cause the precipitation of the second portion of solid particles of the material(s). Thus, the steps of coating the liquid stock, partial liquid removal to partial precipitation, and compression leading to partial fragmentation of the precipitated material(s) into flakes are sequentially correct, but the subsequent steps do not require the complete completion of the previous step to begin, and some steps can coexist with different parts of the film: the liquid stock, the precipitated film, and the layer of compressed aggregated particles from which it is compressed. Based on the same rationality of the process that allows for the simultaneous coexistence of various phases, if all steps are ideally carried out in one cycle through the nip, then it can be understood that different sections of a movable surface (e.g., a rotatable cylinder) may exhibit relative enrichment in the products of the various phases.

[0114] If the outer surface of a rotatable cylinder is the surface having a thin coating of precipitated material (e.g., a flavoring agent) and a coating of liquid stock that changes into a layer of flakes, then particle compression can be performed in the nip between the rotating cylinder and an opposing surface that is brought into contact with each other by a force mechanism through a passage passing through the nip. In this case, the surface coated with the precipitated material and the counter surface move relative to each other. The opposing surface may be movable and may be, for example, a second rotating cylinder. In this case, the two surfaces can enter the nip at the same or different speeds, and the two cylinders rotate in the same direction or, more generally, in opposite directions.

[0115] The nip (e.g., formed between two rotating cylinders urged to contact) is described as providing confinement of a thin film of liquid stock, compression of a film of precipitated material (e.g., flavoring agent), and optionally fragmentation of the film into flakes, although this may not be its only role in this method. While we do not wish to be bound by any particular theory, it is thought that the pressure applied to the film of liquid stock at the nip contributes to removing at least some of the liquid from the film, even at ambient temperature, without further heating of the cylinder surface. Regardless of the possible mechanisms of action relating to a limited volume of liquid stock, a thinned film, a film of precipitated material, and / or flakes fragmented therefrom, it is thought that controlling the nip (e.g., by operating parameters such as speed, temperature, and contact pressure) is important, in particular, as it may determine some properties (e.g., size, morphology, etc.) of the flakes (e.g., flavoring agent) produced therefrom and / or the effectiveness of the process (e.g., production rate).

[0116] In some embodiments, the pressure applied to the nip is at least 10 MPa, at least 50 MPa, or at least 100 MPa. Typically, the pressure applied to the ideal contact line between the surfaces involved in one or more nips in this method is not greater than 1,500 MPa, may not exceed 1,250 MPa, or may not exceed 1,000 MPa. When multiple nips are used in this method, the pressure applied to the first nip does not need to be the same as the pressure applied to the other nips. This is the case when a series of nips are formed radially around a common central cylinder, and each external rotating cylinder is biased to contact them at a different pressure. In some embodiments, the pressure applied to each nip can be independently between 10 MPa and 1,500 MPa, between 50 MPa and 1,250 MPa, or between 100 MPa and 1,000 MPa. The aforementioned pressures are values ​​of the maximum Hertz contact pressure calculated based on the force that can be applied to bring the various nip-forming surfaces into contact.

[0117] The force / pressure applied to prompt the surfaces of the method / apparatus to come into contact in order to form at least one nip does not need to be constant while performing any of the steps disclosed herein. For example, taking a material (e.g., a flavoring agent) that is fed as a dry powder into a single nip and then flaked into flakes that need to pass through the nip one or more times, the force applied by the compression mechanism and the pressure sensed at the nip can be gradually increased until they reach a peak or plateau value within the aforementioned appropriate pressure range. Alternatively, even if the force applied by the compression mechanism is constant, the pressure sensed at different nibs in a series of nibs compressed by the same mechanism may be different. For example, considering a linearly aligned series of nibs formed by a series of rotatable cylinders with gradually decreasing diameters, the pressure sensed at nibs between relatively smaller cylinders will be higher than the pressure sensed at nibs between relatively smaller cylinders, and the pressure will increase as the diameter decreases for the same force.

[0118] Interestingly, as taught herein, the same force mechanism can be used to simultaneously apply force to two or more series of rotary cylinders / nips, each series forming an independent module capable of producing the same or different (e.g., taster) flakes. For illustrative purposes, the same compression mechanism can apply force to a first series of rotary cylinders forming the nip of the first series (e.g., to produce flakes of a first material), and to a second series of rotary cylinders forming the nip of the second series (e.g., to produce flakes of a second material). The first and second series are physically separated and can be arranged in parallel or in series.

[0119] Such a configuration allows for the simultaneous preparation of flakes of two or more different materials on separate nips, which is advantageous when preparing flaked materials that mix one with the other. In such cases, if the first material is a flavoring agent for its intended purpose, the second material does not need to provide flavor on its own. The flaking method described herein is expected to reduce the amount of sodium required for the agent to exert its full effect in food. Since sodium bicarbonate, in products that do not contain natural acids, may require the addition of an acidifying agent to react with it to release carbon dioxide, which ultimately softens the product when coated, it is preferable to simultaneously flake a suitable second material. For example, 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) are some of the weak acids that exist in crystalline form and can be flaked on a second set of nips, and a mixture of the two materials allows for the preparation of baking powder or other food products (e.g., g). Similarly, if none of the materials being flaked are flavoring or odor-masking agents, they may be two or more materials that fit into the same manufacturing process, and the likelihood of flakes of the first material being "contaminated" by flakes of the second material (or third material, etc.) does not have a detrimental effect on the intended manufacturing process.

[0120] Given the relatively high pressure applied at the nip, the rotating cylinder and counter surface are advantageously made of a material having sufficient hardness or other properties that provide mechanical resistance, suitable for withstanding such pressure without significant deformation and / or wear. The rotating cylinder and counter surface may be made of metal (e.g., stainless steel), ceramic (e.g., tungsten carbide (WC)), or polymer (e.g., Kevlar). (R)Since they may be made of or coated with such materials, their outer surfaces that come into contact with each other must have a Vickers hardness of at least 50 HV, at least 100 HV, at least 150 HV, or at least 200 HV. The hardness of the material does not need to be particularly limited, but is generally not greater 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. For any surface, the desired hardness may decrease as the pressure applied to it decreases relatively.

[0121] The hardness of the cylinder or its outer surface depends on a) the exact composition of each cylinder and any coating present, and b) whether the bulk material has been further treated (e.g., annealing, cold working, hardening, heat treatment, or tempering) and, to what extent (e.g., stainless steel can be tempered to 1 / 16, 1 / 4, 1 / 2, 3 / 4, or full hardness). The relative elasticity of a rotating cylinder is expressed above in terms of its hardness, but those skilled in the art of materials and their physical properties can readily "translate" such requirements into other terms such as strength, yield point, etc., and all such alternative or additional parameters are selected to avoid or minimize deformation and / or wear of the cylinder surface under the operating conditions of the method or apparatus.

[0122] In some embodiments, the rotating cylinder(s) and opposing surfaces are made of a sufficiently hard and resilient material, and furthermore, have a desired surface topography (e.g., smooth or textured, whether random or not). In some embodiments, the surfaces pressed against each other are relatively smooth. In such cases, the surface roughness (R) is 500 nm or less, 400 nm or less, 300 nm or less, 200 nm or less, or 100 nm or less. a) can have. Ideally, a perfectly smooth surface has an average surface roughness of zero, but generally R (a)は It is 20nm or larger.

[0123] The temperatures of the rotating cylinder and the opposing surface can be adjusted as desired using any suitable internal or external heating or cooling device. The temperatures of the rotating cylinder(s) and the opposing surface can be selected according to the same principles as those described for the preparation of liquid stocks (e.g., flavoring agents). However, after the application of the liquid stock, it is no longer essential to ensure that the temperature does not exceed the boiling point of the liquid, and the only remaining consideration is the thermal sensitivity of the material.

[0124] Heating can take different forms depending on the temperature to be reached, and can be by conduction, convection, or radiation. Conduction heating can be achieved by placing a heating element beneath the surface or liquid to be heated, or by circulating a hot liquid (e.g., heated oil or water) in a pipe, chamber, or jacket positioned appropriately for its effect. Convection heating can be achieved by blowing a hot gas (usually air) toward the surface to be heated. Radiation heating can be achieved with microwaves in a suitable chamber, but more commonly with an infrared lamp directed to radiate toward the relevant surface or material.

[0125] As those skilled in the art will understand, the rate at which a liquid (e.g., taster) stock is applied to a movable (e.g., wettable) surface depends, in particular, on the surface tension and surface energy of the liquid stock, the desired thickness of the thin film, the rate of removal (e.g., evaporation) of the liquid under operating temperature and pressure conditions, the surface velocity at the nip, the dimensions of the nip, and similar factors. The flow rate, or the metering of the intermittently applied dose, can be determined empirically and adapted as desired.

[0126] A thin film can be formed by running the surface to be coated (e.g., a flavoring or deodorizing agent) through a bath of liquid stock by dropping or spraying the liquid stock onto the surface via one or more nozzles positioned parallel to the contact line of the nip / axial length of the rotatable cylinder, the nozzles supplying the liquid stock upstream of a device (e.g., a doctor blade, air knife, squeegee, etc.) positioned across the width of the movable surface and configured to horizontally move the liquid stock, or by any other method adapted to form a liquid film of minute thickness on the surface. As understood, in some embodiments, the liquid does not need to be applied as a thin film upstream of the nip, and the nip itself plays a role in leveling the excess amount of liquid stock that forms an initial, optionally transient, upstream pool into a thin film downstream.

[0127] As is easily understood, for a given concentration of material (e.g., taster) in a liquid, a relatively thin film of the liquid stock (e.g., taster) allows for relatively faster removal of the liquid or at least a portion of it than a relatively thick film, provided all other conditions of the method are the same. In some embodiments, the thin film has an initial thickness 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 when applied to the surface (before significant removal of the liquid). Typically, the thin film is applied to have an initial thickness of at least 250 nm, at least 500 nm, at least 750 nm, or at least 1 μm.

[0128] Because this method is intended to remove a portion of the liquid over time, the thickness of the liquid stock (e.g., flavoring and deodorizing agents) gradually decreases, first partially, then entirely, until it precipitates as a thin film when the material has essentially completely removed the liquid from the final layer of separable flakes. The thickness of the thin film of precipitate may also decrease over time and with repeated compression. As understood, the “complete removal” of liquid, which is considered to be obtained at the end of the flake-making process, does not mean that the resulting layer of flakes, composed of aggregated and / or compressed particles, and the separable flakes therefrom, will contain no liquid at all, either remaining in a “dry” film or adsorbing in relatively trace amounts onto the flake surface. At the end of the process, the amount of residual liquid in the layer containing compressed and aggregated particles that allow for crushing into commercially important flakes may be acceptable. In some embodiments, at least partial removal of the liquid (e.g., partial evaporation) can be determined by monitoring weight loss under conditions (e.g., temperature and time) adapted to remove essentially all of the liquid without affecting the remaining solid, thus enabling the production of dry layers and / or crushed (e.g., flavoring agent) flakes with a liquid content of 5 wt.% or less. In some embodiments, the flakes contain less than 4 wt.%, less than 3 wt.%, or less than 2 wt.% of the liquid per weight of the flakes. In other embodiments, the liquid content is considered insignificant (or the flakes are considered substantially dry) if the liquid content is 1 wt.% or less, 0.8 wt.% or less, 0.6 wt.% or less, 0.4 wt.% or less, 0.2 wt.% or less, 0.1 wt.% or less, or 0.05 wt.% or less relative to the weight of the (e.g., flavoring agent) flakes. The same upper limit on liquid content also applies to layers of compressed and / or aggregated particles before they are crushed into flakes, which can be considered representative samples of the dry layer.

[0129] The process for preparing (e.g., palatability) flakes using this method can ideally be continuous, but generally, if it relies on one or more nips, it can be carried out in an alternating "stop-and-go" manner. In this case, one dose of liquid is applied, and after this dose of liquid has transformed into flakes, a second dose of liquid is applied. If multiple nips are involved in the process, the second dose of liquid can be applied before the flakes are collected in the last nip. Therefore, the more nips there are, the shorter the time between applications of separated doses, or even the continuous process can be considered.

[0130] As the flakes are compressed by passing through the nip, they gradually form a layer of flakes, naturally detaching from the thin coating placed on the surface, and the flakes crushed in the nip are funneled into a collector by gravity. The flakes can be actively collected additionally or alternatively using, for example, blades, propulsion jets of gas (e.g., air or heated air), or other means suitable for detaching the flakes from the layer of compressed particles or the underlying surface. Typically, flakes that detach spontaneously from the rotating surface on which they are formed are relatively larger and / or thicker than flakes that are actively detached with the help of a detachment device. In general, flakes that detach spontaneously are made of more brittle material.

[0131] Flakes obtained by such methods (e.g., flavored flakes) may not be thin enough after passing through a nip once to form microflakes, submicroflakes, or nanoflakes of the desired dimensions. In such cases, the flaky product recovered from the initial compression nip can be advanced through one or more additional nips until the recovered product exhibits the desired properties for the flakes. After periodic passage through the first nip, once most of the liquid has been removed or evaporated, passing the flakes through additional nips can help remove any residual liquid that may have been absorbed onto the surface of the flakes.

[0132] Alternatively or additionally, flakes obtained by such methods (e.g., flavoring agents) may contain residual amounts of liquid that may not be suitable for their intended use and / or storage stability. Regardless of the reason for its desirable removal, the method may further include a step dedicated to the removal of any residual liquid present. For example, the flakes may be dried.

[0133] Flakes prepared according to the methods disclosed herein (e.g., flavoring and deodorizing agents) have a relatively high specific surface area compared to conventional non-flaked counterparts, and therefore may have an increased tendency to absorb ambient moisture. This phenomenon can cause caking of the flakes, impairing their fluidity and making their transport, handling, storage, and application more difficult. In such cases, the flakes may be treated with additives that can suppress caking, and the method may further include steps to achieve this effect. Alternatively or additionally, the treatment may be physical, and the flakes may be dried before being stored in an environment free from otherwise harmful factors (e.g., dried flakes are stored under vacuum or inert gas conditions, or in a liquid in which they are stable (insoluble), and the liquid is impermeable to harmful factors). For example, flakes consisting of water-soluble flavoring substances can be stored in substantially insoluble edible oil (or a similar lipophilic product that is semi-solid or essentially solid), where the (e.g., vegetable) oil serves to deliver the dispersed flavoring substances to the food during food preparation or prior to consumption.

[0134] In some embodiments, the method may further include sorting the flakes according to size (e.g., flavoring substances) to increase the uniformity of the size of each subgroup thus sorted. For example, the flakes may be sieved through a mesh of a desired opening size. A group of flakes with relatively uniform particle dimensions is expected to provide a relatively consistent effect, as may be required when standardized performance is expected from the flakes or products incorporating them.

[0135] Any steps that may be performed after flake collection, though not limited to those exemplified above, may be referred to as post-processing steps or post-flaking steps. Apparatus or subsystems that enable the execution of such steps in an apparatus for producing such flakes may, accordingly, be referred to as post-processing stations or post-flaking stations.

[0136] Although this method has been described in relation to a single material (e.g., a taster), it can be similarly used to prepare flakes of two or more materials. For example, if each material is crystalline, this method can be used to achieve their co-crystallization, and by compression, flakes of a mixture of the materials (e.g., tasters) can be prepared. In this specification, the terms "material(s)" or "tasterity(s)" may be used to indicate that one or more materials or tasters may be used in the described steps, devices, or products.

[0137] The flakes prepared as described herein, regardless of the number of distinct materials (e.g., flavoring substances) used in their preparation, generally contain one or more individual elements of the precipitated material(s), e.g., single crystals or more of the precipitated flavoring substance having a crystalline structure. The flakes typically consist of several such elements forming a continuous mosaic of the precipitated material(s) (e.g., if the material is a crystalline flavoring substance, crystals of multiple salts or sugars), and the coating of aggregated elements itself is not necessarily continuous. Advantageously, in some embodiments, the mosaic of the precipitated material(s) appears in the resulting flakes as substantially coalesced / substantially absent voids between the various elements forming the flakes.

[0138] Several embodiments of this method and its various steps are shown in Figure 1, where boxes with dashed outlines indicate any of the steps.

[0139] In the first step S01, one or more materials (e.g., flavoring substances) to be manufactured as flakes are provided. Typically, the materials are provided as dry powders of various shapes and dimensions. If the materials(s) are provided as a paste or liquid, the method may begin from step S03 to obtain the desired concentration of the materials(s) and / or viscosity of the liquid stock, or it may begin from step S04 if the materials(s) have a desired concentration (e.g., adapted to form a solution at least close to saturation) and / or the liquid stock has a desired viscosity (e.g., not exceeding 5,000 mPa·s at the temperature of dispersion, dissolution, or application).

[0140] If the material (e.g., a flavoring and deodorizing agent) is provided as a dry powder and one of the material has a relatively large initial size, for example, at least one dimension greater than 5 mm, the material can be reduced in size by any suitable method such that, if desired, preferably all dimensions do not exceed 5 mm or are even smaller and in the micrometer range. For illustrative purposes, this second step S02 consists of optionally grinding the at least one material provided in S01.

[0141] In the third step S03, at least one material (e.g., a taster) (which may optionally be downsized to any desired particle size in the low millimeter range (e.g., between 0.5 and 5 mm) or the low micrometer range (e.g., between 0.5 and 10 μm)) is dissolved or dispersed in a liquid (the number of phases in the liquid stock depends on the relative volume and / or the properties of the liquid and the volume of material dissolved therein). This step can be carried out, as described above, under stirring, heating, and / or pressurization to adapt to the resulting liquid stock.

[0142] In the fourth step S04, a liquid stock (e.g., one or more flavoring substances) is applied to a movable surface (which can optionally be wetted by the liquid stock). Typically, the liquid stock applicator and the surface to which it is applied as a thin liquid film move relative to each other. The applied liquid can be leveled to form a thin film by using a dedicated leveling device to set a desired initial thickness, or / or by displacing the applied liquid (or liquid film of first thickness) toward a nip formed between the movable surface and the opposing surface.

[0143] A nip between two surfaces is formed by biasing one surface relative to the other in a step shown as S05 in Figure 1. The nip can be a single nip or a series of nibs, as will be described in more detail with reference to Figures 2 to 7. In contrast to conventional leveling or thinning devices that are set to maintain a constant spacing for the material being processed, it is emphasized that this nip, formed under continuous biasing pressure, is conversely configured to accommodate a spacing that varies between gaps of up to 400 μm when applying liquid stock to a thickness of 1 μm or less before feeding or after all flakes have been detached from the formed surface.

[0144] Any heating of at least one of the movable surface and the opposing surface is clearly illustrated as S06 following S05, but this is not the only possible sequence of events, and any heating of the surface (or one of them) may be performed alternatively or additionally before the application of the liquid stock (before S04) and / or before the liquid stock reaches the nip (before S05).

[0145] In the seventh step S07, at least a portion of the liquid is removed from the thin film of the liquid stock (e.g., of the taster(s)) to increase the relative concentration of the material(s) in the liquid phase and allow separation from them as solid particles. Ideally, the liquid should be removed quickly enough in a single pass through one nip to ensure the formation of a thin film of completely precipitated material(s) to allow for continuous application of the liquid stock, but this is not essential. Alternatively, the method can be carried out continuously by flowing a thin film of liquid stock through a series of nip, with the concentration of solid particles of the material(s) progressively increasing, and the thin film of precipitated material(s) generally transforming into a dry layer of aggregated particles after the last or final nip. This method can also be carried out in an alternative manner, with respect to the fact that the application of the liquid stock is batch-based, and the thin film of the liquid stock passes through the same nip or a series of nips multiple times, and the gradually precipitating thin film of material generally becomes a dry layer of aggregated particles after passing through the (last or final) nip. The gradual removal of the liquid (e.g., by evaporation, which can be accelerated by heating the nip-forming surface) leads to the precipitation of the material, which can also be a continuous event until all the liquid is essentially removed. For example, considering a flavoring substance made of a crystalline material, the precipitation of the initial portion of the flavoring substance may result in the formation of the first crystals that constitute the nucleating centers of the flavoring substance that subsequently precipitates from the film of liquid stock.

[0146] In the eighth step S08, a thin film of precipitated material (one or more) (e.g., taste substance(s)) is compressed (and optionally, pulverized in the process so that flakes naturally detach from the areas of the sufficiently compressed film). With respect to the gradual removal of the liquid, this gradual compression of solid particles continuously separating from the liquid may occur in one or more passages through the same or different nips. Though referred to as “compression” for simplicity, this step can achieve several effects that may be synchronized, which are not necessarily distinguished, nor are all of them performed. Advantageously, the compression in which solid particles gradually separate from the liquid stock as the liquid evaporates, regardless of the method or means by which it is carried out, is considered to achieve consolidation of the precipitated material(s) into aggregates of particles, where the individual elements of the precipitated material have relatively high cohesive forces among themselves, and the thin film of aggregated particles and the layer of flakes emerging therefrom are relatively uniform (e.g., thickness, etc.). Therefore, while conventional precipitates can form relatively fragile aggregates of individual precipitated elements, the repeated passage of the liquid stock through the nip(s) and the periodic compression of the material precipitated therefrom is thought to initially form amalgam, where the individual precipitated elements fuse with each other. Thus, the flakes obtained by the method of the present invention can have relatively low porosity and / or relatively high transparency. In some embodiments, the (e.g., tasting) flakes have a porosity of at most 30%, at most 25%, at most 20%, or at most 15%. In some embodiments, the flakes have a porosity of at least 1%, at least 2%, or at least 5%.

[0147] In this figure, the removal of the liquid (S07) is shown preceding the compression of the particles (S08) that separate from the liquid stock as solid elements; however, in reality, these steps may occur simultaneously, as both steps are typically repeated periodically. Taking a rotating cylinder as an example of a movable surface on which flakes are formed, the shaping takes place in the nip-forming region of the cylinder that engages with the opposing surface, with the upstream and downstream surfaces of the nip exposed to allow for the evaporation of the liquid.

[0148] In the ninth step S09, the flakes (e.g., flavoring substances) can be recovered from the last surface on which a thin film of precipitated substances is present. If the method is carried out in a series of nips, collection can be carried out in different nips. If the recovered fractions have similar properties (e.g., similar dimensions), different nips can play a role in increasing the productivity of the method. If the fractions collected in different nips have different properties (e.g., different dimensions, aspect ratios, etc.), different nips can play a role in sorting the flakes produced by the method.

[0149] Exemplary different nips related to this method and the apparatus described below will be briefly described with reference to their schematic diagrams, as shown in Figures 2 to 7. In order to clarify these non-limiting nip configurations, some apparatus or apparatus enabling the method steps disclosed herein will not be shown in these figures. Omitted apparatus may be essential and include, for example, a compression mechanism for biasing at least one pair of surfaces to contact to constitute a nip, a drive mechanism (e.g., a motor, connector, etc.) for driving the rotation of at least one rotatable cylinder, and a dosing device capable of periodically supplying a desired dose or desired continuous flow rate of liquid stock to the applicator. Omitted apparatus is optional and includes, for example, a leveling device capable of forming a thin layer of liquid of a desired thickness; a heating device capable of heating the surface to be coated during the process (heat is applied from the back and / or front side of the surface); and a peeling device capable of “scraping” off the thin layer of deposited material(s). Such apparatus may be optionally retractable depending on the selected nip configuration. Such apparatus, as well as any dryers, chambers, flake sorters, and similar apparatus that may be used in conventional flake preparation, are known and do not need to be described in detail herein. Furthermore, all may be placed on and supported by a suitable structure or support frame.

[0150] For the sake of brevity, the operating principles common to all nip configurations will not necessarily be repeated in the following description. To avoid misunderstanding, in these figures, various nip configurations are illustrated with the surfaces forming each nip engaged, but in apparatus including such nip configurations, the surfaces can be disengaged to allow for surface maintenance (e.g., cleaning) or replacement if desired. Furthermore, in some illustrated embodiments, the plane containing the axis of rotation of the rotating cylinder is depicted in a horizontal orientation, but this should not be interpreted restrictively. For illustrative purposes, a pair of counter-rotating cylinders can be angled with respect to the horizontal, with the liquid stock applied at the upper end of the inclined nip and the flakes collected at the lower end of the nip. If the cylinders have appropriate dimensions (e.g., sufficient length) and appropriate operating conditions (e.g., flow rate of the liquid stock, rotational speed and temperature of the cylinders, pressure applied to it as sensed at the nip, etc.), such an arrangement can advantageously enable continuous dispensing of the stock and collection of the flakes produced therefrom.

[0151] Figure 2 schematically illustrates a nip 200 formed by pressing a rotating cylinder 210 having an outer surface 210' (e.g., wettable) against an opposing surface 220 that is planar (and not necessarily static, but typically) and has an outer surface 220' opposite the cylinder. In this figure, an applicator for (e.g., tasting(singular or plural)) liquid stock is indicated by arrow 260, and a collector for (e.g., tasting(singular or plural)) flakes is indicated by container 270.

[0152] The applicator 260 may be any device capable of dispensing liquid (e.g., a nozzle) or coating a surface (e.g., a brush), but the term is also frequently used herein to refer to a dispensing device capable of intermittently dispensing a controllable amount of liquid stock at a predetermined repetitive dispensing rate (e.g., 1 ml per minute) or intermittently dispensing a controllable amount of liquid stock, where the amount repeatedly applied or the flow rate of continuous dispensing is selected so as not to cause excess liquid stock to flow out of the surface forming a nip.

[0153] The collector 270 is depicted downstream of the nip 200 for simplicity, but it may be located at other positions along the path followed by the rotating surface 210'. The cylinder 210 may not only rotate around its axis but also move along the opposing surface 220 (up and down in the illustrated diagram), and since the opposing surface is static, collection of flakes into the collector 270 may also occur from the thin film formed on the surface 220'. A similar effect of causing a thin film of precipitates to form on the surface 220' can be achieved, conversely, by keeping the rotation axis of the cylinder 210 stationary and allowing the opposing surface 220 to move relative to it (up and down in the illustrated diagram), or by displacing both the rotation axis of 210 and the opposing surface 220 in the Z direction, thereby maintaining constant contact between the two surfaces (and thus the nip 200). Flake recovery may result from the spontaneous detachment of flakes, as a thin film of precipitated material is formed from the gradual removal of the liquid or at least a portion of it and compressed as it passes through the nip, each of which is sustained by one or more rotations of cylinder 210 and passage through nip 200. A detachment device may also be used for flake recovery, which can be operated in a controllable manner after the formation of a relatively dry layer consisting of flakes of precipitated and aggregated material, at which stage the flakes typically contain no more than 5 wt% liquid. For example, detachment can be facilitated, if desired, by directing a jet of gas onto the layer consisting of flakes or by bringing a suitable mechanical obstruction (e.g., a blade) towards it and scraping it away from its underlying surface as individual flakes.

[0154] Figure 3 schematically shows a nip 300 formed by pressing a first rotating cylinder 310 having an outer surface 310' (e.g., wettable) against the opposing surface of a second rotating cylinder 320 having an outer surface 320' (e.g., wettable). In this figure, the two cylinders rotate in the same direction (e.g., clockwise) to create a slip in the contact line. An applicator for liquid stock (e.g., tasten) is indicated by arrow 360, and a collector for flakes (e.g., tasten) is indicated by container 370, which are optionally drawn downstream of the nip 300, but may be at other locations along the path favorably followed by the rotating surface 310' and, more favorably, the rotating surface 320'.

[0155] Figure 4 schematically illustrates a nip 400 formed by pressing a first rotating cylinder 410 having an outer surface 410' (e.g., wettable) against the opposing surface of a second rotating cylinder 420 having an outer surface 420' (e.g., wettable). In this figure, in contrast to Figure 3, the two cylinders are rotating in opposite directions (e.g., one clockwise and the other counterclockwise). Ideally, slip at the contact line can be avoided if the two cylinders are moving at the same speed, but this is not essential. An applicator for (e.g., tasting) liquid stock is indicated by arrow 460, and a collector for (e.g., tasting) flakes is indicated by container 470, which are optionally drawn downstream of the nip 400, but may be at other locations along the paths followed by the rotating surface 410' and, favorably, the rotating surface 420'.

[0156] Figure 5 schematically shows a series of linearly aligned nips 500a, 500b, and 500c. Nip 500a is formed by pressing a first rotating cylinder 510 having an outer surface 510' (e.g., wettable) against an opposing surface which is a second rotating cylinder 520 having an outer surface 520' (e.g., wettable). Nip 500b is formed by biasing the second rotating cylinder 520 against an opposing surface which is a third rotating cylinder 530 having an outer surface 530' (e.g., wettable). Nip 500c is formed by biasing the third rotating cylinder 530 against an opposing surface which is a fourth rotating cylinder 540 having an outer surface 540' (e.g., wettable). The applicator for (e.g., tasting) liquid stock is indicated by arrow 560, and the collector for (e.g., tasting) flakes is indicated by container 570, which is optionally drawn downstream of nip 500c, but may be at other positions along the paths followed by the planes of rotation 510', 520', 530', and preferably 540'. If necessary, multiple collectors can be used along a series of nips, as schematically shown in Figures 5-7, for example. In this figure, the linear alignment of the nips is illustrated with four cylinders of similar dimensions, with each set of cylinders rotating in opposite directions, but this is not necessary. The linear alignment of the nips can be achieved with any other number of cylinders equal to or greater than three, where the cylinders are the same or different, rotated in the same or different directions, and / or rotate at the same or different speeds. In a linear alignment of cylinders, in which a single compression system and / or a single motor may be used to bias and / or rotate any two cylinders to rolling contact, each pair of cylinders may be separated from nearby pairs, as is conceivable.

[0157] In some cases, a series of nips (whether or not schematically illustrated in Figures 5-7) may include a sufficiently large number of nips under the operating conditions selected for the preparation of flakes (e.g., flavoring agent) to allow the presence of two or more applicators (e.g., dispensing devices) capable of supplying a liquid stock (e.g., flavoring agent) onto one or more of the outer surfaces of the cylinders constituting the series of nips. The liquid stock supplied by all applicators can be the same, and such a configuration is suitable for continuous dispensing of the liquid stock and collection of the flakes produced therefrom.

[0158] Figure 6 schematically shows a series of nips 600a, 600b, 600c, and 600d radially aligned toward a common central rotating cylinder 610 having an outer surface 610' (not shown in the figure) (for example, wettable). Nip 600a is formed by biasing an opposing surface, which is a second rotating cylinder 620 having an outer surface 620' (not shown in the figure) (for example, wettable), toward the first rotating cylinder 610. Nip 600b is formed by biasing an opposing surface, which is a third rotating cylinder 630 having an outer surface 630' (not shown in the figure) (for example, wettable), toward the first rotating cylinder 610. Nip 600c is formed by biasing an opposing surface, which is a fourth rotating cylinder 640 having an outer surface 640' (not shown in the figure) (for example, wettable), toward the first rotating cylinder 610. Nip 600d is formed by biasing the opposing surface of a fifth rotating cylinder 650, which has an outer surface 650' (not shown in the figure) (e.g., wettable), relative to the first rotating cylinder 610. An applicator for (e.g., one or more tasters) liquid stock is shown by arrow 660, and a collector for (e.g., one or more tasters) flakes is shown by container 670, which is optionally drawn downstream of nip 600c, but may be at other locations along the path followed by the rotating surfaces 610', 620', 630', 640', and preferably 650'. For example, the collector 670 may be located downstream of nip 600d. In this figure, the radial alignment of the nip is shown with four cylinders of similar dimensions positioned on the diametrically opposed side of a common central cylinder, with each outer cylinder rotating in the opposite direction to the central cylinder, although this is not required. The radial alignment of the nip can be achieved with any number of outer cylinders, as long as there are three or more; the cylinders can be the same or different, and they can rotate in the same or different directions and / or at the same or different speeds.

[0159] In particular, in Figure 6, the rotating cylinders 620, 630, 640, and 650 are positioned to contact the outer surface of the central rotating cylinder 610 to which the liquid stock processed by this method is applied. Alternatively, they could face the cylindrical wall of 610 from the inner side. In that case, the rotating cylinder 610 would be a hollow cylinder or drum, and the liquid material would be applied to the inner surface of the hollow cylinder. Similarly, the collector 670 would be positioned within the hollow plenum of 610.

[0160] The presence of numerous cylinders (e.g., 620, 630, 640, and 650) positioned to rotate in contact with the centrally rotating cylinder 610, whether located inside or outside it, allows for different modes of dispensing the liquid stock. For example, instead of dispensing the liquid stock toward a first nip in series by one or more nozzles positioned parallel to the nip and adapted to spray the liquid as needed, the stock can be dispensed by immersing a portion of the cylinder at the first nip through a bath filled with the liquid stock. In the latter case, the appropriate dosage of liquid stock to be dispensed is governed by the surface energy of the cylinder surface immersed in the bath and the surface tension of the liquid stock, and any excess liquid usually drips back into the bath by gravity before the remaining thin film enters the downstream nip.

[0161] Figure 7 schematically illustrates a series of nip configurations combining the principles of linear and radial nip alignment. The nip between the rotating cylinders 710, 720, 730, 740, and 74B is considered to form a linear alignment, while the nip between 71A, 71B, and 710, or 72A, 72B, and 720, or 73A, 73B, and 730, or 74A, 74B, and 740 is considered to form a radial alignment with respect to the rotating cylinders 710, 720, 730, and 740, respectively. An applicator for (e.g., tastent(singular or plural)) liquid stock is indicated by arrow 760, and a collector for (e.g., tastent(singular or plural)) flakes is indicated by container 770, and is optionally drawn downstream of the nip formed by the rotating cylinders 740 and 74C.

[0162] Some of the configurations described above, particularly those involving a series of nips, may include multiple instances of essential or optional equipment not illustrated for clarity. For example, each rotating cylinder may be driven independently by a different motor. Considering leveling and / or peeling devices, they do not necessarily have to be exclusively positioned at the first and last cylinders, but may be repeatedly positioned along a series of nips. Using Figure 6 as an example, the first leveling device may be positioned downstream of the coated liquid stock, facing cylinder 610 upstream of cylinder 620, while the second leveling device may be adjacent to cylinder 620, or again adjacent to cylinder 610 but downstream of nip 600a. Similarly, while a final peeling device might be found peeling flakes from the surface of cylinder 650, there may be an upstream peeling device earlier, for example, in the section between nips 600c and 600d, peeling flakes (e.g., reagents) from the surface of cylinder 610. Depending on the specific structure and mode of operation, as well as the precise relative positioning of the peeling device, additional collectors may be required in addition to the 670.

[0163] In certain embodiments, regardless of the type of alignment (one or more) following a series of nips (e.g., linear and / or radial), the number of nips and the rotating cylinders forming them are selected so that continuous application of a liquid stock (e.g., flavoring agent (one or more)) and collection of flakes (e.g., flavoring agent (one or more)) are possible upon completion of the process under operating conditions set for that purpose.

[0164] According to another aspect of the present disclosure, an apparatus is provided for producing flakes from a liquid stock consisting of a material dissolved or dispersed in a liquid, the apparatus comprising: a) Support frame b) At least two cylinders attached to the frame, wherein at least one of the cylinders is movable relative to the support frame, and c) A biasing mechanism that biases the cylinders to contact each other so as to form at least one nip. d) A drive motor for rotating at least one of the cylinders It is characterized by being equipped with [the following features]. e) A dispensing apparatus for dispensing a liquid stock to at least one of cylinders so as to coat a thin film on the surface of the cylinder, wherein the concentration of the solid material in the thin film increases as the thin film repeatedly passes through at least one nip, resulting in the formation of flakes of the material, and f) A controller for adjusting the rate at which liquid stock is applied to at least one of the cylinders, in accordance with the rate at which liquid is lost from the film while the film continues to pass through at least one nip.

[0165] Since the two or more rotatable cylinders of this apparatus are biased to contact each other while the flaking system is operating, the nip formed between any two adjacent cylinders may vary in spacing during the process. Even though a constant biasing force is applied by the biasing mechanism that biases the cylinders to contact each other, the nip may have a larger gap (separation) when supplying the material to be flaked compared to the gap (if any) that would exist under similar conditions when there is no liquid stock to be applied (e.g., before the application of the stock or at the completion of flaking).

[0166] In some embodiments, the apparatus further includes a leveling device adapted to level the liquid stock (e.g., palatability) into a thin film before passing through a nip. In contrast to the nip preferred herein, the leveling device may be set at a certain distance from the surface to which the liquid is to be leveled. In some embodiments, the apparatus further comprises at least one heating device for heating the liquid stock (e.g., flavoring agent) dispensed by the dispensing device and at least one of the surfaces of two or more rotatable cylinders.

[0167] In some embodiments, the apparatus further comprises a peeling device adapted to peel (e.g., flavoring agent) flakes from a film from which the liquid is removed, in other words, from a thin film or layer of precipitated, aggregated, and compressed solid material that forms the flakes, for recovery by a recovery device.

[0168] In some embodiments, the device further includes a controller that plays a role in continuously or periodically controlling at least one of the following: a- The amount of liquid stock to be dispensed, and / or the periodicity or speed of the liquid stock applied by the dispensing device; b- Force or pressure applied by a force mechanism (also called a compression mechanism); c- The rotational speed of at least one of two or more rotating cylinders; and d- The temperature of the liquid raw material and / or the temperature of any surface of two or more rotating cylinders.

[0169] Such control systems are well known and do not need to be described in further detail herein.

[0170] These systems can be configured based on feedforward proactive control (controlling to achieve a pre-set target value) and / or feedback control (responding to a signal related to the controlled parameter). For example, the inventors have found that the torque of a motor driving a cylinder rotating in a nip section where the material is processed into flakes can predict the timing of new material dosing if the flake processing is intermittent. Thus, a liquid dispensing or dosing device (e.g., arrows 260, 360, 460, 560, 660, and 760 in the figure) can be controlled by such a feedback mechanism to release a new liquid dosing at each (e.g., first) nip (e.g., 200, 300, 400, 500a, 600a, and the nip between rotating cylinders 710 and 720) when the motor torque (a value measured by a torque measuring device) reaches a minimum value (corresponding to the minimum percentage of liquid in the flakes making up the layer), and the amount of new liquid dosing can be controlled at that point. Other suitable controllers can monitor the progress of the flakening process and adjust the dispensing device accordingly. Other control methods target forces or pressures applied by force mechanisms, which can be monitored, for example, via strain gauges placed in close proximity to the nip being controlled.

[0171] In some embodiments, the outer surface of each of the two or more rotatable cylinders of the apparatus is made of or coated with a material that can be wetted with a liquid stock (e.g., sample(s)).

[0172] In some embodiments, the outer surface of each of the two or more rotating cylinders of the apparatus is formed from 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.

[0173] In some embodiments, the outer surfaces of two or more rotating cylinders of the apparatus are formed from or coated with a material having a Vickers hardness of 50 HV to 10,000 HV, 100 HV to 5,000 HV, 150 HV to 3,500 HV, or 200 HV to 2,000 HV.

[0174] In another embodiment, products (which may also be called manufactured products) comprising the flake-shaped water-soluble or water-insoluble material of the present disclosure, and / or the flake-shaped water-soluble or water-insoluble material produced by the present method, and / or the flake-shaped water-soluble or water-insoluble material produced using the present apparatus are also provided.

[0175] In another aspect of this disclosure, a food product is provided that includes the flavoring pieces described in this disclosure, or that is produced by the method described herein, or that is produced using the apparatus described herein.

[0176] In another aspect of this disclosure, a method for improving a product is provided, the method comprising the step of incorporating the product with the flakes disclosed herein and / or flakes produced by the Method and / or flakes produced using the Apparatus, the flakes comprising or constituting at least one active or inactive component. The improvement of the product is not limited to areas in which the product may be improved, such as its chemical effects, physical effects, biological effects, quality, ease of manufacture, storage, or transport, or the cost of manufacture, storage, or transport.

[0177] In another aspect of this disclosure, a method for improving food is provided. The method includes the step of incorporating into food or beverage a flake described in this disclosure, or a flake produced by the method, or a flake produced using the apparatus. The flake may optionally contain taste components. Food improvement is not limited to areas where food improvement is required and achievable by the flakes herein, such as taste, smell, shelf life, texture, appearance, or ease of preparation.

[0178] Food improvements also extend, either in addition to or instead, to ensuring that the characteristics exhibited when the food is freshly manufactured and expected by consumers using all the senses typically involved in evaluating a food product are maintained for a longer period of time or have their decline delayed. Therefore, more broadly, taste components do not necessarily have to provide taste, but rather aid in the perception of the quality of a food product and include, for example, emulsifiers, thickeners, binders, coagulants, texture modifiers, curing agents, leavening agents, stabilizers, preservatives, moisture-proofing agents, pH adjusters, colorants, flavor enhancers, vitamins, mineral nutrients, and other food additives that are expected to have a positive impact on the characteristics of the food. These additives are used for the purposes of consumption, manufacture, processing, handling, packaging, transport, or preservation of food.

[0179] In another aspect of this disclosure, a method is provided for reducing the amount of material in a manufacturing process or a manufactured product. The method includes replacing at least a portion of the material in the process or product with the flakes disclosed herein and / or with flakes produced by the Method and / or with flakes produced using the Apparatus.

[0180] In another aspect of this disclosure, a method is provided for reducing the amount of a taste substance suitable for providing a desired taste to a food. The method includes replacing at least a portion of the taste substance in the food or beverage with flakes of the taste substance disclosed in this disclosure, or flakes of the taste substance produced by the method, or flakes of the taste substance produced using the apparatus.

[0181] For the sake of brevity, this method and apparatus are described as being primarily suitable for the production of flakes of taste components applicable to the food industry or products involving oral administration or use (e.g., products that have a taste or contribute to product quality), but they are also applicable to the production of flakes of other active or inactive components for similar purposes. The raw materials to be flaked do not need to provide a taste, be suitable for animal consumption or use, or be for the food industry. For example, products in which this particular form is beneficial (e.g., processes where dissolution, dispersion, decomposition, release into the environment, absorption by relevant organisms, or a relatively increased specific surface area is beneficial to the efficiency of the product) can be considered products to be flaked. [Examples]

[0182] Example 1: Drying and flakeming of taste substances In this example, taste substances selected from commercially available sugar, salt, and ground coffee were flakened while being supplied as dry powders. Sugar and salt are water-soluble substances, while coffee is considered water-insoluble despite containing water-soluble components. The dried samples were fed into an apparatus equipped with a nip consisting of three rotating cylinders, as schematically shown in Figure 5. Rotating cylinders 510 and 530 are both made of stainless steel 17-4 PH (R) (Vickers hardness 240 HV, average surface roughness R) aThe first cylinder was made of tungsten carbide (less than 1,600 nm) and had a diameter of 30 cm. Rotating cylinder 520 was positioned between cylinders 510 and 530, and was made of tungsten carbide with a diameter of 1 cm. The three cylinders had approximately the same axial length of 25 cm. They rotated in opposite directions at approximately the same speed of 20 revolutions per minute (rpm) while being pressed with a calculated Hertz contact pressure of up to 750 MPa by a compression mechanism (in this case, a hydraulic piston) that generated a force of 1.5 tons. The surface of the rotating cylinder was at an ambient temperature of approximately 23°C. 1 g of sugar was fed at a time, and after passing through the nip six times (hereinafter referred to as the number of cycles), the sugar flakes were collected using a doctor blade coated with ceramic material. The blade was appropriately positioned and oriented to detach the flakes from the base surface. This experiment and the resulting flakes were named DF-1. SEM-FIB micrographs (SEM-FIB microsectional observations) were taken with the particles under study placed in an aluminum pin-type SEM mount and covered with double-sided adhesive carbon tape. Images were acquired at an electron high voltage (EHT) of 1.2 kV, an aperture size of 30 μm, and a magnification of X100 (using a Zeiss Crossbeam 340 microscope). Samples were measured at the beginning and end of the peeling process, and the average size of at least 10 individual grains or flakes detectable within the field of view was evaluated. Typically, measurements were taken with 20-30 discrete particles within one or more fields of view. All initial particles approximated spheres, even if their shape was somewhat cubic, and the original size of the sample is shown as the average diameter. Figure 8A is a photograph of sugar grains before being fed into the instrument, and Figure 8B is a photograph of sugar flakes obtained under the conditions described above.

[0183] The conditions and results obtained using the detailed methods described above and similar drying flake methods are summarized in Table 1 for all taste stimulants prepared and supplied in the same quantities. In this table and subsequent tables, SS refers to stainless steel 17-4 PH (R) WC stands for tungsten carbide, and O represents the average diameter of the supplied particles or the diameter of the rotating cylinder. [Table 1]

[0184] Example 2: Paste-flake formation of the sample In this example, granular coffee with an average diameter of approximately 500 μm was flakened by feeding it as a paste of dry powder dispersed in a viscous medium to an apparatus equipped with a nip, as schematically shown in Figure 4. The first and second rotating cylinders 410 and 420 are identical and made of stainless steel 17-4 (R) (Vickers hardness 240HV, average surface roughness R) aThe particles were less than 1,600 nm in diameter, 30 cm in diameter, and 25 cm in axial length. These were rotated in opposite directions at approximately the same speed of 60 rpm while in contact with a calculated pressure of 370 MPa by a compression mechanism (in this case, a hydraulic piston) that generated a force of 7.5 tons. Granular coffee was mixed in a viscous medium of 20 wt.% xanthan gum dissolved in water at a weight ratio of 1:10. The kinematic viscosity of this medium was approximately 10,000 mPa·s, measured at room temperature using a suitable rheometer (Thermo Scientific (Germany) Haake Mars III). The measurement conditions were C20 / 1° spindle, gap 0.052 mm, volume 0.04 ml, shear-vibration frequency sweep 0.1-100 Hz, gamma 1%. The resulting paste was supplied to a nip, and with the surface of the rotating cylinder kept at room temperature, the process of applying a single 0.5 g of paste and passing it through the nip was repeated 20 times. Then, the coffee flakes, at least partially coated with the viscous medium, were collected from the cylinder surface using a doctor blade positioned at the appropriate angle as previously described. This experiment and the resulting flakes were named PF-1. SEM-FIB micrographs were taken at the beginning and end of the flaking process according to the previously described method, and the average size of at least 10 individual particles or flakes detectable within the field of view was evaluated. Figure 9A is a photograph of the coffee particles before being supplied to the apparatus, and Figure 9B is a photograph of the coffee flakes obtained under the above conditions, both taken at a magnification of 100x.

[0185] The conditions and results obtained using the detailed flake formation method described above are summarized in Table 2. [Table 2]

[0186] Example 3: Flake formation of a liquid containing a sample In this example, water-soluble or water-insoluble materials were supplied as solutions or dispersions in a non-viscous liquid and flakebed using an apparatus with a nip schematically shown in Figure 4 or Figure 5. The materials tested are those usable as taste components and / or for other purposes in additional industries and include: A: salts, citric acid, potassium chloride, sodium bicarbonate, and sodium phosphate monohydrate and dihydrate (water-soluble materials); and B: calcium carbonate, dyes, magnesium stearate, silica, and zinc oxide (water-insoluble materials).

[0187] As examples of non-limited uses for the flake-formed water-soluble materials in this example, salt and citric acid (E330) are known for their dual roles as flavor enhancers and food preservatives, but both have the potential to perform many additional functions in other industries. Potassium chloride is used in the food industry as a substitute for sodium chloride and can be used as a thickener, flavor enhancer, and pH adjuster. It can also be used as an electrolyte supplement in the medical field, a fertilizer in agriculture, and a water softener in related industries. On the other hand, sodium bicarbonate (E500) has the property of imparting a slightly bitter and salty taste. It is mainly known as a baking agent for bread and cakes. However, it has diverse uses in other industries as well (e.g., as a medical antacid to relieve heartburn and excess stomach acid, and as a stain remover in personal care products and cleaning products). Sodium phosphate monohydrate (E339(i)) and dihydrate (E339(ii)), also known as monosodium phosphate (MSP) and disodium phosphate (DSP), are relatively tasteless and odorless, but are used in food as emulsifiers, thickeners, leavening agents, moisture-proofing agents, and pH adjusters. In other industries, they are used in detergents and cleaning products, and in the medical field as laxatives (e.g., before colonoscopy).

[0188] As non-limiting examples of the uses of the flaky material of the water-insoluble material shown in this example, silicon dioxide (silica) is used in the construction industry for concrete production, hydraulic fracturing in crystalline form, glass production, sedatives, production of elemental silicon, as a moisture-proof agent for powdered foods such as spices, as a clarifying agent for juices, beers, and wines, for tablet production in pharmaceuticals, and for removing dental plaque in toothpaste. Zinc oxide is very widely used as a filler and white pigment. It is also included in some rubber, glass, and ceramic products and is used as a catalyst in the chemical industry. It is also used as an anti-rust agent and anti-mold agent for paints. Since zinc is an essential trace element, it is also added to fertilizers, animal feeds, and vitamin supplements. It is also used in cosmetics and medical products due to its antibacterial action and deodorizing effect. Due to its property of strongly absorbing ultraviolet (UV) light, it is used in sunscreen products. Near-infrared (NIR) dyes (e.g., NIR983A of QCR Solutions Corp) are used for generating images read by special infrared detectors and are utilized in security solutions from images that fade from QR codes to semi-erased images, as research tools in chemical biology and the medical field, and for diagnostic imaging. Tumor-specific imaging with NIR dyes may open the way to photothermal therapy and photodynamic therapy. Magnesium stearate is used in the food industry and the pharmaceutical industry as an emulsifier, binder, thickener, moisture-proof agent, lubricant, mold release agent, and defoaming agent. The various uses of calcium carbonate have already been described and will not be repeated here..

[0189] The procedure involved briefly grinding ordinary table salt (sodium chloride, NaCl) with an average particle size of approximately 500 μm in a coffee mill to produce fine salt with an average particle size of approximately 50 μm. This fine salt was mixed with water in a 1:3 weight ratio at room temperature and stirred until completely dissolved. For reference, this solution is considered nearly saturated, with a sodium chloride weight percentage concentration of 25 wt.% relative to the total weight of the solution. In contrast, a solution containing approximately 35 g of sodium chloride per 100 g of pure water (i.e., approximately 26.5 wt.%) relative to the total weight of the solution) at the same temperature becomes saturated. The resulting liquid raw material was supplied to the nip of the apparatus schematically shown in Figure 4. Rotating cylinders 41 and 420 are both made of stainless steel 17-4 PH. (R) (Vickers hardness 240 HV, average surface roughness R) a The particles were less than 1,600 nm in diameter, 30 cm in diameter, and 25 cm in axial length. These were rotated in the opposite direction at approximately the same speed of 60 rpm while being compressed by a compression mechanism (hydraulic piston with a force of 7.5 tons) with a calculated Hertz contact pressure of 370 MPa. The cylinders were rotated in the opposite direction while the surface of the rotating cylinders was kept at room temperature. 0.5 ml of liquid was applied once to the approximate center of the cylinder, allowing the liquid to spread along the nip in both directions parallel to the axis. After passing the nip 38 times, the salt flakes were collected using a doctor blade adjusted to the appropriate orientation as described above. The flakes obtained in this experiment were named LF-1. SEM-FIB micrographs were taken at the beginning and end of the flake formation process according to the method described earlier, and the average size of at least 10 individual grains or flakes detectable within the field of view was evaluated. Figure 10A is a 100x magnified image of the salt particles before they were dissolved and supplied to the apparatus, and Figure 10B is a 1,000x magnified image of the salt flakes obtained under the above conditions.

[0190] The conditions and results obtained by the above detailed method and similar liquid stripping methods are summarized in Table 3A and the following paragraphs when the material is water-soluble, and in Table 3B when the material is water-insoluble. In each part and example of this table, water is pure double-distilled water, and Citric Ac. represents citric acid. In the case of LF-2 and LF-3, the surfaces of the rotating cylinders 410 and 420 were preheated to the desired temperature by blowing hot air onto the rotating surfaces. Further, the liquid stocks of the salt solution and the salt dispersion were applied at the same temperature obtained by stirring on a hot plate. In the case of LF-4 and LF-5, the apparatus included a series of nips as schematically shown in FIG. 5. In LF-4, the rotating cylinders 510, 520, and 530 were the same as those described in Example 1. In LF-5, a series of six identical cylinders were arranged linearly, allowing a single flow through each nip, continuous application of the liquid raw material to the first cylinder, and continuous collection of the flakes of the flavoring substance at the sixth cylinder.

Table 3A

[0191] FIG. 11A is a 100-fold magnified photograph of salt grains before being dispersed and supplied to the apparatus, and FIG. 11B is a 1,000-fold magnified photograph of salt flakes obtained in LF-3 under the above conditions.

[0192] For LF-1 to LF-6, in the following experiments not described in the previous table, 0.5 ml of the liquid stock was administered once near the center of the cylinder length to promote a uniform distribution of the liquid along the nip.

[0193] In LF-7, the configuration was similar to that described in LF-1, but instead of supplying a solution, a liquid stock was supplied as a dispersion. The stock was prepared by dispersing a salt in an insoluble liquid. Finely ground salt, with an average diameter of approximately 50 μm, was dispersed at a rate of 3 g in 100 ml of isopropyl alcohol. After passing through the nip 10 times, a piece of sodium chloride with 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 was observed. The thickness was almost the same as in LF-1, while the planar dimensions (and aspect ratio) of the piece were relatively larger. In particular, isopropyl alcohol is more volatile than water, and at the room temperature in which the experiment was conducted, pieces were obtained more quickly from the dispersion in alcohol than from the aqueous solution. Figures 12A and 12B are 100x magnified photographs of the particles before being dispersed in an insoluble liquid and supplied to the apparatus, and the piece obtained under the conditions of LF-7, respectively.

[0194] The LF-8 through LF-10 have a similar configuration to the one described for the LF-1, but differ in that the cylinder is rotated at a speed of 120 rpm at room temperature (compared to 60 rpm for the LF-1).

[0195] In LF-8, a nearly saturated solution of a water-soluble substance was prepared by dissolving sodium bicarbonate (NaHCO3) in water at a weight ratio of 1:10. After passing through the nip, the sodium bicarbonate, which was spherical with an average diameter of approximately 70 μm before dissolution, produced flake-like particles 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.

[0196] In LF-9, a nearly saturated solution of a water-soluble substance was prepared by dissolving sodium phosphate dibasic salt (Na2HPO4) in water at a weight ratio of 1:10. As a result,

[0197] After passing through 10 nip passes, the spherical sodium dihydrate phosphate, with an average diameter of approximately 200 μm before dissolution, yielded flakes 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 using this method.

[0198] In LF-10, the raw material for the water-soluble material was prepared by dissolving sodium phosphate monohydrate (NaH2PO4) in water at a weight ratio of 1:14. Using this method, the sodium phosphate monohydrate particles, which were spherical with an average diameter of approximately 400 μm before dissolution, were converted into 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 after passing through the nip 10 times. Figures 13A and 13B are 100x magnified photographs of the sodium phosphate particles before being dispersed and supplied to the apparatus, and the flakes obtained in LF-10 under the above conditions.

[0199] In the LF-11, the cylinder is made of zirconia instead of stainless steel (Vickers hardness 1300 HV, average surface roughness R a The cylinders were fabricated at approximately 250 nm, and each pair had a diameter of 6 cm (not 30 cm) and an axial length of 6 cm. A liquid stock consisting of a solution of ultrafine salt prepared with LF-1 was applied to the cylinders at room temperature while rotating at 300 rpm. The zirconia cylinders were brought into contact with the stock at a calculated Hertz contact pressure of 350 MPa using a properly configured compression mechanism (in this case, a pneumatic piston). The average flake thickness t after passing through the nip was approximately 5 μm, the average longest planar dimension L was approximately 400 μm, and the aspect ratio ASP was approximately 80.

[0200] In LF-12, the cylinders were made of zirconia, with a diameter of 11 cm and an axial length of 25 cm. A liquid raw material consisting of a 25 wt.% potassium chloride (KCl) aqueous solution with an initial particle size of approximately 500 μm was applied to the cylinders, which were heated to 70°C, while rotating at 100 rpm. The zirconia cylinders were brought into contact with a calculated Hertz contact pressure of 225 MPa by a properly tuned pneumatic compression mechanism. After passing through the nip, the flakes had an average thickness t of approximately 25 μm and an average longest planar dimension L of approximately 450 μm.

[0201] The aspect ratio ASP was approximately 18. The LF-13 salt flakes were prepared using a similar setup to that described for LF-12, but the cylinder was heated to 65°C and processed while rotating at 250 rpm.

[0202] Furthermore, while LF-1 to LF-12 involved applying a single dose of 0.5 ml of liquid to the center of the nip, LF-13 involved applying larger doses to multiple locations along the nip to promote uniform distribution of the liquid. In LF-13, a 25 wt.% sodium chloride aqueous solution with a particle size of approximately 500 μm before dissolution was applied simultaneously to three locations along the nip. Approximately 1.2 ml was administered to each location. After 40 treatments following passage through the nip, the average thickness t of the flakes obtained was approximately 25 μm, the average longest planar dimension L was approximately 800 μm, and the aspect ratio ASP was approximately 32.

[0203] Table 3B summarizes the materials and conditions used in the production of LF-14 to LF-18, as well as the details of flake formation of water-insoluble materials (dispersed or dissolved), and the resulting flakes. Here, Mg Ste. represents magnesium stearate. For all samples, the nip configuration followed Figure 4, with two stainless steel cylinders, 30 cm in diameter and 25 cm in axial length, rotated at 60 rpm, and the liquid sample and surface were maintained at room temperature. Furthermore, since the pressure applied by the hydraulic piston was 370 MPa for each sample in this series, this information is omitted from the following tables. In all cases, a single 0.5 ml of liquid raw material was administered to the central position of the nip. [Table 3B]

[0204] LF-14 through LF-17 represent dispersions containing water-insoluble materials that do not dissolve in water at the added concentration. In contrast, LF-18 used a water-insoluble liquid (i.e., acetone) to dissolve the NIR dye. As can be inferred from the dimensions of the flakes obtained in this series of experiments, the flakes typically consist of solid particles periodically compressed as they pass through the nip in the current process. Furthermore, considering the planar dimensions of the flakes, particle aggregation is also likely occurring. This assumption was confirmed by applying a liquid stock containing much smaller dispersed particles. The resulting flakes, under appropriate operating conditions, sometimes exhibited thicknesses exceeding the size of a single particle, particularly a single compressed particle. For example, using ZnO particles ten times smaller with an initial diameter of approximately 0.5 μm, flakes with a thickness exceeding 2 μm were formed.

[0205] Figures 14A and 14B show magnified images (1,000x) of the particles before they were dispersed and supplied to the apparatus, and magnified images (100x) of the flakes obtained with LF-14 under the above conditions.

[0206] Figures 15A and 15B are photographs of NIR dye NIR983A particles, showing the state before dissolving and supplying to the instrument (X1,000x) and the state of the flakes obtained in LF-18 under the above conditions (X1,000x).

[0207] Example 4: Improvement of flake dissolution rate In this example, the solubility of flakes prepared according to Example 3 in water at room temperature was compared to the solubility of different types of unflaked reference samples. Unless otherwise noted, all experiments reported in this and subsequent examples were performed using flakes flaked off the surface of a rotating cylinder using a properly positioned doctor blade.

[0208] The dissolution rate of the flakes consisting of salts was determined by measuring the electrical conductivity of various salt compositions prepared by dissolving the sample or reference samples in water. The ionic conductivity of the solution changes due to the dissolution of salts. 40 mg of the salt sample dried at 120 °C and then stored in a desiccator at room temperature was added to 80 ml of double-distilled water while stirring at 400 rpm at room temperature. The electrical conductivity was measured by applying an alternating voltage through an electrode immersed in the solution sample and measuring the resulting current. The conductivity (i.e., the measured current) increased as long as the salt dissolved and then reached a plateau. The time from the addition of the salt until the steady value of the current was reached was recorded. Each conductivity measurement was repeated at least three times, and the time (seconds) from the start of dissolution until the current reached the steady value was measured with a chronometer and reported as the average value of all repetitions in Table 4.

Table 4

[0209] The dissolution rate was qualitatively evaluated by a method in which a known amount of the sample was placed on a glass slide, a known volume of the solvent was added at a distance until a liquid bridge was formed by the operator, and observed with a confocal microscope at a magnification of x228. For each material, two samples of the uncrushed raw material and the same crushed material were tested. Repeated observations were made for all samples. By this method, it was found that the dissolution rate of sodium phosphate monohydrate and sodium phosphate dihydrate crushed as described in LF-10 and LF-9 respectively in water was clearly faster than in the uncrushed state.

[0210] Example 5: Density of the sample In this example, for the sample pieces of sodium chloride or potassium chloride prepared according to Example 3, the bulk density and tap density were measured based on the uncrushed standard powder (used in the preparation).

[0211] The sample pieces of sodium chloride and potassium chloride were prepared by the methods described in LF-11 and LF-12 respectively. The bulk density p of each sample BThe pre-dried sample is placed in a known volume V B The mass is measured using a precision measuring cylinder filled with a certain substance, and the container is repeatedly struck until the volume does not re-contract. The final steady-state value is then used to measure the volume V. T We estimate the tapping density P from there. γ The following was calculated. Typically, the tapping was performed at a rate of twice per second for one minute. Flake samples were collected from two sources: first, flakes that detached naturally from the surface of a rotating cylinder, and second, flakes that were actively detached by applying a blade to the surface of the rotating cylinder. The blade was positioned in the direction of detaching the flakes. The results are shown in Table 5, where naturally detached flakes are denoted with the subscript S, and actively detached flakes are denoted with the subscript A. Additional information and calculated factors are also shown. [Table 5]

[0212] As is clear from the table above, the flakes prepared by the currently taught method have a volume density p compared to the corresponding reference (unflaked) material. B and tap density P γ The F2 ratio of flake samples (F2 = ρ T / ρ B ) is greater than the same ratio calculated with the corresponding reference material, indicating superior filling capacity.

[0213] Considering the aspect ratio of the flake sample to the granular raw material, the factors calculated based on the above measurements further amplified the difference between the flakes and raw material prepared by the method taught herein. For example, the F3 ratio (F3 = ASP / ρ B ) is 0.85~1.25 cm 3 For the value of / g, at least 60 cm 3 / g is the F4 ratio (F4 = ASP / ρ) T ) is 0.74-0.79 cm 3 At least 40 cm for the / g value 3 It was / g.

[0214] Example 6: Crystal structure analysis of crystalline tastants Crystal structure analysis of salt flakes was performed using X-ray powder diffraction (XRPD) with compressed flake pellets. Data were obtained using a Panalytical Empyrean III multi-purpose diffractometer (K α Data was collected using a pixCEL 3D detector mounted on a line (λ=1.541 Å) in one-dimensional line detection mode, with the X-ray tube operated at v=45 kV and I=40 mA. Each sample was directly fixed to a stainless steel ring-type back-filled sample holder. During measurement, the sample was rotated at 8 revolutions / min, and measurements were taken in the range of 5–140° 2θ. Phase identification and size-strain analysis were performed using Reitveld refinement, combining the HighScore Plus powder diffraction data analysis suite (version 5.1) and the ICDD (International Diffraction Data Center) powder diffraction file (PDF4+) database (2022 edition).

[0215] Pellet 1 was made from standard salt granules with an average particle size of approximately 500 μm (used to be crushed to form ultrafine salt), Pellet 2 was made from ultrafine salt granules with an average particle size of approximately 50 μm (used to be dissolved to form LF-1 flakes), and Pellet 3 was made from LF-1 salt flakes prepared by the method described in Example 3.

[0216] The diffraction peaks obtained from the analyzed samples were relatively similar in position and included known characteristic peaks of sodium chloride (approximately 31.7°, 45.4°, 66.2°, 75.3°, etc.). The diffraction peaks of the flake samples were slightly broader than those obtained from the reference granular samples. Phase identification revealed that all samples contained more than 99.5 wt.% NaCl. The microstrain values ​​(%) and grain sizes of each sample are shown in Table 6. [Table 6]

[0217] As is clear from the table above, the flaky salt produced by this method has a crystal grain size approximately four times smaller and a microstrain value at least three times higher than that of the original raw material. Similar results were observed in additional salt flake samples prepared according to the teachings of this invention. To understand whether these remarkable changes are due to the shape (flaky) of the produced material or to the method of preparation, commercially available salt flakes (trade name: Cargill Alberger) were also used. (R) Shur-Flo (R) A similar analysis was performed on Fine Flake Salt. The crystalline grain size of this control sample was 2,513 Å, and the microstrain was 0.017%, which was close to the results for pellet 1 and different from the results for pellet 3. Therefore, the values ​​observed in flakes freshly prepared by this method are thought to be due to repeated compression during the manufacturing process, rather than the shape of the flakes themselves. Thus, in crystallographic analysis of flakes made from crystalline materials, if the crystalline grain size is smaller and / or the microstrain value is larger than that of the same material prepared by conventional methods, such flakes are presumed to have been prepared by this method. Such identification is easy if the flakes have not been exposed to environmental conditions that are detrimental to the crystal structure. For example, in the case of hygroscopic materials such as salt, exposure to humidity can affect the flakes. Therefore, it is desirable to perform such analysis on freshly prepared flakes or flakes that have been properly stored from factors that affect crystallographic behavior.

[0218] Example 7: A flake-like substance consisting of a mixture of materials containing taste substances. Flaky materials can be prepared from liquid stocks containing multiple ingredients, for example, by combining two or more taste substances. The following mixtures were prepared according to a modification of Example 3, some of which are summarized in Table 7.

[0219] In the first series of experiments, individual taste substances were supplied as a mixing material to jointly form flakes. The first taste substance was sodium chloride, consisting of grains with an initial particle size of approximately 500 μm, dissolved in water in a weight ratio of 1:3 (i.e., 25 wt.%). Using 34 g of this NaCl solution, 16 g of fresh red peppers were mixed with a Ninja Blender (model Nutri-Blender Plus BN303) at 700 watts for approximately 20 seconds, grinding and homogenizing until a smoothie-like mixture was obtained. The mixture was filtered through a cloth to separate the pulp. The separated brownish liquid stock was fed into a nip formed between two identical stainless steel cylinders, as shown in Figure 4. Each cylinder was fitted with a zirconia sleeve, and each sleeved cylinder had a diameter of 11 cm and an axial length of 20 cm. The cylinders were heated to 65°C and brought into contact with each other at a calculated Hertz contact pressure of 365 MPa using a pneumatic piston while rotating at 250 rpm. 1.5 ml of liquid containing salt and chili extracted during the blending process was simultaneously applied to two locations along the nip. Each application amount was 0.75 ml. After passing through the nip, the flakes containing the salt and fresh chili flavor were collected by gravity after 45 passes. The flakes detached from the cylinder over time. This experiment and the resulting flakes were named LF-19, and the average size was evaluated by microscopy according to the method described in detail, with analysis of 20-30 individual particles. The conditions and results of the above liquid flake method for preparing flakes of mixed materials (such as flavored or colored salt) are summarized in Table 7, omitting descriptions of the nip structure and operating settings. [Table 7]

[0220] As described above, all flakes achieved an aspect ratio of 55 or higher. In addition to dimensional evaluation, flavor and / or color were also tested. LF-19 and LF-20 flakes imparted spiciness in addition to their basic salty taste. LF-19 flakes were slightly brownish, LF-20 flakes were pale red, and LF-21 flakes were a stronger red, but there was no change in taste.

[0221] In the second experimental series, the materials constituting the flakes prepared according to the teachings of the present invention were detergents supplied as a mixture. Powdered laundry detergents can cause problems if they do not dissolve properly during the washing process. For example, solid residue may remain, causing white spots on clothing or accumulating in the washing machine drain. This tendency is particularly pronounced when using cold or hard water. Powdered laundry detergents typically consist of surfactants (nonionic, anionic, and / or cationic) for removing dirt, polymers (e.g., to stabilize other components, ensure the detergent's effectiveness under a wide range of conditions, and remove odors), builders (e.g., to prevent removed dirt from returning to clothing), bleaches, oxidizing agents, fabric softeners, pH buffers, enzymes, solvents, colorants, fragrances, etc., some of which may have poor solubility in water under certain conditions.

[0222] A commercially available powdered laundry detergent (Ariel, manufactured by Procter & Gamble) containing relatively coarse particles with an average initial diameter of approximately 500 μm was suspended in water at a weight ratio of 1:9 (i.e., 10 wt.%). This liquid stock suspension was fed into a nip formed between two identical stainless steel cylinders, each 30 cm in diameter and 25 cm in axial length, as shown in Figure 4. The cylinders were brought into contact with each other at a calculated Hertz contact pressure of 370 MPa using a hydraulic piston while rotating at 120 rpm without heating. A single 1 ml of the liquid raw material was applied near the center of the nip, and after 40 cycles of passing through the nip, the flakes containing the detergent mixture were removed from the cylinder surface using a suitable scraper. The flakes obtained from this experiment were named LF-22, and the average dimensions were measured under a microscope after analysis of 20-30 solid particles. The average thickness t of the detergent flakes was approximately 10 μm, the longest planar dimension L was approximately 600 μm, and the calculated aspect ratio was approximately 60.

[0223] In additional experiments, the "coarse" particles of the detergent were briefly ground in a coffee grinder to produce finer detergent particles with an average diameter of approximately 50 μm. These finer detergent particles were suspended in water at a weight ratio of 1:1 (i.e., 50 wt.%), with process and other parameters set similarly to those for LF-22. This experiment and the resulting flakes were named LF-23, and their dimensions were similar to those previously measured for LF-22 flakes.

[0224] The dissolution rates (DT, in seconds) of LF-22 and LF-23 detergent flakes in water were evaluated according to the method described in detail in Example 4, compared to coarse-grained detergent powders prepared directly or indirectly. 110 mg of the sample (LF-22 or LF-23 flakes, or the original coarse grains) was added to 80 ml of water while stirring at 970 rpm. While the reference powder took 13.27 seconds to dissolve, the flakes prepared by the method described above achieved similar solubility approximately 10 times faster, in 1.34 seconds and 1.49 seconds, respectively.

[0225] The volumetric density and tap density of LF-22 detergent flakes were compared to the corresponding densities of the crude detergent powders from which they were prepared. Each density was measured according to the method described in detail in Example 5, in grams per cubic centimeter (g / cm³). 3 The volume density is 0.80 g / cm³ for natural particles of the detergent. 3 From LF-22 flakes, 0.40 g / cm³ 3 It decreased to [a certain value]. Meanwhile, the tap density decreased from 0.93 g / cm³ for the reference to 0.64 g / cm³ for the LF-22 flakes. 3 It decreased to that level. Meanwhile, the tap density was 0.93 g / cm³, which is below the standard value. 3 From LF-22 flakes, 0.64 g / cm³ 3 It decreased to that point.

[0226] Factors calculated based on these measurement results resulted in even greater differences between the flakes prepared using the methods taught herein and the reference material. For example, the current flakes differ from the natural particles of the detergent in 0.08 sec. -1 In contrast, the F1 ratio (F1=ASP / DT) is approximately 44.78 sec. -1 This shows the F2 ratio (F2 = ρ T / ρ B The ratio was approximately 1.60 (compared to 1.16 for the control sample), indicating superior packing ability, and the F3 ratio (F3 = ASP / ρ) B ) is 150 cm 3 / g (1.25 cm of the control sample) 3 ( / g) is the F4 ratio (F4 = ASP / ρ T ) is 93.75 cm 3 / g (approximately 1.08 cm of the control sample) 3 It was / g).

[0227] The results above further support the possibility that materials, mixtures, and pure compounds other than taste substances may also benefit from the teachings of the present invention. In the case of detergents, a dissolution rate of the active ingredient approximately 10 times faster is expected to improve the effectiveness of products containing or comprising the same active ingredient (e.g., laundry powder). Such an improvement in effectiveness would, alternatively or additionally, allow for a reduction in the amount of active ingredient in the final product while maintaining similar effectiveness compared to similar products containing the same active ingredient in a different form (e.g., conventional).

[0228] Example 8: Effects of various parameters on the process and flakes As is readily apparent and as has already been described in detail, several operating parameters can be modified in the method relating to this disclosure. These variables primarily relate to the material supplied to the nip (e.g., application amount, number of application points along the rotating cylinder, application frequency, concentration of material at each dose, properties of the dissolve / dispersion, etc.) and the operating conditions of the appropriate apparatus (e.g., area of ​​the rotating cylinder (axis length and diameter), cylinder speed and temperature, nip length, pressure at the nip, etc.). In this example, the effects of the aforementioned exemplary parameters were examined.

[0229] Unless otherwise specified in the table below, each experiment was repeated by administering a single dose of 1 ml of liquid stock—25 wt% sodium chloride dissolved in water with an initial particle size of approximately 500 μm—at intervals of a few seconds (e.g., less than 1 minute). The dose was administered each time to the central position along the nip, as shown in Figure 4. The dose was administered until the previously administered liquid stock had transformed into a flaky substance that could detach from the rotating cylinder, allowing the cylinder surface to form a new flaking substance by administering another dose. The time between doses was recorded for each experiment as it depended on the operating conditions (cylinder temperature, dimensions and speed, volume and substance concentration per dose, ambient humidity, etc.). Using these observed time intervals, the administration frequency was calculated as the number of doses per hour. For example, if 10 seconds elapsed between two applications in a particular experiment, the application frequency could be said to be 360 ​​times / hour.

[0230] The nip was formed between two identical stainless steel cylinders fitted with zirconia sleeves, each sleeve-fitted cylinder having a diameter of 11 cm and an axial length of 20 cm. The parameters tested included cylinder temperature (25°C, 45°C, 60°C, 75°C, 90°C), cylinder rotation speed (100 rpm, 200 rpm, 250 rpm, 300 rpm, 400 rpm), calculated Hertz contact pressure until the cylinders made contact using a pneumatic piston (110 MPa, 182 MPa, 258 MPa, 365 MPa, 447 MPa), application volume (0.6 ml, 1 ml, 1.8 ml, 3 ml, 6 ml, 9 ml, 10 ml), number of application points along the nip (1 and 3), and final salt concentration in water (25 wt.% and 59 wt.%). The experiment was completed 10 minutes after the initial dose, and the sections collected under various conditions were weighed to assess the yield and analyzed in an appropriate manner to determine the average dimensions and other important characteristics (such as moisture content).

[0231] Details of each experiment (including changes from the main settings and frequency of dose application) and exemplary results are summarized in Tables 8A to 8D below. [Table 8A]

[0232] As can be seen from the table above, collected from a series of experiments applying a single 1 ml dose, increasing the temperature of the rotating cylinder (both heated to the temperatures shown in the table by internal electric heating elements, where applicable) improved the rate of flake formation, as expected from the accelerated evaporation of water from the applied liquid stock, and consequently increased the frequency with which a dose could be applied to the nip of the rotating cylinder.

[0233] Under the conditions of this study, the temperature in the high-temperature range did not appear to have a significant effect on the dimensions of the obtained flakes. All flakes obtained at high temperatures were relatively similar, with an average thickness t of approximately 25 μm, an average longest planar dimension L of approximately 1,200 μm, and an aspect ratio ASP of approximately 48. However, flakes obtained at room temperature were thinner and smaller than those obtained at high temperatures (t approximately 10 μm, L approximately 500 μm), and their aspect ratios were similar at all temperatures. Similar behavior, where production rate and dosing frequency increased as the nip temperature rose, was also observed at additional rotation speeds of 100 rpm, 300 rpm, and 400 rpm.

[0234] In similar experiments, the stock solution was preheated before application to the nip, reaching a temperature similar to that of the rotating cylinder (when heated above ambient temperature). Under the conditions of this study, preheating the liquid to a temperature similar to the cylinder surface temperature did not significantly affect the resulting production rate or flake size. [Table 8B]

[0235] As can be seen from the table above, obtained from a series of experiments using a single 1 ml dose, increasing the cylinder rotation speed improved the flake generation rate, as expected from the increased number of times the coated liquid stock passed through the nip in the same amount of time. This, coupled with the fact that the speed itself promotes evaporation, accelerated the removal of liquid from the coated dose, allowing for more frequent application of the next dose. The generation rate tended to remain constant at higher speeds. Under the conditions of this study, increasing the rotation speed from 100 rpm to 400 rpm did not have a significant effect on the flake dimensions. All obtained flakes were relatively similar, with an average thickness t of approximately 25 μm, an average longest planar dimension L of approximately 1,200 μm, and an aspect ratio ASP of approximately 48. Similar behavior, where the production rate increases with cylinder rotation speed, was also observed at additional temperatures of 45°C, 75°C, and 90°C.

[0236] For comparison, an experiment called LF-LS was conducted at a low speed of 3 rpm using a similar nip. The cylinder was heated to 90°C, and the applied pressure was the same at 365 MPa. The production rate of 60 g / h was equivalent to the production rate achievable at approximately 150 rpm and 60°C, but the rapid decrease in rotational speed affected the size of the resulting flakes. The LF-LS flakes were approximately five times larger (L approximately 6,400 μm) and eight times thicker (t approximately 195 μm) compared to the equivalent produced at high speed (100-400 rpm), and the aspect ratio decreased from 48 at high speed to 33 at low speed. While we do not intend to be bound by any particular theory, it is thought that the reduced speed reduces the number of times the nip passes over a given time (e.g., 10 minutes in this experiment), and as a result, the time the liquid raw material and the film or coating formed therefrom are exposed to the nip's compressive environment is reduced. Furthermore, it is believed that the increased speed will increase the relative velocity between the outer surface of the cylinder and the surrounding air, making it easier to remove any liquid vapor that may be generated. [Table 8C]

[0237] As can be seen from the table above, as the calculated Hertz contact pressure sensed at the nip increases, the frequency of repeated dose application increases, the flake generation rate increases non-linearly, and each tends to plateau at high pressure. Notably, in the stages prior to reaching the plateau, the pressure at the nip also affected the flake thickness and longest planar dimension, although the aspect ratio remained relatively stable.

[0238] Although not shown in the table above, it has also been confirmed that increasing the cylinder surface area achieved by using larger diameter rolls can relatively increase production speed and application frequency, provided that all other parameters are the same except for the dimensions of the resulting flakes. [Table 8D]

[0239] As can be seen from the table above, increasing the volume of stock liquid distributed to the nip during each application reduces the frequency of needing a new dose, leading to a non-linear increase in flake production rate, while larger dose sizes tend to result in a plateau in production rate. The optimal volume for each dose is expected to be determined, among other things, by the cylinder dimensions (setting the length of the nip and the surface area coated by the liquid film), the cylinder temperature, the cylinder rotation speed, and the force applied to reach a predetermined contact pressure at the nip. Interestingly, the volume of the applied dose also affects the flake thickness, but with less effect on the longest planar dimension, and therefore also affects the flake aspect ratio.

[0240] Similar experiments were conducted at 90°C, 250 rpm, and 365 MPa with a 1 ml dose to evaluate the effect of material (in this case, sodium chloride) concentration. Increasing the salt concentration from 25 wt.% to 59 wt.% simultaneously increased the rate of salt flake formation from 244 g / h to 566 g / h, with application frequencies of 976 and 959 doses / hour, respectively. Since the liquid stock containing 59 wt.% salt is an overloaded dispersion rather than a solution, in this experiment, regardless of the final solid content concentration, the sample solution was prepared using ultrafine sodium chloride ground in-house to a particle size of less than 5 μm, rather than the previous 500 μm. Under the conditions of this study, the initial salt concentration in the liquid stock does not appear to have a significant effect on flake size. In all cases, the average thickness t was approximately 18 μm, the average longest planar dimension L was approximately 1,400 μm, and the aspect ratio ASP was approximately 78, showing relatively similar characteristics. Similar behavior, where the production rate increased with the salt concentration in the liquid stock, was also observed at additional temperatures of 45°C and 75°C.

[0241] Similar experiments were conducted at 65°C, 250 rpm, and 365 MPa to test the effect of the number of application points along the nip. The total application volume remained the same each time. When the liquid stock was applied at a single (central) point along the nip (as before) with a dose of 1.8 ml, the salt flake generation rate was found to be 132 g / h. When the same liquid stock was applied at three equally spaced points along the nip, with a dose of 0.6 ml (i.e., 1.8 ml total) administered to each point, the salt flake generation rate increased to 175 g / h. Under the conditions of this study, the number of points along the nip used to apply the liquid stock did not appear to have a significant effect on the flake dimensions. In all cases, the average thickness t was approximately 20 μm, the average longest planar dimension L was approximately 1,200 μm, and the aspect ratio ASP was approximately 60, all of which were relatively similar.

[0242] The inventors found that the torque of the motor rotating the cylinder could be useful in predicting the interval, and therefore the frequency, of subsequent dose applications. During the application of the first dose, the liquid spreading along the nip generates a force resisting the rotation of the cylinder, and this force is thought to gradually decrease as the liquid is removed. Once the flakes formed by the application of the first dose are ready (e.g., relatively dry), the motor rotating the cylinder exhibits a minimum torque required to maintain a substantially constant speed. At this point in the cycle, the flakes can be removed (or detached naturally), and a new dose can be applied upstream of the nip to begin the next preparation cycle. Therefore, over time, as new doses of the flake-forming material are repeatedly applied, the motor's torque value follows a sinusoidal curve. This can be used for a feedback mechanism that monitors the torque of the motor rotating the cylinder. Each time the monitored torque reaches its minimum under operating conditions, a signal is sent to the liquid stock dispenser, and a new dose is released.

[0243] In all the experiments described above, the production rate, expressed in grams per hour, was evaluated by weighing all the flakes produced during a 10-minute run and calculating the predicted weight for 60 minutes based on that. Samples were also taken to measure the moisture content of the flakes. For this purpose, approximately 1 g of each flake produced under the above conditions was placed in an aluminum crucible and its exact weight was measured. The crucible was then placed in an oven set to 120°C for 2 hours to remove residual moisture. The weight of the dried samples was measured and the moisture content was calculated. The moisture content of all flakes produced in this example was less than 1% by weight.

[0244] Example 9: Comparison of flakes from this embodiment with commercially available samples The flakes produced in this example and the above example were compared to commercially available samples (some granular, others classified as "plate-like") produced from the same material. In this example, all test specimens were produced from sodium chloride. Using a 25 wt.% liquid raw material with an initial salt particle size of 500 μm, four types of flakes produced by the method described herein were named LF-24 to LF-27. Their production conditions and measured dimensional averages are shown in Table 9. [Table 9]

[0245] Nine commercially available sodium chloride samples (CS-1 to CS-9) were independently measured for their dimensions using the same microscopy method applied to the aforementioned flakes. The average values ​​of the measured dimensions are shown in Table 10. For samples with significant granularity (aspect ratio of approximately 1), one dimension was ignored and marked with a negative sign. [Table 10]

[0246] As is clear from the table above, none of the comparison salt samples, including some that are commercially available as "flakes," have an aspect ratio exceeding 10. The highest aspect ratios were 7.2 for CS-1 flakes and CS-3 diamond crystal. (R) It was 6.9. CS-3 Diamond Crystal (R) This product features a distinctive hollow pyramidal crystal structure, excellent sensory properties, rapid solubility, strong adhesion, and low density. For reference, Table 9 shows that all flake samples prepared according to this method have an aspect ratio of 35 or greater.

[0247] For LF-24 to LF-27 and CS-1 to CS-9, comparative tests were conducted with a) dissolution rate DT (measured in seconds as detailed in Example 4) with the sample stirring speed set to 400 rpm to 970 rpm; and b) volume density ρ B and tap density ρ T This was measured in grams per cubic centimeter, following the method described in detail in Example 5.

[0248] The results of these comparative studies and the factors derived therefrom are detailed below and summarized in Table 11. [Table 11]

[0249] As is evident from the table above and as confirmed in different experimental series, almost all of the flakes of this disclosure dissolved rapidly in less than approximately 2 seconds, with the majority dissolving in less than 1 second. For comparison, CS-5 (the material used to prepare the flakes of this specification) dissolved in 8.95 seconds in the same experimental series (consistent with the previously reported 8.7 seconds). Furthermore, CS-1 and CS-3, the closest commercially available materials to the flakes in this series, showed dissolution times of at least 3 seconds. This suggests that the flakes of this specification may dissolve more rapidly than existing products considered similar.

[0250] Of particular note is the ratio F1 (F1 = ASP / DT, in seconds) of the sample's aspect ratio ASP to its dissolution rate DT. -1 A significant difference was observed between the inventive flakes and commercially available comparative samples when the F1 coefficient was calculated. The average F1 coefficient of the comparative samples was approximately 0.76, with the highest values ​​for CS-1 and CS-3 being 1.59 and 2.32, respectively. However, the average value of the flakes prepared by the method taught herein was approximately 60 times higher, with the lowest F1 coefficient in this set exceeding 15.

[0251] Regarding the volume density and tap density of the samples, it can generally be seen that the flakes of the present invention have a lower density than commercially available comparative samples. The difference between these two groups is the tap density ρ of each sample. T and volume density ρ B This can be emphasized by calculating the dimensionless ratio F2. This ratio is mathematically F2 = ρ T / ρ B This is expressed as follows. The average tap density of comparative samples is about 20% higher than the volume density (i.e., F2 ~1.19), and in the case of flakes produced by the method of the present invention, this density difference widens to 96% (i.e., F2 ~1.96). This suggests that the flakes of the present invention have superior filling properties compared to existing products, which may make them easier to package, store, and transport, and thus commercially advantageous.

[0252] Of particular note are the aspect ratio (ASP) and volume density (ρ) of the sample. B A significant difference was observed between the flakes of the present invention and commercially available comparison samples when calculating the ratio F3 (in cubic centimeters / gram). The average F3 of the comparison samples was approximately 4.61, while the highest values ​​for CS-1 and CS-3 were 16.7 and 11.8, respectively. The average F3 of the flakes produced by the method of the present invention was more than 40 times higher, and the lowest F3 coefficient in this set exceeded 90.

[0253] Similar results were obtained for the aspect ratio ASP and tap density ρ of the sample. T This was also observed when calculating the ratio F4. F4 is ASP / ρ T(Units are cubic centimeters / gram) and expressed mathematically. The average F4 coefficient of the comparison samples was approximately 3.96, with the highest values ​​observed for CS-1 and CS-3 being 14.18 and 10.58, respectively. In contrast, the average F4 coefficient of the flakes prepared by the method described herein was approximately 25 times higher, with the lowest F4 coefficient in this set exceeding 60.

[0254] In summary of the comparisons performed in this embodiment, the flakes of the present invention are believed to be distinct from existing products considered equivalent. Features characterizing the flakes of the present invention include directly measurable values, such as the flakes being relatively thin and / or having relatively large longest dimensions, and / or values ​​derived from such measurements, such as the calculated aspect ratio between characteristic sizes being relatively higher than that of standard flakes. Such distinguishing features and the possible values ​​for each measurement parameter have been discussed previously and will not be repeated here.

[0255] To highlight the specificity of the flakes of the present invention, the calculable parameters include factors F1 through F4. The limitations set forth below are established primarily based on flakes produced from salt, although they may characterize these factors in some cases. However, as shown in the detergent described in Example 7, the following lower, upper, and / or intermediate ranges are believed not to be limited to this particular material.

[0256] In some cases, the ratio F1 (mathematically expressed as F1 = ASP / DT) of the flake aspect ratio ASP to the dissolution rate DT of the invention is 5 or greater, 10 or greater, 15 or greater, 25 or greater, 50 or greater, 75 or greater, or 100 or greater. In some embodiments, F1 is 500 or less, 400 or less, 300 or less, 200 or less, or 150 or less. In specific cases, F1 is in the range of 5 to 500, 10 to 300, or 10 to 150.

[0257] In some cases, the tap density ρ of the flakes of the present invention T and bulk density ρ B The ratio F2(ρT / ρ B F2 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 some embodiments, F2 is 5.0 or less, less than 4.5, less than 4.0, or less than 3.5. In particular, 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.

[0258] In some cases, the aspect ratio ASP and volume density ρ of the flakes of the present invention B The ratio F3 is mathematically expressed as F3 = ASP / ρ B The ratio F3 of the flake of the invention, represented by ASP to the volume density ρB, is 25 or more, 50 or more, 75 or more, 100 or more, 150 or more, 200 or more, 250 or more, 300 or more, or 350 or more. In some embodiments, F3 is 1,000 or less, 750 or less, 500 or less, or 400 or less. In particular, F3 is between 25 and 1,000, between 50 and 750, between 75 and 500, or between 100 and 400.

[0259] In some cases, the aspect ratio ASP and tap density ρ of the flakes of the invention T The ratio F4 is mathematically given by F4 = ASP / ρ T The ratio F4 of the section ratio ASP to the tap density ρT of the present invention, as represented by , 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 some embodiments, F4 is 500 or less, 400 or less, 300 or less, or 200 or less. In particular, F4 is in the range of 20 to 500, 40 to 400, 60 to 300, or 80 to 200.

[0260] Figures 16A to 16E are 100x magnified images of commercially available table salt produced according to prior art, with an aspect ratio of 2 or greater. These images were taken using the SEM-FIB microscopy method described herein. Figure 16A shows CS-1 (Asp ~7.2) flakes. Figure 16B shows CS-3 (Asp ~6.9) diamond crystals.(R) Cavity particles: Figure 16C shows topping flakes of CS-4 (Asp ~2.4), Figure 16D shows coarse-grained flakes of CS-6 (Asp ~2.7), and Figure 16E shows fine-grained flakes of CS-7 (Asp ~2.4). Figure 16F is shown nearby for convenience of comparison and shows the current flake LF26 (Asp ~53). As can be seen from the figures, most of the particles in the comparison samples are commercialized as flakes by the supplier, but the shapes actually observed are closer to flattened lumps than thin, flat flakes, as can be seen from the relatively low aspect ratio (between 2.4 and 7.2). As is clear from the figures, the high aspect ratio of the current flakes gives them a characteristic shape, and the planar surfaces are relatively smoother compared to the corresponding edges of the samples compared at this magnification.

[0261] Example 10: Compressibility of flakes Similar to Example 9, when flakes prepared according to this instruction were compared with commercially available samples of the same material, the flakes generally had a higher density (ρ) than the commercially available comparison samples. T and / or ρ B ) is low, or tap density ρ T and bulk density ρ B The dimensionless ratio F2 was found to be higher. This suggests that the flakes of this embodiment may have better packing properties than existing products. In this embodiment, we aimed to confirm these results by evaluating the compressibility of the flakes and their ability to recover to their original volume density after compression.

[0262] Flakes designated LF-28 were prepared by periodically supplying 1.5 ml each of 25 wt.% sodium chloride liquid stock to a nip formed between two cylinders with a diameter of 11 cm and an axial length of 20 cm, according to the method described herein. The cylinders were heated to 65°C, rotated at 250 rpm, and brought into contact under a pressure of 365 MPa by a pneumatic piston. The resulting flakes 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 samples were compared with some commercially available samples previously described.

[0263] First, a syringe with an injection capacity of 50 ml was weighed, and the test material was gently filled to a volume of 50 ml. After filling, the syringe was weighed, and the initial density of the sample was measured, and the volume density ρ was determined. B The (grams / cubic centimeter) was calculated. The piston was pushed in and the test material was compressed until it could no longer be compressed. The volume of the compressed material was measured and the compressive density ρ of the sample was determined. C The uncompressible density ρ was calculated. After the samples were left in a compressed state for approximately 18 hours, the piston was removed and the samples were taken out of the cylinder to restore their uncompressible density. The unconstrained samples were gently refilled into each syringe and checked to see if they returned to their original volume of 50 ml or if any changes had occurred that resulted in a different uncompressed volume. DC This was calculated based on the volume recovered by the sample after overnight compression.

[0264] Compression density ρ of each sample C and initial volume density ρ B Dimensionless ratio F5(ρ C / ρ B The compressibility of each sample was evaluated by calculating the compressibility factor. The results and the factors derived from them are summarized in Table 12. [Table 12]

[0265] As is evident from the table above, the comparative samples showed, on average, a compressed density approximately 30% higher than their volumetric density (i.e., F5 ~1.29). However, for flakes prepared by the teaching method herein, the difference between these two densities jumped to three times (i.e., F5 ~3.33). All commercially available samples were recovered after depressurization, and their depressurized density ρ DC The initial volume density ρ B It was identical or similar to the original. On the other hand, the flakes of the present invention exhibited a reduced-pressure density that was slightly higher than the original volume density.

[0266] While not intended to be bound by any particular theory, the aspect ratio of the flakes of the present invention (ASP ~68) is at least an order of magnitude larger than the average aspect ratio of the comparison material (ASP ~3.4, peak value of approximately 7 for CS-1 and CS-3), suggesting that the flakes of the invention may have partially fractured during the experimental compression process. However, even with the fractured flakes, the average of the comparison samples was approximately 0.8 g / cm³. 3 In contrast, approximately 0.4 g / cm³ 3 Relatively low decompression density ρ DC The brittleness of the material, i.e., its ability to deform under compression, depends on the initial aspect ratio. Therefore, a dimensionless factor F6 was calculated based on F5, which estimates the relationship between the initial aspect ratio ASP and compressibility. Mathematically, F6 is expressed as F6 = ASP / F5, and it was found to highlight the difference between this sample and the comparison sample.

[0267] This example confirms that this sample, with its superior F2, F5, and F6 values, possesses better filling capacity than existing products, and is expected to facilitate packaging, storage, and transportation.

[0268] Furthermore, this example provides parameters for calculating additional factors F5 and F6 that highlight the characteristics of this sample. The limitations shown below are established for flakes made from salt, but the lower limits, upper limits, and ranges between them are not considered to be limited to this particular material.

[0269] In some cases, the compressive density ρ of this flake C and initial volume density ρ B The ratio F5 (mathematically F5 = ρ) C / ρ B The F5 (represented by ) is 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 some embodiments, F5 is 10.0 or less, 7.5 or less, 5.0 or less, or 4.0 or less. In specific cases, F5 is in the range of 1.6 to 10.0, 1.8 to 7.5, 2.0 to 5.0, 2.2 to 4.5, or 2.4 to 4.0.

[0270] In some cases, the compression ratio F6 (mathematically expressed as F6 = ASP / F5), estimated from the aspect ratio ASP and F5 of the flakes of the invention, 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 some embodiments, F6 is 200 or less, 150 or less, 100 or less, 75 or less, or 50 or less. In particular, F6 is in the range of 6 to 200, 10 to 150, 20 to 100, 20 to 75, or 20 to 50.

[0271] Example 11: Sensory evaluation of taste samples The effect of the form of a taste substance on the correspondingly perceived taste can be tested using human subjects. Taste substances before being flaked by the methods disclosed herein can be tested "as is" or after being applied to or mixed with food products that do not contain the taste substance. For example, the taste substance can be applied to popcorn or mixed with a relatively tasteless edible gel. The proportion of the reference taste substance or flaked taste substance applied to or mixed with the food is kept the same, and the intensity of the taste provided by the taste flakes is compared. Conversely, after setting the amount of a reference taste substance to a satisfactory level, food samples are prepared by gradually reducing the amount of taste substance flakes until a similar satisfactory level is obtained. This method allows for the establishment of how much the amount of taste substance can be reduced when using flaked taste substances instead of a standard reference taste substance.

[0272] This study evaluated the ability of sodium chloride flakes, prepared according to the LF-26 manufacturing method, to provide a satisfactory saltiness in additive-free french potato slices. The effect of the flavor component flakes of the present invention on the saltiness of potato chips coated with them was compared to that of commercially available CS-8 flakes. One gram of test flakes was uniformly coated onto 100 grams of uncoated french potato slices in a seasoning tumbler drum and evaluated by a panel of at least five trained individuals.

[0273] Trained panels rinsed their mouths with mineral water between each evaluation and consumed similar amounts of food samples, assigning a taste intensity value to each sample from a baseline (0, representing no change in taste compared to a food control coated with CS-8 flakes) to a maximum of 10, which represents an intensity exceeding this baseline. Each panelist repeated the sensory evaluation four times at 5-minute intervals, consuming food samples randomly assigned to either reference CS-8 or the currently used LF-26 flakes in each evaluation round.

[0274] The taste score for each food sample was calculated by summing the results of all panel members and repeated tests and dividing by the total number of tests to obtain a calculated mean taste score for each food sample. In the first series of tests, it was observed that LF-26 flakes provided a significantly stronger salty taste than commercial CS-8 flakes used as a reference, when the weight of salt flakes per chip was equivalent. In the second experiment, the relative amount of LF-26 flakes on bare potato slices was gradually reduced (e.g., -30%, -50%, -75%) until a taste similar to that of CS-8 flakes applied to 1g of potato slices per 100g was obtained. As a result, it was found that even with a reduction of approximately 30-40% in the weight of LF-26 (i.e., 0.6-0.7g of salt per 100g of potato chips), a taste similar to the reference product could be provided.

[0275] This experiment was repeated using sodium chloride flakes prepared similarly to LF-13, compared to commercially available CS-8. All trained panel members (8 in this study) confirmed that it was possible to provide a taste similar to the CS-8 standard (applied at 1g of salt per 100g of potato chips) while reducing the relative amount of LF-13 flakes applied to bare potato slices by at least approximately 30–35% (i.e., 0.65–0.70g of salt per 100g of potato chips). This estimate is based on the observation that when the amount of flakes according to the invention was reduced to 75% of the weight of the standard flakes, no panel member could distinguish between the test sample and the standard. When the amount of LF-13 was reduced to 50% of the CS-8 standard, a quarter of the panel members identified chips using the tested flakes as "less salty," and when the amount of tested flakes was further reduced to 25% of the standard, half of the panel members perceived a difference in taste.

[0276] The salt used as a reference in this sensory evaluation has been reported to have a sodium-reducing effect compared to conventional table salt. Cargill conducted consumer sensory evaluations, and Alberger (R) It has been reported that fine flake salt (i.e., CS-8) ​​provides equivalent flavor to table salt in smaller quantities and reduces sodium by 30%. In other words, 1g of CS-8 provides the same saltiness as approximately 1.4g of table salt. The results of this experiment showed that when the amount of flakes used according to this instruction was less than approximately 0.65-0.7g, it provided the same taste as 1g of CS-8 (when applied to 100g of potato chips). Therefore, it can be inferred that 0.65-0.7g or less of LF-13 or LF-26 flakes is taste-equivalent to approximately 1.4g of table salt. Thus, the sodium chloride flakes of the present invention have the potential to reduce sodium by at least 50% compared to conventional table salt.

[0277] Example 12: Pre-treatment of raw materials As reported in previous examples, the raw materials to be flaked and / or the liquid raw materials prepared therefrom can be pre-treated before use in this method or apparatus. For example, in Example 3, raw materials with an average diameter of approximately 500 μm were ground to an average diameter of approximately 50 μm to facilitate the preparation of the stock solution; in Example 8, raw materials with an average diameter of approximately 500 μm were ground to an average diameter of approximately 5 μm to facilitate the preparation of the stock solution and stock dispersion. In the same example, the stock solution was pre-heated to match the surface temperature of the rotating cylinder. These pre-treatments were carried out as a separate step before applying the liquid raw materials to the surface of the rotating cylinder. In this example, the pre-treatment was carried out in conjunction with the following steps of the flaking process.

[0278] The pretreatment apparatus was structurally similar to the flaking apparatus described previously. It consisted of two cylinders with zirconia outer surfaces, each fitted with a zirconia sleeve. The cylinders, 11 cm in diameter and 20 cm in axial length, were heated to 65°C, rotated at 250 rpm, and brought into contact at a calculated Hertz contact pressure of 365 MPa using a pneumatic piston. The rotation axis of the pretreatment apparatus cylinders was positioned slightly inclined relative to the horizontal plane, resulting in the nip height being higher at one end than the other. Furthermore, in contrast to the aforementioned flaking experiment, the liquid raw material (a solution of 25 wt.% NaCl dissolved in water) was continuously supplied to the upper end of the nip at a sufficient flow rate (approximately 33 ml / min), forming a liquid reservoir along the entire nip. Overflow occurred at the lower end of the nip. This supply rate was excessive for flake production under similar conditions, but it continued until the material moving along the nip was sheared upstream and overflowed at its lower end. The substance supplied at the upper end of the nip was a clear solution, while the substance discharged at the lower end was a whitish sludge, confirming at least an initial concentration effect. This was confirmed by gravimetric analysis, which showed the sludge's salinity to be at least 50 wt.%, and the calculated flow rate at the discharge point was approximately 16 ml / min at its maximum. The kinematic viscosity of the concentrate was found at room temperature and a shear rate of 100 s. -1It was measured at approximately 1,500 mPa·s.

[0279] Without being bound by any particular theory, it is thought that some of the water contained in the liquid stock is removed as it passes through the nip, and non-volatile substances are recirculated to the upstream pool, and despite continuous supply from the top of the liquid stock, the concentration of solid material in the pool gradually increased. As the solution changes into a dispersion (as indicated by the increase in the turbidity of the liquid), the solidified particles are subjected to shear forces generated by the rotating cylinder. This resulted in a second effect: particle size reduction of the material. In this experiment, salt with an initial diameter of 500 μm dissolved in the liquid supplied to the top of the nip was sheared into cubic particles with an average side length of approximately 2.5 μm in the resulting sludge. This dramatic particle size reduction was achieved in a few seconds (less than 10 seconds with current equipment). For comparison, a standard ball mill method required 1.5 hours for similar particle size reduction. This pretreatment of the liquid raw material can be used as a raw material supplied inline to the nip of a flake apparatus, as described, for example, in Example 8 assuming a raw material of 59 wt.% salt, to simultaneously achieve material concentration and particle size reduction during dispersion.

[0280] Example 13: Specific surface area of ​​flakes Using this method, flakes of material prepared according to precedents can be measured for their specific surface area (SSA) and compared to the specific surface area of ​​the corresponding material before flaking. The surface area of ​​the sample is measured by gas adsorption according to a standard method using the ASAP 2020 Accelerated Surface Area and Porosimetry System from Micromeritics Instrument Corporation. Briefly, the sample is weighed, a packing rod is inserted into a measuring glass tube with known free space, and it is sealed with a frit seal that allows gas to enter and exit. The sample is dried overnight under vacuum. The dried sample is subjected to a vacuum step under heating, reaching a target temperature of 30°C at a heating rate of 1°C / min. Vacuuming is performed at a rate of 5 mmHg / s and continued until a vacuum of 10 μmHg is reached. The measuring glass tube is transferred to liquid nitrogen and a nitrogen gas injection step is performed. This step is continued for 10 minutes to allow for the physical adsorption of molecules to the surface of the dried sample. Excess nitrogen gas is evacuated under a vacuum of 100 mmHg, and measurements are collected for 120 minutes with a 5-second equilibrium interval. Each measurement is repeated at least three times, and the specific surface area of ​​each sample is calculated using the BET method.

[0281] Example 14: Fluidity of flakes The influence of material morphology on fluidity can be determined by appropriate methods. For example, if flakes or reference particles of a water-soluble substance do not flow regularly and consistently freely through the calibrated orifice of a flowmeter specified by Hall flowmeters (ASTM B213) or Kearney flowmeters (ASTM B964), the weight of the sample flowing through the orifice of that flowmeter can be measured.

[0282] The experiment should preferably be conducted in a temperature and humidity controlled laboratory to ensure relatively low relative humidity and stable temperature conditions. Since the flow is measured without the use of auxiliary means, a dry, clean flowmeter funnel is fixed on a stand placed on a stable workbench. With the funnel outlet sealed, a predetermined weight of sample, dried at 120°C for 2 hours, is carefully placed into the funnel without tapping, vibrating, or moving the sample in a way that would artificially stack it. The outlet is opened, and the timing device is started simultaneously to measure the time it takes for the last sample to exit the outlet. Multiple flow tests can be performed, using fresh, dry samples in each test, and the flow times corresponding to the same sample can be averaged. Flow times for different samples, or the average values ​​of repeated tests performed with different samples, can be compared. The flow rate is calculated and normalized based on a funnel-dependent factor.

[0283] Overview of the work example As is evident from the table above and the results, the method and exemplary apparatus for carrying them out are suitable for the rapid production of microflakes, and in some experiments produced a sufficient proportion of separable submicroflakes. All flakes, regardless of the average thickness range (approximately 0.5–200 μm), exhibited a dimensionless major-to-major ratio of at least approximately 5 (see LF-6), with the majority being at least 30 or greater. The current flakes are all composed of solid particles, which are at least compressed, and in most cases, it is thought that the particle clusters aggregate due to the pressure by which the liquid is gradually compressed as the liquid is removed during separation from the liquid.

[0284] The feasibility of current flakening methods and apparatus has been demonstrated primarily with taste substances (single or in mixtures), but this is not limited to such types of compounds. Water-soluble and water-insoluble materials with additional applications in industries other than the food industry have also been successfully flaked. Flakes of water-soluble materials can be produced by applying a relatively low-viscosity liquid to a movable surface and supplying it as a solution (e.g., LF-1 to LF-6, and LF-8 to LF-13) or dispersion (e.g., LF-7) when a compression nip is formed between the liquid and the opposing surface. A similar phenomenon has been observed with insoluble materials by flaking them from a dispersion (e.g., LF-14 to LF-17) or solution (e.g., LF-18).

[0285] Advantageously, the flakes prepared by this method showed improved dissolution rates compared to the reference material (e.g., sample) before flaking. In quantitative measurements of salt or detergent mixtures (see LF-1 and LF-22), a dissolution rate acceleration of approximately 10 times was observed. Similar increases in dissolution rates have also been reported for sodium phosphate dihydrate and sodium phosphate monohydrate (see LF-9 and LF-10). Interestingly, the volume density and tumble density of the actively flaked flakes of the salts with improved dissolution rates were also approximately 10% of the volume density or tumble density of the reference salt, respectively. Furthermore, notably, in the case of taprants with a crystalline structure, the flaked taprants exhibited a structure with at least approximately 3 times more microstrain compared to the crystals of the reference taprant (those dissolved to form the flakes). The size of the crystal particles in the flakes was found to be approximately 36 times smaller than that of the reference granular taste substance, further supporting the idea that the flakes (e.g., taste substance) prepared by the method disclosed herein were subject to constraints not typically present in naturally growing crystals (e.g., compressive force sensed when compressed at the nip(s)). The flakes described herein exhibited compressibility suitable for standard commercial processes.

[0286] When sodium chloride flakes were considered as an exemplary taste substance, sensory evaluation tests showed that they provided a flavor comparable to the reference salt while being present in relatively small amounts. Current experiments suggest the possibility of reducing sodium content by at least 50% compared to regular table salt.

[0287] These methods have been shown to be applicable not only to flavor and food industries, but also to different materials that impart diverse activities to flakes. Importantly, flakes produced by this method or apparatus have been shown to have unique properties, expressed in measurable characteristics and values ​​that can be calculated from them, including ratios of ASP to F1 through F6. In some cases, these flakes can be distinguished by one or more of the above characteristics.

[0288] Features described herein that we consider to be uniquely inventive, in addition to those asserted in the attached claims, are specified in the following clauses to provide a fair basis for future divisional patent applications.

[0289] 1. A method for producing flakes, comprising the steps of: a) preparing a stock containing at least one material; b) applying the stock to a first movable surface to form a uniform layer of the stock of material thereon; c) periodically passing the material through at least one nip formed by pressing the first movable surface toward an opposing surface; thereby gradually forming solid particles of the material, which are compressed and aggregated in step c), thereby forming flakes made from the material.

[0290] 2. The method according to paragraph 1, further comprising the step of applying the raw materials in a dry state.

[0291] 3. The method according to paragraph 1, wherein the raw material is applied in paste form, the kinematic viscosity of the paste raw material is 5,000 millipascals·seconds (mPa·s) or more, and further includes a step of gradually removing the liquid present in the paste raw material.

[0292] 4. The method of paragraph 1, wherein the raw material is applied as a liquid raw material, and if necessary the viscosity is 5,000 mPa·s or less, the method further includes a step of gradually removing the liquid present in the liquid raw material.

[0293] 5. In the method of Clause 3 or Clause 4, the liquid present in the paste raw material or liquid raw material is selected to react with at least one material contained in the raw material, thereby causing the chemical composition of the flake to differ from the chemical composition of one or more materials present in the raw material.

[0294] 6. The method according to any one of claims 3 to 5, wherein the liquid is removed from the paste stock or liquid stock by evaporation in one or more cycles.

[0295] 7. In any of the methods of claims 1 to 6, the average thickness t of the flakes does not exceed 200 μm.

[0296] 8. A method according to any one of claims 1 to 7, wherein the average major axis ratio ASP (ratio of the longest planar dimension L of the flake to the maximum thickness t) is 10:1 or greater on average.

[0297] 9. A method according to any of paragraphs 1 to 8, wherein the flakes, which consist of compressed and aggregated particles of a solid material, have a liquid content of less than 5% by weight.

[0298] 10. A method according to any of the methods described in paragraphs 1 to 9, wherein the separation distance at the nip of opposing nip-forming surfaces is dynamically variable, decreasing to 1 μm or less when the raw material or its derived flakes are absent, and optionally up to 400 μm when the raw material is present.

[0299] 11. An apparatus for producing flakes from a stock consisting of at least one material, the apparatus comprising: a) Support frame, b) Two cylinders mounted on a support frame, with at least one cylinder movable relative to the support frame, c) A force transmission mechanism that applies force to bring the cylinders into contact with each other, and d) A device comprising a drive motor for rotating at least one cylinder, e) A coating apparatus for coating a raw material into at least one cylinder to form a film containing solid particles of the material on the surfaces of both cylinders, configured such that the number or concentration of solid particles increases each time the film passes through a nip during use, and f) A controller that adjusts the application speed of the raw material based on an empirically created table that predicts such a speed, based on one of the following: the rotational speed of the motor-driven cylinder, the force acting on the nip, the surface temperature of the cylinder, or the composition of the raw material.

[0300] 12. In the apparatus of paragraph 11, the measuring device is adapted to apply a paste-like or liquid stock, and the number or concentration of solid particles gradually increases each time the film passes through the nip during use.

[0301] 13. The apparatus according to paragraph 12, further comprising a heating device for facilitating the removal of liquid contained in the paste or liquid raw material.

[0302] 14. An apparatus for producing flakes from raw materials consisting of at least one material, the apparatus is: a) Support frame, b) Two cylinders mounted on the frame, with at least one cylinder being movable relative to the support frame, c) a force transmission mechanism that applies force to bring the cylinders into contact with each other, and d) a drive motor that rotates at least one of the two cylinders. e) a dispensing device for dispensing raw material into at least one cylinder to form a film containing solid particles of the material, the number or concentration of solid particles increasing each time the film passes through the nip during use, f) a torque measuring device for measuring the torque applied by the drive motor, the torque varying according to the proportion of solid particles in the film, and g) a controller for adjusting the rate at which the material is supplied by the material supply device according to the measured torque.

[0303] 15. Apparatus for producing flakes from a liquid raw material, wherein the liquid raw material contains a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame; b) two cylinders mounted on the support frame, with at least one cylinder movable relative to the support frame; c) a force transmission mechanism that applies a force to press the cylinders into contact with each other; and d) a drive motor for rotating at least one of the two cylinders, characterized in that: e) the apparatus coats at least one cylinder with the liquid raw material to form a thin film on the surface of the cylinder, the concentration of the solid material in the thin film increases each time the thin film passes through a nip, resulting in the formation of flakes of the material; and f) a controller that adjusts the rate of the liquid raw material being coated onto the cylinder to match the rate at which the liquid is lost from the thin film as the thin film continues to pass through the nip.

[0304] 16. Apparatus for producing flakes from a liquid raw material, comprising a material dissolved or dispersed in a liquid, the apparatus comprising: a) a support frame; b) two cylinders mounted on the support frame, with at least one cylinder movable relative to the support frame; c) a force transmission mechanism that applies force to bring the cylinders into contact with each other; d) a drive motor for rotating at least one of the cylinders; and e) an apparatus for coating a film of the liquid raw material onto the cylinders while the cylinders are rotating, wherein at least one of the cylinders is internally heated, and the concentration of the solid material increases each time the film passes through a nip, resulting in the formation of flakes of the material on the cylinders.

[0305] 17. A flake made of sodium chloride, wherein the material has at least one of the following crystallographic characteristics: A - The size of the sodium chloride crystal grains in the flakes is at least 20%, at least 30%, at least 40%, or at least 50% smaller than the size of the unflaked sodium chloride crystal grains for reference, and the size of the crystal grains in the flakes is at least twice, at least three times, or at least four times smaller than the size of the reference crystal grains, as is required; and B- The microstrain value of sodium chloride in flakes shall be at least 20%, at least 30%, at least 40%, or at least 50% of the microstrain value of reference unflaked sodium chloride. However, the microstrain value in flakes shall optionally be at least twice, at least three times, or at least four times the microstrain value of the reference unflaked sodium chloride.

[0306] 18. Flakes made from at least one material, having thin planar dimensions, wherein each flake has a longest dimension, the multiple flakes have an average longest dimension (L) in the plane, each flake has a maximum thickness, the multiple flakes have an average maximum thickness (t) from one side of the plane to the other, and the multiple flakes have an average aspect ratio (Asp=L / t) of at least 10:1, due to the flakes having a dimensionless aspect ratio between the longest dimension and the maximum thickness. The flakes are characterized by at least three structural features described in any one of a) to j) below, and at least one, at least two, or at least three features described in any one of k) to y) below: a) t is 200 μm, 150 μm, 100 μm, 80 μm, 60 μm, or 40 μm or less; b) t is 20 μm, 18 μm, 16 μm, 14 μm, 12 μm, or 10 μm or less; c) t is 9 μm, 8 μm, 7 μm, 6 μm, 5 μm, 4 μm, 3 μm, or 2 μm or less; d) t is 1 μm, 0.9 μm, 0.8 μm, 0.7 μm, 0.6 μm, 0.5 μm, 0.4 μm, or 0.3 μm or less; e) t is 50 nm or greater, 100 nm or greater, 150 nm or greater, or 200 nm or greater; f) L is 10,000 μm or less, 7,500 μm or less, 5,000 μm or less, 4,000 μm or less, 3,000 μm or less, 2,000 μm or less, 1,500 μm or less, or 1,000 μm or less; g) L is 500 μm or less, 400 μm or less, 300 μm or less, 200 μm or less, 100 μm or less, or 50 μm or less; 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; i) Asp must be at least 20:1, at least 30:1, at least 40:1, or at least 50:1; j) Asp is at most 150:1, at most 125:1, at most 100:1, or at most 75:1; k) The specific surface area SSA of the piece is at least 0.001 m². 2 / g, at least 0.005 m 2 / g, at least 0.01 m 2 / g, at least 0.05 m 2 / g, at least 0.1 m 2 / g, at least 0.2 m 2 / g, at least 0.3 m 2 / g, at least 0.4 m 2 / g, or at least 0.5 m 2 / g; l) The flakes have a maximum SSA (Specific Surface Area) of 10 m². 2 / g, up to 8 m 2 / g, up to 6 m 2 / g, up to 4 m 2 / g, or up to 2 m 2 / g is; m) The dissolution rate DT of the flakes (measurable in water at 23°C) and the ratio of F1 = ASP / DT are at least 5, at least 10, at least 15, at least 25, at least 50, at least 75, or at least 100; n) The flakes have a measurable dissolution rate DT in water at 23°C, and the ratio F1=ASP / DT is 500 or less, 400 or less, 300 or less, 200 or less, or 150 or less; o) Flakes have a tap density of ρ T and bulk density ρ B It has the ratio F2 = ρ T / ρ B is at least 1.25, at least 1.5, at least 1.75, at least 2, at least 2.25, at least 2.5, or at least 2.75; p) Flakes have a tap density ρ T and bulk density ρ B It has the ratio F2 = ρ T / ρ B is 5 or less, 4.5 or less, 4 or less, or 3.5 or less; q) Flakes are ρ B The volume density and F3 = ASP / ρ B The ratio is at least 25, at least 50, at least 75, at least 100, at least 150, at least 200, at least 250, at least 300, or at least 350; r) Volume density of the flake ρ B The ratio F3 = ASP / ρ B The maximum is 1,000, 750, 500, or 400; s) Tap density of flakes ρ T and ratio F4 = ASP / ρ T However, it is at least 20, at least 40, at least 60, at least 80, at least 100, at least 120, at least 140, at least 160, or at least 180; t) Tap density of flakes ρ T The ratio F4 = ASP / ρ T The maximum is 500, 400, 300, or 200; u) The flake has a compressible density of ρ C and volume density ρ B It has the ratio F5 = ρ C / ρ B is at least 1.6, at least 1.8, at least 2.0, at least 2.2, at least 2.4, at least 2.6, at least 2.8, at least 3.0, or at least 3.2; v) The flake has a compressible density ρ C and volume density ρ B It has the ratio F5 = ρ C / ρ B is 10 or less, 7.5 or less, 5 or less, or 4 or less; w) Flake has a compressible density of ρ C and volume density ρ B It has the ratio F6 = (ASP × ρ B ) / ρ Cis at least 6, at least 10, at least 15, at least 20, at least 25, at least 30, at least 35, or at least 40; x) The flake has a compressible density of ρ C and volume density ρ B It has the ratio F6 = (ASP × ρ B ) / ρ C is up to 200, up to 150, up to 100, up to 75, or up to 50; and y) The flake material is a crystalline material.

[0307] 19. Flakes as described in paragraph 17 or 18, manufactured by any method and / or apparatus described herein or included in the claims.

[0308] 20. Flakes as described in paragraph 18 or 19, wherein at least one of the one or more materials constituting the flakes is a flavor component adapted to flavor a product contained in or constituting the same product.

[0309] 21. A flake according to any of paragraphs 18 to 19, wherein the material is sodium chloride and the crystalline material has at least one of the following crystallographic features: A - The size of the sodium chloride crystal grains in the flake is at least 20%, at least 30%, at least 40%, or at least 50% smaller than the size of the reference unflaked sodium chloride crystal grains; the size of the crystal grains in the flake is optionally at least 2 times, at least 3 times, or at least 4 times smaller than the size of the reference crystal grains; and B- The microstrain value of sodium chloride in the flake is at least 20%, at least 30%, at least 40%, or at least 50% greater than the microstrain value of reference non-flake sodium chloride, and the percentage value of microstrain in the flake is at least 2 times, at least 3 times, or at least 4 times the percentage value of the reference microstrain.

[0310] 22. In a flake as described in paragraph 18 or 19, at least one of the one or more materials constituting the flake is an active or inactive component that provides effects and / or manufacturing advantages to a product containing or consisting of the flake.

[0311] 23. A food product comprising the flakes described in any of paragraphs 17 to 20, wherein the flakes are placed on and / or contained within the food product and do not dissolve in the food product.

[0312] 24. Products containing the flakes described in any of headings 18, 19, or 22.

[0313] 25. A method for improving a food product, comprising the step of incorporating a flake described in any of paragraphs 20 to 22 into the food product.

[0314] 26. A method for improving the effect of a manufactured product, comprising the step of incorporating the flakes described in any of paragraphs 19, 22, and 24 into the manufactured product.

[0315] 27. A method for reducing the amount of a taste component that provides a desired taste to a food. The method includes replacing at least a portion, or optionally all, of the taste component in the food with the flakes described in paragraph 20 or 21.

[0316] 28. A method for reducing the amount of an active or inactive component suitable for imparting a desired efficacy to a manufactured product. The method includes replacing at least a portion, and optionally all, of the component in the manufactured product with the flakes described in paragraph 22.

[0317] In the specification, for clarity, certain features described in separate embodiments may be provided in combination in a single embodiment. Conversely, for brevity, various features of the specification described in a single embodiment may be provided separately, as appropriate subcombinations, or in appropriate form in other embodiments described in the specification. Certain functions described in various embodiments are not considered essential functions of the embodiment unless the embodiment would not function without that element.

[0318] This disclosure is illustrated with various specific embodiments for illustrative purposes only, but such specifically disclosed embodiments are not to be considered limiting. Those skilled in the art will devise many other alternatives, modifications, and variations of such embodiments based on the applicant's disclosure herein. Therefore, this specification is not limited to, but encompasses, all alternatives, modifications, and variations that fall within the spirit and scope of this specification and its scope.

[0319] In the description and claims herein, the verbs “include,” “incorporate,” and “have,” as well as their conjugations, are used to indicate that the object of such verb does not constitute a complete enumeration of the characteristics, components, steps, elements, or parts of the subject of such verb. However, it is assumed that the compositions of the Disclosure essentially include or consist of the components described, the methods of the Disclosure essentially include or consist of the process steps described, and the apparatus of the Disclosure essentially includes or consists of the apparatus described.

[0320] Terms describing position or motion (e.g., “up,” “down,” “right,” “left,” “bottom,” “down,” “lowered,” “low,” “up,” “up,” “risen,” “high,” “vertical,” “horizontal,” “front,” “back,” “rear,” “forward,” “upstream,” and “downstream,” and their grammatical variations are used herein for illustrative purposes only, to describe the relative position, arrangement, or movement of a particular component, or to indicate a first component and a second component in the current illustration, or both. These terms do not necessarily mean, for example, that a “down” component is below an “up” component. Such directions, components, or both, may be inverted, rotated, moved in space, arranged or positioned diagonally, arranged horizontally or vertically, or similarly modified.

[0321] In this specification, the singular forms "a," "that," and the definite article refer to the plural form and mean "at least one" or "one or more" unless the context explicitly indicates otherwise. In this specification, the expression "at least one of A and B" means either A or B, and in some examples, it may mean both A and B.

[0322] Unless otherwise specified, the use of the phrase "and / or" between the last two items in a list of options indicates that it is appropriate and possible to select one or more of the listed options.

[0323] The term “exemplary” in this specification means “serving as an example, case, or illustrative example.” An example described as exemplary should not be construed as preferable or advantageous to other examples, nor should it preclude the adoption of features from other examples.

[0324] In this specification, unless otherwise specified, the adjectives “substantially,” “approximately,” and “about” modify the conditions or relationships of the characteristics or features of the currently disclosed embodiments of the invention, meaning that the conditions or characteristics are within the tolerances permissible for the operation in the intended use of the embodiment, or within the range of variation arising from the measurement method and / or measuring instrument. For example, where “about” or “approximately” precedes a number, this could mean ±15%, ±10%, or ±5%, or a suitable ± variation within these ranges, and in some cases, it could mean an exact value. Furthermore, unless otherwise specified, the terms of the embodiments disclosed herein (e.g., numerical values), even without such adjectives, have a tolerance for deviation from the exact meaning of the relevant term, and the embodiments or their relevant parts are to be interpreted as operating and functioning as described, or as being able to achieve the operation and function as understood by those skilled in the art.

Claims

1. A method for producing flakes, wherein the method is a) A step of supplying a liquid raw material in which at least one solid material is dissolved or dispersed in a liquid, b) A step of applying the liquid raw material to the first movable surface to form a thin film of the liquid raw material on the first movable surface. c) Periodically, until the liquid content of the flakes is less than 5% by weight, i) evaporate at least a portion of the liquid from the thin film of the liquid raw material to increase the concentration of solid particles in the thin film, and ii) apply pressure to the thin film by passing it through at least one nip formed by pressing opposing nip-forming surfaces together, thereby gradually forming layers of flakes consisting of aggregated and compressed solid particles. A method for producing flakes, including [the specified ingredient].

2. A manufacturing method according to claim 1, wherein the average maximum thickness t of the flakes is 200 μm or less.

3. A manufacturing method according to claim 1 or 2, wherein the average aspect ratio ASP between the longest planar dimension L of the flake and the maximum thickness t of the flake is at least 10:

1.

4. A manufacturing method according to any one of claims 1 to 3, wherein the liquid raw material is applied by an applicator, the first movable surface and the applicator are in relative motion during the application process, and at least one of the formation of the thin film of the liquid raw material, the concentration of the solid particles in the thin film, and the acquisition of the flakes is caused by the passage of the nip.

5. A manufacturing method according to any one of claims 1 to 4, further comprising the step of forming the thin film of the liquid raw material before passing through the at least one nip.

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

7. A manufacturing method according to any one of claims 1 to 6, wherein the liquid raw material is applied to the first movable surface at a temperature higher than the ambient temperature and at least 5°C lower than the boiling point of the liquid.

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

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

10. A manufacturing method according to any one of claims 1 to 9, further comprising the step of recovering flakes downstream of at least one nip-forming surface.

11. A manufacturing method according to any one of claims 1 to 10, wherein the liquid raw material is continuously applied and the resulting flakes are continuously collected.

12. A manufacturing method according to any one of claims 1 to 11, wherein the opposing nip-forming surfaces of the nip each have a dynamically variable spacing, the spacing decreases to 1 μm or less when none of the liquid raw material, the thin film, the flake layer, or the flakes obtained therefrom are present, and optionally the spacing is 400 μm or less when the liquid raw material is present.

13. A manufacturing method according to any one of claims 1 to 12, wherein the material is crystalline.

14. A manufacturing method according to any one of claims 1 to 13, wherein at least one of the at least one solid material is a flavor substance.

15. Apparatus for producing flakes from a liquid raw material comprising at least one material dissolved or dispersed in a liquid, Support frame and Two cylinders, each attached to the support frame and at least one of which is movable relative to the support frame, A force mechanism that applies force to bring the two cylinders into contact with each other to form a nip, A drive motor for rotating at least one of the two cylinders, A supply device for applying the liquid raw material onto at least one cylinder to form a film on the surfaces of both cylinders, A torque measuring device for measuring the torque applied by the aforementioned drive motor, A controller that adjusts the dispensing speed of the liquid raw material by the supply device based on the measured torque, Equipped with, During use, the film repeatedly passes through the nip, increasing the concentration of solid particles in the material. The torque changes according to the proportion of liquid in the membrane.

16. The apparatus according to claim 15, wherein the supply device is configured to dispense the liquid raw material in individual amounts, and the controller adjusts the amount of individual dispensing and / or the repetition rate.

17. The apparatus according to claim 15, wherein the supply device is configured to dispense a continuous flow of the liquid raw material, and the controller adjusts the flow rate of the continuous flow.

18. The apparatus according to any one of claims 15 to 17, wherein at least one cylinder is heated during use, at least one device heats the cylinder, and the device is located inside and / or outside the heated cylinder.

19. A device according to any one of claims 15 to 18, wherein the force mechanism includes a pneumatic piston or a hydraulic piston including an accumulator.

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

21. The apparatus according to claim 20, further comprising a peeling device for separating the flakes from the surface of the cylinder, wherein the separation relies on a low proportion of liquid in the film.

22. The apparatus according to claim 21, wherein the peeling device is in reciprocally contacting at least one surface of the cylinder and is arranged such that the separated flakes are collected by the recovery device, and the peeling device is selected from the group consisting of a doctor blade and a scraper.

23. The apparatus according to any one of claims 15 to 22, further comprising a leveling device configured to bring the liquid raw material applied by the supply device to a uniform height before it passes through the nip.

24. The apparatus according to any one of claims 15 to 23, a) A pre-treatment station located upstream of the supply device and in fluid communication with the supply device, configured to (i) heat the liquid raw material, (ii) reduce the size of the material dispersed in the liquid raw material, and / or (iii) increase the concentration of the material dissolved or dispersed in the liquid raw material, and b) A flake formation post-processing station configured to (i) dry the recovered flakes and / or (ii) sort the recovered flakes and / or (iii) recycle flakes that do not fit the desired dimensions into a feeder. A device further comprising at least one of the following.

25. The apparatus according to any one of claims 15 to 24, wherein the rotation axis of the cylinder is not horizontal, and the supply device is arranged such that it applies the liquid raw material to the upper end of the cylinder 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 pressed against one of the two cylinders to form at least one additional nip, A device in which three or more cylinders are arranged linearly or radially relative to each other.

27. The apparatus according to any one of claims 15 to 26, wherein, during use, the opposing nip-forming surfaces of the nip have a dynamically variable spacing between them, the spacing decreases to 1 μm or less when none of the liquid raw material, the film, or the flakes obtained therefrom are present, and optionally, the spacing is 400 μm or less when the liquid raw material is present.

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