A nicotine pouch and a method of making the same

Abstract

The application discloses a nicotine bag and a preparation method thereof, and belongs to the technical field of novel tobacco products. The nicotine bag comprises a bag body formed by a packaging material and contents encapsulated in the bag body, wherein the contents comprise a nicotine source, a filler, a pH regulator, and optionally, a flavoring agent, a humectant and a sweetener. The water contact angle of the inner side surface of the packaging material is 40-90 degrees, and the water contact angle of the outer side surface is 70-130 degrees, thereby forming a gradually increasing hydrophilic-hydrophobic gradient from the inside to the outside. The packaging material is provided with micropores penetrating through the thickness of the packaging material, and the porosity is 10-60%. The application can precisely control the release behavior without changing the content formula by constructing the porosity and the hydrophilic-hydrophobic gradient, and the process is simple and suitable for large-scale production.

Description

Technical Field

[0001] This invention belongs to the field of novel tobacco product technology, specifically relating to a nicotine pouch and its preparation method. Background Technology

[0002] Influenced by the international tobacco control movement, cigarette consumption has shown a downward trend year by year, making the regulation of tobacco products and the demand for alternative products more urgent than ever before. Smokeless tobacco products, due to their obvious advantages such as not burning and producing no smoke, are gaining momentum against this trend and are gradually becoming an important supplement to tobacco consumption in a tobacco control environment, attracting widespread attention from major tobacco companies worldwide. Among many potential smokeless tobacco alternatives, nicotine pouches, as a new type of nicotine product, are gradually entering consumers' field of vision and are developing rapidly due to their significant characteristics such as convenience and low harm.

[0003] Nicotine pouches have a broad market base globally, particularly in Northern Europe and the United States, and their market share is gradually expanding with the rise of new tobacco products. Globally, in 2023, nicotine pouches, as a rapidly growing tobacco product in recent years, continued their high-speed growth, with sales volume increasing by 43.5% year-on-year to 15.51 billion pouches and sales revenue increasing by 61.1% year-on-year to US$7.86 billion. The United States accounted for 75.8% of global nicotine pouch sales. With the continuous development of market trade and the expansion of the new tobacco product market, the production and sales of nicotine pouches are gradually showing a global trend. More and more international tobacco companies are beginning to establish a global presence in the nicotine pouch market, driving the globalization of nicotine pouch production.

[0004] The release rate of nicotine and flavor components is a crucial factor affecting the user experience of nicotine pouches. A release rate that is too fast, while providing a strong nicotine satisfaction in a short time, can lead to the active ingredients being released too quickly, resulting in insufficient subsequent release and a poor sustained experience. Conversely, a release rate that is too slow can prevent consumers from experiencing nicotine satisfaction immediately upon initial use, negatively impacting the product experience. Therefore, achieving precise control over the release rate of nicotine pouches to balance initial release speed and sustained release effect is a key technological direction in current nicotine pouch product development.

[0005] In existing technologies, the regulation of nicotine bag release behavior mainly focuses on optimizing the content formulation. For example, the release behavior of nicotine and flavor components can be altered by adjusting nicotine particle size, changing filler composition, adding sustained-release excipients, or constructing multi-layered particle structures. While these technologies can regulate the release rate to some extent, they typically require redesigning the content formulation for different release requirements, resulting in complex processes, high production costs, and limited product development flexibility.

[0006] In addition, some existing technologies attempt to regulate nicotine release through packaging materials. For example, some technologies apply functional chemical coatings to the surface of non-woven packaging materials to improve their permeability and thus influence nicotine release; others use chewable packaging materials, altering their permeability through user chewing to promote nicotine release. However, these methods typically rely on additional chemical treatment layers or the user's mechanical action, resulting in relatively simple release regulation methods that struggle to address both rapid and sustained release needs. Furthermore, they suffer from complex processes and limited applicability.

[0007] In addition, existing technologies have proposed an asymmetrical design approach with different saliva permeability on both sides of the bag. However, such solutions usually rely on the structural differences of the material itself or adopt complex multi-layer composite processes. Moreover, the means of controlling the permeability difference are relatively simple, making it difficult to achieve precise and continuous adjustment of the release rate.

[0008] Further analysis reveals that packaging materials not only encapsulate the contents, but their own liquid transport and diffusion properties are also crucial factors determining nicotine release behavior. The pore structure of the packaging material determines the channels through which saliva enters the packaging bag and where dissolved nicotine diffuses, while the hydrophilic / hydrophobic properties of the packaging material surface affect the liquid wetting rate and solute diffusion behavior. However, current research on packaging materials mainly focuses on material type or surface treatment processes, and has not yet comprehensively considered the synergistic effect of porosity and hydrophilic / hydrophobic properties from the perspective of the intrinsic structural parameters of the packaging material to systematically design and precisely control the nicotine release rate.

[0009] Therefore, there is an urgent need to provide a new nicotine pouch and its preparation method, which can achieve a wide range and fine control of the release rate of nicotine and flavor components by designing the structural parameters of the packaging material itself, without changing the contents formula or relying on additional mechanical action, thereby meeting the diverse needs of different consumers for fast-release, standard-release and slow-release products. Summary of the Invention

[0010] In a first aspect, the present invention provides a nicotine bag comprising: A bag formed by packaging materials, and the contents sealed inside the bag; The contents include nicotine sources, fillers, pH adjusters, and optional flavorings, humectants, and sweeteners; The water contact angle of the inner surface of the packaging material is 40° to 90°, and the water contact angle of the outer surface is 70° to 130°. The packaging material has micropores that extend through its thickness. The porosity of the packaging material is 10% to 60%. Porosity is defined as the percentage of the total open area of ​​the micropores to the total surface area of ​​the packaging material.

[0011] Furthermore, the packaging material is a composite structure formed by thermoforming and bonding at least two layers of fiber web, including: Inner hydrophilic layer, and Outer hydrophobic layer.

[0012] Furthermore, the fiber material of the inner hydrophilic layer is selected from one or more of viscose fiber, cotton fiber, and Lyocell fiber.

[0013] Furthermore, the outer hydrophobic layer is selected from hydrophobic fiber layers of polypropylene, polyethylene, polyester and polylactic acid, or is a hydrophobic layer formed by applying a hydrophobic coating to the surface of a hydrophilic fiber substrate.

[0014] Furthermore, the outer hydrophobic layer is a hydrophobic layer formed by applying a hydrophobic coating to the surface of a hydrophilic fiber substrate; Furthermore, the material for the hydrophobic coating is selected from at least one of silane coupling agents, food-grade wax emulsions, silicone oil emulsions, polyurethane hydrophobic coatings, and fatty acid modified starch. Furthermore, the amount of hydrophobic coating applied is 0.5% to 15% of the dry weight of the outer fiber.

[0015] Furthermore, the average pore size of the micropores ranges from 5 μm to 200 μm; Furthermore, micropores are formed through mechanical drilling, thermal needle piercing, hydroentangling, laser drilling, or ultrasonic perforation processes.

[0016] Furthermore, the micropores are tapered, with the outer opening diameter being smaller than the inner opening diameter.

[0017] Furthermore, the porosity of the packaging material is 35% to 60%, the average pore size of the micropores is 30 μm to 100 μm, and the nicotine release rate of the nicotine bag is ≥65% within 3 minutes.

[0018] Furthermore, the porosity of the packaging material is 10% to 20%, the average pore size of the micropores is 10 μm to 25 μm, and the nicotine release rate of the nicotine bag within 30 minutes is 70% to 80%.

[0019] In a second aspect, a method for preparing a nicotine bag according to the first aspect is provided, comprising the following steps: Step S1: Prepare packaging material such that the water contact angle of the inner surface of the packaging material is 40° to 90° and the water contact angle of the outer surface is 70° to 130°; Step S2: Perform microporous forming treatment on the packaging material to achieve a micropore porosity of 10% to 60%; Step S3: Mix the nicotine source, filler, pH adjuster, and optional flavoring, humectant, and sweetener evenly to obtain the contents; Step S4: Use the packaging material obtained in step S2 to form a bag, fill the contents into the bag and seal it to obtain a nicotine bag.

[0020] Furthermore, in step S2, the micropore forming process adopts laser drilling technology. By adjusting the laser focus position or utilizing the different thermal response characteristics of the packaging material, a conical hole structure with an outer opening diameter smaller than the inner opening diameter is formed.

[0021] Compared with the prior art, the present invention has the following beneficial effects: This invention breaks through the existing technical approach that mainly relies on the formulation of the contents to regulate release behavior. By designing the porosity and hydrophilicity gradient of the packaging material, the saliva penetration rate and nicotine diffusion rate are synergistically controlled, thereby achieving precise regulation of the release rate of nicotine and flavor components. Different release modes, such as rapid release, standard release, and slow-and-long-lasting release, can be obtained as needed. The inner side of the packaging material has good hydrophilicity, which promotes rapid entry of saliva into the bag, allowing the nicotine source to dissolve quickly; the outer side of the packaging material has strong hydrophobicity, which increases the mass transfer resistance when the nicotine solution diffuses into the oral cavity, reducing the instantaneous release rate of the active ingredient. This creates an "easy-in, difficult-out" release mechanism, ensuring initial satisfaction while extending the release duration and improving the consumer experience. The results of the examples and comparative examples show that only when the porosity and hydrophilicity gradient are designed synergistically can both initial release rate and sustained release performance be balanced.

[0022] This invention primarily achieves release regulation through the structural parameters of packaging materials. Different release curves can be obtained without frequent adjustments to nicotine sources, fillers, and other formulation components, which helps reduce product development costs, improve product development efficiency, and maintain the stability and consistency of the content formulation system. Attached Figure Description

[0023] The above description of this application and the following detailed embodiments will be better understood when read in conjunction with the accompanying drawings. It should be noted that the drawings are merely examples of the claimed technical solutions.

[0024] Figure 1 A schematic flowchart of a method for preparing a nicotine bag according to an embodiment of the present invention is shown. Detailed Implementation

[0025] The detailed features and advantages of this application are described below in the specific embodiments. The content of this description is sufficient to enable any person skilled in the art to understand the technical content of this application and implement it accordingly. Based on the specification, claims and drawings disclosed in this specification, a person skilled in the art can easily understand the related objectives and advantages of this application.

[0026] In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined to have the following meanings: All figures used to represent component amounts, properties (e.g., weight-average molecular weight), reaction conditions, etc., should be considered in all cases modified by the terms "within the unavoidable margin of error" or "about". Therefore, the numerical values ​​set forth herein are approximate and may vary depending on the desired properties sought to be obtained by the present invention. The principle of equivalents, which is applied to a minimum and not intended to limit the scope of the claims, should be applied, for example, each value should be interpreted at least according to the reported significant digits and by applying conventional rounding techniques.

[0027] All other terms used herein for special definition are intended to have the general meaning understood by one of ordinary skill in the art, in particular meaning that one of ordinary skill in the art can directly and without doubt determine how the technical solutions of the invention can be implemented after reading the claims, specification and drawings.

[0028] Even if there are incomplete descriptions, omissions, or ambiguities in the grammar, words, punctuation, graphics, symbols, etc. of the claims, specification, and drawings of this invention, those skilled in the art can still arrive at the only correct understanding by reading the claims, specification, and drawings as a whole without extensive reasoning or experimentation, and effectively exclude various incorrect interpretations that are not aimed at achieving the purpose of this invention.

[0029] The "range" disclosed herein is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of a particular range. Ranges defined in this way can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a specific parameter, it is expected that ranges of 60-110 and 80-120 are also expected. Furthermore, if minimum range values ​​of 1 and 2 are listed, and if maximum range values ​​of 3, 4, and 5 are listed, then the following ranges are all expected: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In this application, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed in this article; "0-5" is simply a shortened representation of these numerical combinations. Furthermore, when a parameter is stated as an integer ≥2, it is equivalent to disclosing that the parameter is, for example, an integer such as 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0030] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions.

[0031] Unless otherwise specified, all the technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0032] Unless otherwise specified, all steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially. For example, the method includes steps (a) and (b), indicating that the method may include steps (a) and (b) performed sequentially, or it may include steps (b) and (a) performed sequentially. For example, the mention that the method may also include step (c) indicates that step (c) may be added to the method in any order; for example, the method may include steps (a), (b), and (c), or it may include steps (a), (c), and (b), or it may include steps (c), (a), and (b), etc.

[0033] Unless otherwise specified, the terms "comprising" and "including" as used herein can be open-ended or closed-ended. For example, "comprising" and "including" may mean that other components not listed may also be included, or that only the listed components may be included.

[0034] In the description of this article, it should be noted that, unless otherwise stated, "above" and "below" include the number itself, and "several" in "one or more" means two or more.

[0035] In this description, unless otherwise stated, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, the condition "A or B" is satisfied by any of the following conditions: A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0036] Unless otherwise specified, percentages (%) in this document refer to percentages by mass relative to the composition.

[0037] Unless otherwise stated herein, the sum of the contents of the components in the composition is 100%.

[0038] In this document, unless otherwise stated, “combination of” means a multi-component mixture of the elements, such as two, three, four, and up to the maximum possible multi-component mixture.

[0039] Unless otherwise specified, the term "a" as used in this specification means "at least one".

[0040] The terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0041] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0042] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings. Unless otherwise specified, the experimental methods described in the embodiments of the present invention are conventional methods, and the materials and reagents used in the following embodiments are commercially available unless otherwise specified.

[0043] One object of the present invention is to provide a nicotine bag comprising: A bag formed by packaging materials, and the contents sealed inside the bag; The contents include nicotine sources, fillers, pH adjusters, and optional flavorings, humectants, and sweeteners; The water contact angle of the inner surface of the packaging material is 40° to 90°, and the water contact angle of the outer surface is 70° to 130°. The packaging material has micropores that extend through its thickness. The porosity of the packaging material is 10% to 60%. Porosity is defined as the percentage of the total open area of ​​the micropores to the total surface area of ​​the packaging material.

[0044] As used herein, a “nicotine pouch” refers to a product in the form of a mixture of one or more components contained within a liquid-permeable container (e.g., a liquid-permeable pouch). Such mixtures in the form of liquid-permeable delivery pouches are typically used by placing a delivery pouch containing the mixture in the mouth of a human subject / user. Typically, the delivery pouch is placed somewhere in the user’s mouth, such as below the lips, in the same manner as commonly used oral tobacco products. The pouch is preferably not chewed or swallowed. Exposure to saliva then allows some components of the mixture (e.g., flavorings and / or nicotine) to pass through the, for example, water-permeable pouch, providing the user with flavor and satisfaction, and the user does not need to spit out any part of the mixture. After approximately 10 to 60 minutes of use / enjoyment, typically approximately 15 to 45 minutes, a significant portion of the mixture has been ingested by the human subject, and the delivery pouch can be removed from the consumer’s mouth for disposal. Nicotine pouches typically do not contain tobacco but directly contain the nicotine source.

[0045] As used in this article, the water contact angle refers to the angle between the tangent of the gas-liquid interface and the solid-liquid interface at the solid-liquid-gas three-phase interface when a drop of deionized water is placed on the surface of a solid material (usually the angle inside the droplet, denoted as θ).

[0046] The water contact angle can be measured using a contact angle meter, and the standard measurement method (seat drop method) is as follows: The material to be tested is fixed flat on a stage. A drop of approximately 2-5 μL of deionized water is added to the surface of the material using a precision injection needle. A high-magnification camera is used to capture a side view image of the droplet on the solid surface in real time. The instrument's built-in software fits the droplet profile and automatically calculates the angle between the tangent and the bottom surface, which is the water contact angle.

[0047] In the packaging material of this invention, a hydrophilic-hydrophobic gradient is constructed using the water contact angle. The inner side of the material is hydrophilic, even approaching moderate wettability. When a user places it in their mouth, the hydrophilic surface exerts a capillary attraction on water (saliva), rapidly drawing the saliva into the bag, wetting and dissolving the nicotine salts on the microcrystalline cellulose. The outer side of the material is hydrophobic. At this point, the outer side repels saliva and aqueous solutions. When a nicotine-containing liquid solution inside the bag attempts to "leak out," the hydrophobic barrier on the outer side significantly increases the resistance to liquid penetration.

[0048] In some embodiments, the packaging material is a composite structure formed by thermoforming and bonding at least two layers of fiber webs, including: an inner hydrophilic layer and an outer hydrophobic layer.

[0049] In some embodiments, the fiber raw material for the inner hydrophilic layer is selected from one or more of viscose fiber, cotton fiber, and Lyocell fiber, preferably Lyocell fiber. Lyocell fiber is produced by wet spinning using N-methylmorpholine-N-oxide (NMMO) as a solvent. When viscose fiber is used, it is of food-grade specifications. The inner hydrophilic layer is formed by wet or dry web forming processes, with a fiber length preferably from 5 mm to 25 mm, and is dried after chemical bonding (using food-grade acrylate emulsion or polyvinyl alcohol binder).

[0050] The outer hydrophobic layer can be formed in two ways: Method 1 involves using hydrophobic synthetic fibers, such as polypropylene (PP) fibers or polylactic acid (PLA) fibers, to prepare a fiber web via spunbonding or meltblowing; Method 2 involves using a hydrophilic fiber substrate, such as viscose fiber or Lyocell fiber, and applying a hydrophobic coating to its surface. The hydrophobic coating material is selected from at least one of the following: silane coupling agents (such as octyltriethoxysilane), food-grade wax emulsions (such as palm wax emulsions, beeswax emulsions), silicone oil emulsions, polyurethane hydrophobic coatings, or fatty acid-modified starch. The hydrophobic coating is applied by one of the following methods: dip coating, spray coating, blade coating, roller coating, or transfer coating. The coating amount (by dry weight) is 0.5% to 15% of the outer fiber mass, preferably 1% to 10%, corresponding to a coating surface density of approximately 0.5 g / m² to 10 g / m² (dry weight).

[0051] In this invention, the micropores penetrate the thickness direction of the inner packaging material, and their formation process is selected from one of mechanical perforation, thermal needle perforation, hydroentangling perforation, laser perforation, or ultrasonic perforation. In some embodiments, the average pore diameter of the micropores is 5 μm to 200 μm, preferably 10 μm to 100 μm, and more preferably 15 μm to 60 μm. The micropores are distributed uniformly or in a gradient on the material surface. The pore shape is selected from one of circular, elliptical, rectangular, slit-shaped, or irregular shapes. Preferably, the micropores have a conical pore structure, that is, the opening diameter on the outer surface is smaller than the opening diameter on the inner surface (D2 / D1 < 1). Advantageously, the hydrophilicity-hydrophobicity difference on both sides of the packaging material works synergistically with the conical pore (D2 / D1 < 1). When the outer contact angle is greater than the inner contact angle, the droplet is hindered by the Laplace pressure difference in the conical pore, forming a "one-way valve" effect. The larger the outer hydrophobic angle, the stronger this blocking effect on reverse diffusion.

[0052] The packaging material according to the present invention can be a woven material, a non-woven material, and / or a composite material including both woven and non-woven materials, or cotton paper. The bag according to the present invention is a saliva-permeable bag. Preferably, the bag is a non-woven bag. The bag can be prepared using methods known in the art, and its sealing can be achieved by heat sealing, cold sealing, or ultrasonic sealing, etc.

[0053] As used in this article, "nicotine," also known as nicotine alkaloid, is an organic compound with the chemical formula C. 10 H 14 N2, with the structural formula shown in Formula I. Nicotine belongs to the alkaloid class of compounds. Alkaloids are a class of nitrogen-containing basic organic molecules that exhibit base-like chemical properties, forming salt solutes in water or reacting with acids. The nicotine structure contains a pyridine ring and a pyrrolidine ring, and its nitrogen atom readily accepts protons (H). + Nicotine is alkaline and can neutralize acids to form salt compounds. Free nicotine has a high pH (approximately 8.0-10.0) and causes strong irritation to the mucous membranes of the mouth and throat. Nicotine salts significantly reduce irritation and provide a gentler user experience by lowering the pH (approximately 5.0-7.0).

[0054] (I)

[0055] In this invention, the nicotine source may include one or more of nicotine and nicotine derivatives.

[0056] Nicotine derivatives include one or more of nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bonded nicotine.

[0057] Nicotine salts can be selected from nicotine hydrochloride, nicotine phosphate, nicotine sulfate, nicotine pyruvate, nicotine formate, nicotine oxalate, nicotine ascorbate, nicotine glycolate, nicotine acetate, nicotine isovalerate, nicotine valerate, nicotine propionate, nicotine caprylate, nicotine lactate, nicotine levulinate, nicotine sorbate, nicotine malate, nicotine fumarate, nicotine salicylate, nicotine glycinate, nicotine tartrate, nicotine succinate, nicotine citrate, nicotine benzoate, and nicotine oil. Nicotine aconitate, nicotine butyrate, nicotine cinnamate, nicotine caprate, nicotine 3,7-dimethyl-6-octenate, nicotine 1-glutamate, nicotine heptaate, nicotine hexanoate, nicotine 3-hexenoate, nicotine trans-2-hexenoate, nicotine isobutyrate, nicotine laurate, nicotine 2-methylbutyrate, nicotine 2-methylvalerate, nicotine myristate, nicotine nonanoate, nicotine palmitate, nicotine 4-pentenoate, nicotine phenylacetate, and nicotine 3-phenylpropionate are among one or more of these.

[0058] Additional ingredients that may include the compositions disclosed herein or representative types that may be used to manufacture the bagged products disclosed herein include fillers, thickeners, film-forming agents, binders, buffers and pH control agents, anti-adhesion agents, flow aids, sweeteners, humectants, preservatives and antioxidants, surfactants, colorants, lubricants and processing aids.

[0059] In one embodiment of the present invention, the pH adjuster is selected from acetic acid, adipic acid, citric acid, fumaric acid, gluconic acid-δ-lactone, gluconic acid, lactic acid, malic acid, maleic acid, tartaric acid, succinic acid, propionic acid, ascorbic acid, phosphoric acid, sodium orthophosphate, potassium orthophosphate, calcium orthophosphate, sodium diphosphate, potassium diphosphate, calcium diphosphate, pentasodium triphosphate, pentapotassium triphosphate, sodium polyphosphate, potassium polyphosphate, carbonic acid, sodium carbonate, sodium bicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, magnesium oxide, glycerol, phosphate buffer, amino acids, or any combination thereof.

[0060] In some embodiments, the sweeteners include aspartame, acesulfame potassium, cyclamate, saccharin, sodium saccharin, sucralose, neotame, sodium cyclohexylsulfamate, stevia, licorice, disodium glycyrrhizate, tripotassium and trisodium glycyrrhizate, glucose, fructose, sucrose, maltose, corn syrup, starch sugar and lactose, sorbitol, maltitol, isomaltitol, palaginitol, xylitol, lactitol, mannitol, erythritol and dextran.

[0061] In some embodiments, the filler includes one or more of cellulose and cellulose derivatives, starch, maltodextrin, and cyclodextrin. In some embodiments, the filler includes microcrystalline cellulose.

[0062] In some embodiments, the humectant includes one or more of glycerol and ethylene glycol.

[0063] In some embodiments, the cooling agent includes one or more of menthol, WS-23, WS-3, menthone glycerol acetal, and menthyl lactate.

[0064] In some embodiments, the preservative includes one or more of benzoic acid, sodium benzoate, sorbic acid, and potassium sorbate.

[0065] In some embodiments, the spices are selected from peppermint, cinnamon, cherry, coconut, coffee, chocolate, vanilla, citrus (such as grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruit, cherry, cinnamon, peppermint, deer hoof grass, spearmint, eucalyptus, apple, pear, peach, strawberry, apricot, raspberry, cherry, pineapple, lemongrass, lime, chili, capsaicin, citrus, tobacco flavor, bergamot, smoky flavoring, plum, eucalyptus, clove, bay leaf, fennel, thyme, cedar leaf, and nutmeg.

[0066] refer to Figure 1 One object of the present invention is to provide a method for preparing a nicotine bag, comprising the following steps: Step S1: Prepare packaging material such that the water contact angle of the inner surface of the packaging material is 40° to 90° and the water contact angle of the outer surface is 70° to 130°; Step S2: Perform microporous forming treatment on the packaging material to achieve a micropore porosity of 10% to 60%; Step S3: Mix the nicotine source, filler, pH adjuster, and optional flavoring, humectant, and sweetener evenly to obtain the contents; Step S4: Use the packaging material obtained in step S2 to form a bag, fill the contents into the bag and seal it to obtain a nicotine bag.

[0067] In some embodiments, the micropore forming process in step S2 uses laser drilling technology, which forms a tapered hole structure with an outer opening diameter smaller than the inner opening diameter by adjusting the laser focus position or utilizing the different thermal response characteristics of the packaging material.

[0068] In one specific embodiment, the method for preparing the nicotine bag of the present invention includes the following steps: Step S1: Prepare inner packaging materials A double-layer nonwoven nonwoven substrate containing an inner hydrophilic layer and an outer hydrophobic layer is prepared using wet web forming or dry web forming processes.

[0069] Inner hydrophilic layer: The wet web forming process is used, with Lyocell fiber or food-grade viscose fiber as raw material, with fiber length from 5mm to 25mm. After chemical bonding (food-grade acrylic emulsion or PVA adhesive), it is dried.

[0070] Outer hydrophobic layer: PP fiber web is prepared by spunbonding or meltblowing; or a hydrophilic fiber web is prepared first, and then a hydrophobic coating is applied by impregnation coating, spraying, scraping coating, roller coating or transfer coating, with a coating amount of 0.5 g / m² to 10 g / m² (dry weight).

[0071] Two layers of fiber webs are stacked and bonded together by hot rolling to form an integrated composite nonwoven fabric.

[0072] Step S2: Micropore forming

[0073] The nonwoven fabric substrate obtained in step S1 is subjected to microporous forming. Taking laser drilling as an example, a CO2 laser with a wavelength of 10.6 μm, a power of 20 W, and a pulse width of 0.5 ms is used. The target pore size and porosity are achieved by controlling the pore spacing and pulse parameters. Conical pore structures can be formed simultaneously by adjusting the laser focus position or utilizing the different thermal response characteristics of the bilayer materials. The different thermal response characteristics of the bilayer materials refer to the difference in melting point / thermal decomposition temperature between the inner hydrophilic layer and the outer hydrophobic layer. Under the same laser parameters, the ablation rates of the two layers are different, thus making the formation of conical pores more controllable.

[0074] Step S3: Prepare contents

[0075] Nicotine source (such as pharmaceutical grade nicotine tartrate dihydrate or nicotine benzoate), flavoring components, fillers (food grade microcrystalline cellulose), pH adjusters (such as sodium carbonate, sodium bicarbonate), humectants (such as propylene glycol, glycerin), sweeteners, etc. are mixed evenly according to a predetermined ratio to obtain the contents particles with an average particle size of 200μm to 400μm.

[0076] Step S4: Filling and Shaping

[0077] The inner packaging material obtained in step S2 is cut into sheets of a predetermined size (e.g., 40mm × 20mm). Two sheets are stacked together and heat-sealed along three sides to form a bag with one open end. The contents granules from step S3 are filled into the bag according to a predetermined dosage (e.g., 500mg), and the open end is heat-sealed. A secondary hydrophobic treatment can be selectively applied to the outer surface.

[0078] In the preparation method, the order of steps S2 and S3 can be interchanged.

[0079] Example

[0080] Experimental materials and instruments

[0081] Table 1. Names of Raw Materials and Suppliers

[0082] Table 2. Instruments used in the experiment and their suppliers

[0083] Test methods

[0084] (1) Water contact angle

[0085] An optical contact angle meter was used with the seated drop method. The specific steps are as follows: A sample of the inner packaging material to be tested was taken and cut into a 20mm × 20mm square piece. The piece was then flatly attached to the sample stage of the contact angle meter, ensuring the surface was free of wrinkles and contamination. A 2μL drop of deionized water was added to the surface of the piece using a microsyringe. After the droplet stabilized for 10 seconds, a side view image of the droplet was captured using a high-precision camera. The instrument's software was used to fit the droplet profile based on the Young-Laplace equation and automatically calculate the water contact angle. Five different locations were measured for each sample, and the arithmetic mean was taken as the final water contact angle for that sample.

[0086] (2) In vitro release test

[0087] A flow cell dissolution device coupled with an ultra-high performance liquid chromatography-photodiode array detector (UPLC-PDA) system was used.

[0088] Test conditions: Dissolution temperature: 37℃ Flow rate: 8 mL / min System mode: Closed-loop mode Flow cell type: Powder-specific flow cell Sampling time points: 3 minutes, 10 minutes, 30 minutes Sample volume per time: 1 mL (3) Porosity The determination was performed using image analysis, and the specific steps are as follows: A sample of the inner packaging material to be tested was taken, cut into 10mm × 10mm pieces, and after gold sputtering, a microscopic photograph of the material surface was taken using a scanning electron microscope (SEM) at an appropriate magnification. At least 10 different fields of view were randomly selected for each sample. The obtained SEM images were imported into image analysis software, and micropore regions were identified and extracted using a grayscale thresholding method. The percentage of the sum of the open areas of micropores in each field of view relative to the total area of ​​that field of view was calculated, and the arithmetic mean of all fields of view was taken as the porosity of the sample.

[0089] (4) Average aperture

[0090] This invention uses a capillary flow aperture gauge to determine the average pore size of micropores. The specific steps are as follows: Take a sample of the inner packaging material to be tested, cut it into a circular test piece of appropriate size, and completely immerse it in a low surface tension liquid, ensuring that all micropores are fully filled. Place the immersed test piece into the sample cell of a capillary flow pore size analyzer and seal it. Using clean compressed air or nitrogen as the driving gas, gradually increase the gas pressure from one side of the sample. Once the gas pressure overcomes the capillary pressure of the liquid in the micropores, the liquid is gradually discharged from the pores, forming a detectable gas flow rate. The instrument automatically records the gas flow rate changes under different pressures, calculates the pore size distribution according to the Washburn equation, and automatically fits the average flow pore size using software; this is the average pore size described in this invention. Three test pieces are measured for each sample, and the average value is taken as the final result.

[0091] When the micropore has a conical structure and the outer opening diameter is smaller than the inner opening diameter, the measured average pore diameter reflects the equivalent pore diameter at the narrowest point of the channel, i.e., the outer opening.

[0092] Example 1

[0093] This embodiment provides a fast-release nicotine bag, the preparation method of which is as follows: (1) Lyocell fiber was used as raw material with a fiber length of 10 mm. The fiber web was formed by wet web forming process and chemical bonding was carried out using food-grade acrylic emulsion as binder. After drying, the inner hydrophilic layer fiber web was obtained with a basis weight of 18 g / m² and a water contact angle of 55°.

[0094] Polypropylene (PP) spunbond fiber web with a basis weight of 12 g / m² was used. An octyltriethoxysilane hydrophobic coating was applied to its surface by spraying at a rate of 2 g / m² (dry weight). After drying, the water contact angle was measured to be 105°.

[0095] The inner hydrophilic fiber web and the outer hydrophobic fiber web are stacked together and hot-rolled and bonded at 150°C and 5MPa to obtain an integrated composite nonwoven fabric with a total basis weight of 30g / m² and a thickness of 0.15mm.

[0096] (2) CO2 laser drilling technology (wavelength 10.6μm, power 20W, pulse width 0.5ms) was used to drill holes in the composite nonwoven fabric. The hole spacing was 0.3mm, the average hole diameter was 50μm, and the porosity was 42%. By adjusting the laser focus position, the ratio of the outer opening diameter to the inner opening diameter D2 / D1≈0.8 was made to form a conical hole structure.

[0097] (3) Weigh out 55 parts of microcrystalline cellulose, 5 parts of nicotine tartrate dihydrate, 2 parts of peppermint flavoring, 3 parts of sodium carbonate, 10 parts of propylene glycol, 10 parts of water, and 0.5 parts of sucralose sweetener by mass, mix them evenly, and sieve to obtain contents particles with an average particle size of about 300 μm.

[0098] (4) Cut the microporous inner packaging material into 40mm×20mm sheets, stack the two sheets together and heat seal along three sides to form a bag with one open end. Fill the bag with 500mg of the contents particles and heat seal the open end to obtain a fast-release nicotine bag.

[0099] Example 2

[0100] This embodiment provides a standard release nicotine bag, the preparation method of which is as follows: (1) Lyocell fiber and food-grade viscose fiber were mixed at a mass ratio of 7:3 as raw materials. The fiber length was 12 mm. The fiber web was formed by wet web forming process. Food-grade acrylic emulsion was used as a binder for chemical bonding. After drying, the inner hydrophilic layer fiber web was obtained with a basis weight of 16 g / m². Its water contact angle was measured to be 50°.

[0101] A fiber web was prepared using Lyocell fiber as raw material, with a basis weight of 10 g / m². A hydrophobic coating of palm wax emulsion was applied by impregnation coating, with a coating amount of 5 g / m² (dry weight). After drying, the water contact angle was measured to be 112°.

[0102] The inner hydrophilic fiber web and the outer hydrophobic fiber web are stacked together and hot-rolled and bonded at 145℃ and 5MPa to obtain an integrated composite nonwoven fabric with a total basis weight of 26g / m² and a thickness of 0.12mm.

[0103] (2) Mechanical punching process was adopted, using a needle roller with a needle diameter of 35μm for piercing, with a punching density of about 300 holes / cm². The average hole diameter was measured to be 35μm and the porosity was 25%.

[0104] (3) Weigh out 50 parts of microcrystalline cellulose, 4.5 parts of nicotine benzoate, 1.5 parts of fruit flavoring, 2.5 parts of sodium bicarbonate, 8 parts of glycerin, 8 parts of water and 0.3 parts of acesulfame potassium sweetener by mass, mix them evenly, and sieve to obtain contents particles with an average particle size of about 300 μm.

[0105] (4) Using the same filling method as in Example 1, with a filling amount of 500mg, a standard release nicotine bag was prepared.

[0106] Example 3

[0107] (1) Cotton fiber and Lyocell fiber were mixed at a mass ratio of 5:5 as raw materials. The fiber length was 15 mm. The fiber web was formed by wet web forming process. Polyvinyl alcohol (PVA) was used as a binder for chemical bonding. After drying, the inner hydrophilic layer fiber web was obtained with a basis weight of 18 g / m². Its water contact angle was measured to be 42°.

[0108] A fiber web was prepared using Lyocell fiber as raw material, with a basis weight of 12 g / m². A water-based polyurethane hydrophobic coating was applied by spraying, with a coating amount of 8 g / m² (dry weight). After drying, the water contact angle was measured to be 125°.

[0109] The inner hydrophilic fiber web and the outer hydrophobic fiber web are stacked together and hot-rolled and bonded at 155℃ and 6MPa to obtain an integrated composite nonwoven fabric with a total basis weight of 30g / m² and a thickness of 0.18mm.

[0110] (2) The hot needle piercing process was adopted, and a heated fine needle with a needle diameter of 18μm was used for piercing. The piercing density was about 150 holes / cm². The average pore diameter was measured to be 18μm and the porosity was 14%. By controlling the temperature of the hot needle piercing, the outer pore opening was contracted to form a conical pore structure, D2 / D1≈0.6.

[0111] (3) Weigh out 55 parts of microcrystalline cellulose, 3.5 parts of nicotine free base, 1.0 part of peppermint flavor, 3.0 parts of potassium carbonate, 12 parts of propylene glycol, 12 parts of water, and 0.4 parts of sucralose sweetener by mass, mix them evenly, and sieve to obtain contents particles with an average particle size of about 300 μm.

[0112] (4) Using the same filling method as in Example 1, a slow-release nicotine bag with a filling amount of 500mg was prepared.

[0113] Example 4

[0114] This embodiment provides a nicotine bag with a gradient micropore distribution, and its preparation method is as follows: (1) Using the same layer structure and materials as in Example 2, the two layers were hot-rolled and composited at 145°C and 5MPa, with a total basis weight of 26g / m² and a thickness of 0.12mm.

[0115] (2) A programmed CO2 laser perforation process is adopted. The laser parameters are controlled by a computer program along the longitudinal direction of the bag body, so that the micropore diameter gradually decreases from 40μm to 20μm from one end to the other end, and the porosity gradually decreases from 30% to 18%, forming a gradient distribution of gradually decreasing pore diameter along the direction of the bag body.

[0116] (3) The same contents formulation and preparation method as in Example 2 were used.

[0117] (4) When cutting the inner packaging material, the end with the larger aperture should correspond to the entrance direction of the bag (close to the front of the mouth), and the end with the smaller aperture should correspond to the rear of the bag. The remaining filling steps are the same as in Example 2.

[0118] Comparative Example 1

[0119] This comparative example uses the same materials and preparation method as Example 2, the difference being that no palm wax emulsion hydrophobic coating is applied to the outer hydrophobic layer, meaning the outer surface remains hydrophilic. The water contact angles on both the inner and outer surfaces were measured to be approximately 50°. The porosity of the composite nonwoven fabric is 25%, with an average pore size of 35 μm, consistent with Example 2.

[0120] Comparative Example 2

[0121] This comparative example uses the same layer structure and hydrophobic coating as Example 2. The difference is that a lower micropore density is used in the micropore forming step, so that the porosity is reduced to 8%. The other parameters are the same as those in Example 2.

[0122] Comparative Example 3

[0123] This comparative example uses the same materials and preparation method as Example 2, the difference being that a hydrophobic coating is applied to both the outer and inner surfaces, increasing the water contact angle on the inner surface from 50° to 110°, while maintaining the outer contact angle at 112°. This means both the inner and outer surfaces are hydrophobic, thus eliminating the hydrophilic-hydrophobic gradient. The porosity is 25%, and the average pore size is 35 μm.

[0124] Comparative Example 4

[0125] This comparative example aims to verify the control effect of adjusting porosity alone without a hydrophilicity-hydrophobicity gradient. The same materials and preparation methods as in Examples 1 and 3 were used, except that no hydrophilicity-hydrophobicity difference was set on the inner and outer sides, the water contact angle was approximately 50°, and only the porosity was changed.

[0126] Two samples were prepared: Comparative Example 4a had a porosity of 14%, and Comparative Example 4b had a porosity of 35%.

[0127] Comparative Example 5

[0128] This comparative example aims to verify that a favorable release mechanism can only be achieved when the wetting gradient direction is "inner hydrophilic, outer hydrophobic". The same materials and preparation methods as in Example 2 were used, except that a hydrophobic coating (water contact angle 110°) was applied to the inner surface, while the outer surface remained hydrophilic (water contact angle 50°), thus forming a reverse wetting gradient of inner hydrophobic and outer hydrophobic. The porosity was 25%, and the average pore size was 35 μm, consistent with Example 2.

[0129] The table below summarizes the key parameters and in vitro release test results for all embodiments and comparative test cases.

[0130]

[0131] Note: ">95" indicates that the release was basically complete and monitoring was not continued until 30 min; "—" indicates that no valid data was obtained at this time point (or there was no need for measurement); the pore sizes of Comparative Examples 2 and 4 were not specifically calibrated because they were not optimized parameters.

[0132] The table clearly shows that only by synergistically designing appropriate porosity with an inside-out hydrophilic / hydrophobic gradient can a balance be achieved between initial release satisfaction and overall durability. Examples 2 and 3 represent successful examples of standard release and slow, sustained release, respectively, while Comparative Examples 1-4 all exhibited problems with release that was either too fast or too slow.

[0133] In the foregoing description of exemplary embodiments / specific implementations of the present invention, various features of the invention are sometimes combined in a single embodiment / specific implementation or its figures and description, with the aim of simplifying the disclosure and aiding in the understanding of one or more of the various aspects of the invention. However, the method of description of the invention should not be construed as reflecting an intention that the claimed features are more than expressly stated in each claim, except where explicitly stated otherwise or in obvious technical contradiction or exclusion. Rather, the inventive aspect reflected in the claims lies in not all the features of a single foregoing disclosed embodiment / specific implementation. Therefore, the claims following the detailed description are expressly incorporated herein by reference, each claim existing independently as a separate embodiment / specific implementation of the invention.

[0134] The terminology and expressions used in this specification are for illustrative purposes and not for limitation. Their use is not intended to exclude any equivalents of the shown and described features or portions thereof, but rather to facilitate the understanding that various modifications may be possible within the scope of the invention. Therefore, it should be understood that while the invention has been specifically disclosed through preferred embodiments, exemplary embodiments, and optional features, those skilled in the art may adopt variations or modifications of the concepts disclosed herein, and such variations and modifications are therefore considered to be within the scope of the invention as defined by the appended claims. The specific embodiments given in this specification are examples of useful embodiments of the invention, and it will be apparent to those skilled in the art that the invention can be practiced using many variations of the devices, device components, and method steps disclosed herein.

[0135] The foregoing description of specific embodiments has fully disclosed the general features of the invention, enabling others to easily modify and / or adapt such embodiments for various applications by applying knowledge within the scope of the art, without excessive experimentation and without departing from the general conception of the invention. Therefore, based on the teachings and guidance provided herein, it is intended that such modifications and alterations be included within the meaning and scope of equivalents of the disclosed embodiments. It should be understood that the wording or terminology used herein is for descriptive purposes and is not intended to be limiting; thus, the wording or terminology in this specification will be interpreted by those skilled in the art based on the foregoing teachings and guidance.

[0136] Furthermore, the scope of the invention should not be limited to any of the exemplary embodiments described above, but only to the appended claims and their equivalents.

Claims

1. A nicotine bag, characterized in that, include: A bag formed by packaging materials, and the contents sealed within the bag; The contents include nicotine sources, fillers, pH adjusters, and optional flavorings, humectants, and sweeteners; The water contact angle of the inner surface of the packaging material is 40° to 90°, and the water contact angle of the outer surface is 70° to 130°. The packaging material has micropores distributed throughout its thickness, and the porosity of the packaging material is 10% to 60%, defined as the percentage of the total open area of ​​the micropores to the total surface area of ​​the packaging material.

2. The nicotine bag according to claim 1, characterized in that, The packaging material is a composite structure formed by hot-pressing and bonding at least two layers of fiber mesh, including: Inner hydrophilic layer, and Outer hydrophobic layer.

3. The nicotine bag according to claim 2, characterized in that, The fiber material of the inner hydrophilic layer is selected from one or more of viscose fiber, cotton fiber, and Lyocell fiber; The outer hydrophobic layer is selected from hydrophobic fiber layers of polypropylene, polyethylene, polyester and polylactic acid, or is a hydrophobic layer formed by applying a hydrophobic coating to the surface of a hydrophilic fiber substrate.

4. The nicotine bag according to claim 3, characterized in that, The outer hydrophobic layer is a hydrophobic layer formed by applying a hydrophobic coating to the surface of a hydrophilic fiber substrate; The hydrophobic coating material is selected from at least one of silane coupling agents, food-grade wax emulsions, silicone oil emulsions, polyurethane hydrophobic coatings, and fatty acid modified starch. The amount of the hydrophobic coating applied is 0.5% to 15% of the dry weight of the outer fiber.

5. The nicotine bag according to claim 1, characterized in that, The average pore size of the micropores is 5 μm to 200 μm; the micropores are formed by mechanical drilling, thermal needle piercing, hydroentangling, laser drilling or ultrasonic piercing processes.

6. The nicotine bag according to claim 1, characterized in that, The micropore is a conical pore, and the outer opening diameter of the conical pore is smaller than the inner opening diameter.

7. The nicotine bag according to claim 1, characterized in that, The porosity of the packaging material is 35% to 60%, the average pore size of the micropores is 30 μm to 100 μm, and the nicotine release rate of the nicotine bag is ≥65% within 3 minutes.

8. The nicotine bag according to claim 1, characterized in that, The porosity of the packaging material is 10% to 20%, the average pore size of the micropores is 10 μm to 25 μm, and the nicotine release rate of the nicotine bag within 30 minutes is 70% to 80%.

9. A method for preparing a nicotine bag as described in any one of claims 1 to 8, characterized in that, Includes the following steps: Step S1: Prepare packaging material such that the water contact angle of the inner surface of the packaging material is 40° to 90° and the water contact angle of the outer surface is 70° to 130°; Step S2: Perform microporous molding treatment on the packaging material to make the porosity of the micropores 10% to 60%; Step S3: Mix the nicotine source, filler, pH adjuster, and optional flavoring, humectant, and sweetener evenly to obtain the contents; Step S4: Use the packaging material obtained in step S2 to form a bag, fill the contents into the bag and seal it to obtain the nicotine bag.

10. The preparation method according to claim 9, characterized in that, The micropore forming process described in step S2 uses laser drilling technology. By adjusting the laser focus position or utilizing the different thermal response characteristics of the packaging material, a tapered hole structure with an outer opening diameter smaller than the inner opening diameter is formed.

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