Nicotine bag and preparation method of nicotine filling particles

Abstract

The invention discloses a preparation method of a nicotine bag and a nicotine filling particle, and the preparation method comprises the following steps: step A, mixing nicotine nicotine salt powder with additive powder to obtain a powder mixture; step B, carrying out pre-wetting treatment on the powder mixture by utilizing pure water to obtain a premix; and step C, placing the premix and the adhesive solution in a fluidized bed granulator to prepare the nicotine filled particles. According to the nicotine filled particles, under the condition that no other pellet core exists, powdery nicotine is used as a material, accurate regulation and control are carried out through key process parameters in the fluidized bed granulation process, the abnormal conditions of adhesion, caking, excessive dust and the like in the granulation process are reduced, and the stability is improved. And the nicotine bag prepared by taking the nicotine filling particles as contents is better in dissolution effect, relatively stable in nicotine release, full and consistent in flavor in the oral cavity, free of'cliff type 'stimulation or attenuation, and strong in consumer experience feeling.

Description

Technical Field

[0001] This patent belongs to the field of novel tobacco technology, specifically relating to a method for preparing a nicotine pouch and nicotine filling particles. Background Technology

[0002] Nicotine pouches, as a novel type of oral tobacco product, have gained widespread attention globally in recent years. This product absorbs nicotine through the oral mucosa, utilizing controlled-release technology to achieve a stable delivery of nicotine while balancing taste comfort and dosage accuracy, providing users with an alternative to traditional tobacco.

[0003] As the core contents of nicotine pouches, the physical properties (such as particle size distribution, porosity, and flowability) and chemical properties of the filler granules directly determine the release rate, palatability, and stability during storage. However, existing technologies mostly focus on the chemical stability and release kinetics of the granules. For example, patent document CN119837290A discloses a method for preparing nicotine products and nicotine composite materials. This method uses microcrystalline cellulose as microsphere powder, and mixes nicotine, sweeteners, and a coating solution to form a mixed solution, which is then sprayed onto the surface of the microsphere powder to form a nicotine composite material. However, this method does not directly use powdered nicotine as a raw material for granulation, relying solely on traditional coating processes. This leads to problems such as uneven particle size, poor flowability, and poor nicotine stability during the granulation process.

[0004] In the field of new tobacco products, existing technologies have not fully recognized the crucial impact of the uniformity of filling particles on taste consistency, irritation, and aftertaste persistence. This results in taste fluctuations between batches or within a single bag, making it difficult to meet the high-end market's demand for quality stability. Furthermore, because nicotine is a low-melting-point, highly volatile organic compound, excessively fine nicotine powder is prone to electrostatic adsorption, while excessively coarse powder easily absorbs moisture and clumps, leading to poor flowability and uneven internal pores in the prepared filling particles. Therefore, existing technologies cannot directly use nicotine powder as a raw material to prepare filling particles.

[0005] Therefore, it is necessary to develop a new method for preparing nicotine filling particles that can use nicotine powder as a raw material to prepare nicotine filling particles. This method can improve the uniformity of the filling particles while ensuring the high stability of nicotine during processing, thereby improving the onset and duration of physiological satisfaction from nicotine packets and enhancing the overall taste experience. Summary of the Invention

[0006] The purpose of this patent is to provide a method for preparing nicotine pouches and nicotine filling granules, so that nicotine powder can be used as raw material to prepare nicotine filling granules without other cores. While ensuring the high stability of nicotine during processing, the uniformity of the filling granules can be improved, thereby improving the onset and duration of physiological satisfaction of the nicotine pouch and improving the overall taste experience.

[0007] Although fluidized bed technology has been used to improve uniformity in the manufacturing process of raw materials such as microcrystalline cellulose, and the uniformity of nicotine powder is generally assumed in the art, the inventors were surprised to find that even so, in the process of remanufacturing nicotine powder from raw materials, the original uniformity was destroyed due to the reorganization of particles. Therefore, the present invention is needed to solve the problem of abrupt changes in taste.

[0008] To solve the above-mentioned technical problems, this patent provides the following technical solution: A method for preparing nicotine-filled granules includes the following steps: Step A: Mix nicotine salt powder with additive powder to obtain a powder mixture; Step B: Pre-wet the powder mixture with pure water to obtain a premix; Step C: Place the premix and binder solution in a fluidized bed granulator to prepare nicotine-filled granules.

[0009] Furthermore, in step B, the pure water accounts for 1-2%, 2-3%, or 3-5% of the mass of the powder mixture.

[0010] Furthermore, in step C, the concentration of the adhesive solution is 4.5~5.5%.

[0011] Furthermore, the specific parameters of the fluidized bed granulator are as follows: inlet air temperature is 80~95℃, air velocity is 0.5~1.5m / s, adhesive solution spraying rate is 10~30 g / min, adhesive atomization pressure is 0.1~0.3 MPa, and the temperature of the sprayed powder bed is maintained at 40~45℃.

[0012] Furthermore, in step A, the mass percentage of nicotine salt powder is 1.0~3.0%.

[0013] Furthermore, the additive powder includes 92.0-94.0% by weight of filler, 3.0-5.0% by weight of sweetener, and 0.4-0.7% by weight of pH buffer.

[0014] Furthermore, the filler includes one or a combination of two of microcrystalline cellulose, powdered cellulose, or starch.

[0015] Furthermore, pH buffers are used to adjust the overall pH value. pH buffers include pH adjusters and / or buffers, wherein the pH adjuster includes one or more combinations of sodium carbonate, sodium bicarbonate, sodium phosphate, disodium hydrogen phosphate, and calcium carbonate; and the buffer includes one or more combinations of carob gum, glycerin, and propylene glycol.

[0016] Furthermore, sweeteners include one or more combinations of mannitol, sorbitol, sucrose, saccharin, sucralose, glucose, maltose, corn syrup, cyclamate, aspartame, acesulfame potassium, steviol glycosides, xylitol, salts of butyric acid (e.g., potassium butyric acid), alitane, cyclohexanesulfonic acid and its salts, glycyrrhizin, dihydrochalcone, kiwifruit protein, indigofera protein, or steviol glycosides.

[0017] Another aspect of this patent provides a nicotine-filled particle, which is prepared by the above-described method for preparing nicotine-filled particles.

[0018] Furthermore, the particle size of the nicotine-filled particles is 150~200μm, 200~300μm, or 300~500μm.

[0019] Furthermore, the porosity of the nicotine-filled particles is less than 35%.

[0020] Another aspect of this patent provides a nicotine pouch, comprising a saliva-permeable pouch and the aforementioned nicotine filling particles.

[0021] Furthermore, the amount of nicotine filling particles added to each nicotine bag is 400~600 mg, 600~800 mg, 800~1200 mg, 1200~1500 mg, or 1500~2000 mg.

[0022] Furthermore, the saliva-permeable pouch is made of medical-grade nonwoven fabric, lyocell, modal, or Tencel; the medical-grade nonwoven fabric is one or more combinations of polypropylene fiber, polyester fiber, polyamide fiber, polytetrafluoroethylene fiber, and glass fiber.

[0023] Furthermore, the cumulative dissolution rate of nicotine in the nicotine bag reached 100% from minute 0 to minute 30.

[0024] This patent provides a method for preparing nicotine pouches and nicotine-filled granules. Without other pellets, the method involves pre-wetting a mixture of powdered nicotine salts and additives, then precisely controlling parameters in a fluidized bed. A binder solution is sprayed onto the surface of the pre-wetted mixture to prepare the nicotine-filled granules. This reduces abnormalities such as adhesion, clumping, and excessive dust during granulation, thus improving the stability of the nicotine-filled granules. This not only improves production efficiency but also increases the final product yield and reduces production costs due to a higher proportion of particles within the target particle size range. Furthermore, nicotine pouches prepared using nicotine-filled granules as the filling material exhibit better nicotine dissolution, more stable nicotine release, and a full, consistent flavor in the mouth without abrupt drops or decay, providing consumers with a better consumption experience. Attached Figure Description

[0025] The above content of this patent 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 solution.

[0026] Figure 1 This is a scanning electron microscope image of the nicotine-filled particles in Embodiment 1 of this patent; Figure 2 This is a scanning electron microscope image of the nicotine-filled particles in Embodiment 2 of this patent; Figure 3 This is a scanning electron microscope image of the nicotine-filled particles in Comparative Example 1 of this patent. Figure 4 This is a scanning electron microscope image of the nicotine-filled particles in Comparative Example 2 of this patent. Figure 5 This is a scanning electron microscope image of the nicotine-filled particles in Comparative Example 3 of this patent. Figure 6 Scanning electron microscope image of nicotine-filled particles in Comparative Example 4 of this patent; Figure 7 The nicotine dissolution curve of the nicotine bag in Test Example 1 of this patent is shown (where the horizontal axis is time in (min); the vertical axis is dissolution rate, indicated by (%)). Detailed Implementation

[0027] 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.

[0028] 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 to be modified in all cases by the terms "within the unavoidable margin of error" or "approximately". Therefore, the numerical values ​​presented herein are approximate and may vary depending on the desired properties sought to be obtained by this patent. 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.

[0029] All other terms used herein for special definition are intended to have the general meaning understood by one of ordinary skill in the art, and in particular, meaning that one of ordinary skill in the art, upon reading the claims, specification and drawings of this patent, can directly and without doubt determine how the technical solution of this patent can be implemented.

[0030] 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 patent, a person 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 eliminate various incorrect interpretations that are not aimed at achieving the purpose of this patent.

[0031] 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.

[0032] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions.

[0033] Unless otherwise specified, all the technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0034] 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.

[0035] 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.

[0036] 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.

[0037] 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).

[0038] Unless otherwise specified, percentages (%) in this document refer to percentages by mass relative to the composition.

[0039] Unless otherwise stated herein, the sum of the contents of the components in the composition is 100%.

[0040] 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.

[0041] Unless otherwise specified, the term "a" as used in this specification means "at least one".

[0042] 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.

[0043] 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.

[0044] 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.

[0045] This patent provides a method for preparing nicotine bags and nicotine-filled granules, comprising the following steps: S1. Preparation of nicotine-filled particles, the specific steps are as follows: (1) Mix 1.0-3.0% by weight of nicotine salt powder (2.0% by weight of nicotine base), 92.0-94.0% by weight of filler, 3.0-5.0% by weight of sweetener and 0.4-0.7% by weight of pH buffer to obtain a powder mixture.

[0046] The nicotine salt powder includes one or more combinations of nicotine hydrochloride, nicotine dihydrochloride, nicotine citrate, nicotine tartrate, nicotine hydrogen tartrate, nicotine hydrogen tartrate dihydrate, nicotine sulfate, nicotine resin salt, or nicotine salicylate.

[0047] Fillers include one or a combination of two of microcrystalline cellulose (MCC), powdered cellulose, or starch.

[0048] Sweeteners include one or more combinations of mannitol, sorbitol, sucrose, saccharin, sucralose, glucose, maltose, corn syrup, cyclamate, aspartame, acesulfame potassium, steviol glycosides, xylitol, salts of butyric acid (e.g., potassium butyric acid), alitane, cyclohexanesulfonic acid and its salts, glycyrrhetinic acid, dihydrochalcone, kiwifruit protein, indigofera protein, or steviol glycosides.

[0049] pH buffers are used to adjust the overall pH value. pH buffers include pH adjusters and / or buffers, wherein pH adjusters include one or more combinations of sodium carbonate, sodium bicarbonate, sodium phosphate, disodium hydrogen phosphate, and calcium carbonate; and buffers include one or more combinations of carob gum, glycerin, and propylene glycol.

[0050] (2) Add 1-5% pure water by mass to the powder mixture prepared in step (1) above for pre-wetting treatment to obtain a premix.

[0051] (3) Mix the adhesive with pure water at a mass ratio of 1:17~21 to obtain an adhesive aqueous solution with a mass concentration of 4.5~5.5%, which is the adhesive solution.

[0052] The adhesive includes an aqueous solution of hydroxypropyl methylcellulose (HPMC), polyvinylpyrrolidone (PVP), or hydroxypropyl cellulose (HPC). In some other embodiments, ethanol may also be used as a solvent to dissolve the adhesive.

[0053] (4) Place the premix prepared in step (2) and the binder solution prepared in step (3) into a small top-spray fluidized bed granulator (commercially available, expansion chamber working volume about 10 L). Adjust the air inlet temperature of the small top-spray fluidized bed granulator to 80~95℃, the air velocity to 0.5~1.5 m / s, the spray rate of the binder solution to 10~30 g / min, the atomization pressure of the binder to 0.1~0.3 MPa, and maintain the temperature of the powder bed sprayed to 40~45℃. After stopping the spraying, continue drying and then remove excess powder by sieving to obtain nicotine-filled granules.

[0054] S2. Prepare the nicotine pouch, the specific steps of which are as follows: The nicotine-filled granules prepared in step S1 above are placed in a saliva-permeable pouch as the contents, and then cut, sealed, heat-pressed and sterilized with ultraviolet light to obtain a nicotine pouch. Each nicotine pouch contains 400-2000 mg of contents and 0.1-1.0 mg of nicotine.

[0055] Saliva-permeable sachets can be made of medical-grade nonwoven fabric, lyocell, modal, or tencel. The quantitative dosage of saliva-permeable sachets can be 25-35 g / m³. 2 Among them, medical-grade nonwoven fabric is one or more combinations of polypropylene fiber, polyester fiber, polyamide fiber, polytetrafluoroethylene fiber and glass fiber.

[0056] Example 1

[0057] S1. Preparation of nicotine-filled particles, the specific steps are as follows: (1) Mix 2.0% nicotine tartrate powder, 93.5% microcrystalline cellulose powder (commercially available, MCC PH-102), 4.0% mannitol and 0.5% sodium bicarbonate solution evenly to obtain a powder mixture.

[0058] (2) Add 1% pure water by mass to the powder mixture prepared in step (1) above for pre-wetting treatment, let stand for 15 min, and obtain the premix.

[0059] (3) Mix hydroxypropyl methylcellulose (commercially available, HPMC E5) and pure water at a mass ratio of 1:19 to obtain a 5% hydroxypropyl methylcellulose aqueous solution, which is the adhesive solution.

[0060] (4) Place the premix prepared in step (2) and the binder solution prepared in step (3) into a small top-spray fluidized bed granulator (commercially available, expansion chamber working volume about 10 L). Adjust the air inlet temperature of the small top-spray fluidized bed granulator to 80℃, the air velocity to 0.5 m / s, the spray rate of the binder solution to 10 g / min, the atomization pressure of the binder to 0.1 MPa, and maintain the temperature of the powder bed sprayed to 40~45℃. After stopping the spraying, continue drying and then remove excess powder by sieving to obtain nicotine-filled granules.

[0061] The nicotine-filled particles were observed using a scanning electron microscope, and the results are as follows: Figure 1 As shown, the particles are finer, have better uniformity in size distribution, and moderate agglomeration. The yield of the obtained particles (150~500μm) is 96.5%, the porosity is 32%, and the angle of repose is 28°, showing excellent flowability. However, the excessively fine particles may cause the nicotine release rate to be too fast. Although the effect is rapid, the duration of action is weakened.

[0062] S2. Prepare the nicotine pouch, the specific steps of which are as follows: The nicotine-filled granules prepared in step S1 above are placed in a saliva-permeable pouch as the contents, and then cut, sealed, heat-pressed and sterilized with ultraviolet light to obtain a nicotine pouch. Each nicotine pouch contains 500 mg of contents and 0.1 mg of nicotine.

[0063] Example 2

[0064] S1. Preparation of nicotine-filled particles, the specific steps are as follows: (1) Mix 2.0% nicotine tartrate powder, 93.5% microcrystalline cellulose powder (commercially available, MCC PH-102), 4.0% mannitol and 0.5% sodium carbonate-glycerol solution evenly to obtain a powder mixture.

[0065] (2) Add 1% pure water by mass to the powder mixture prepared in step (1) above for pre-wetting treatment, let stand for 15 min, and obtain the premix.

[0066] (3) Mix hydroxypropyl methylcellulose (commercially available, HPMC E5) and pure water at a mass ratio of 1:19 to obtain a 5% hydroxypropyl methylcellulose aqueous solution, which is the adhesive solution.

[0067] (4) The premix prepared in step (2) and the binder solution prepared in step (3) are placed in a small top-spray fluidized bed granulator (commercially available, expansion chamber working volume about 10 L). The air inlet temperature of the small top-spray fluidized bed granulator is adjusted to 95℃, the air velocity is 1.5 m / s, the spray rate of the binder solution is 30 g / min, the atomization pressure of the binder is 0.3 MPa, and the temperature of the sprayed powder bed is maintained at 40~45℃. After stopping the spraying, continue drying and then remove excess powder by sieving to obtain nicotine-filled granules.

[0068] The nicotine-filled particles were observed using a scanning electron microscope, and the results are as follows: Figure 2 As shown, the uniformity of single particle size distribution is at a moderate level, with fewer clusters. The moderate particle size and clustering can achieve a balance between the saliva penetration rate and the nicotine release rhythm.

[0069] S2. Prepare the nicotine pouch, the specific steps of which are as follows: The nicotine-filled granules prepared in step S1 above are placed in a saliva-permeable pouch as the contents, and then cut, sealed, heat-pressed and sterilized with ultraviolet light to obtain a nicotine pouch. Each nicotine pouch contains 500 mg of contents and 0.1 mg of nicotine.

[0070] Comparative Example 1

[0071] Compared with Example 1, the difference is that this comparative example does not use pure water for pre-wetting treatment to prepare nicotine filling particles, and the nicotine filling particles are placed in saliva-permeable pouches with the same filling amount as in Example 1. The nicotine pouches are obtained by cutting, sealing, hot pressing and ultraviolet sterilization.

[0072] The nicotine-filled particles were observed using a scanning electron microscope, and the results are as follows: Figure 3 As shown, the particle agglomeration units are relatively large, the particle size distribution is generally uniform, and the agglomeration is strong. This characteristic can reduce the risk of local particle accumulation in the filter bag and reduce the foreign body sensation during use. However, insufficient size uniformity can easily lead to local fluctuations in nicotine loading, affecting the consistency of product efficacy experience. Compared with Example 1, the fine powder separation during granulation increased by 30%, resulting in material waste.

[0073] Comparative Example 2

[0074] Compared with Example 1, the difference is that the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example is adjusted to 70°C, the air velocity is 1.0 m / s, the spray rate of the adhesive solution is 15 g / min, the atomization pressure of the adhesive is 0.2 MPa, the temperature of the sprayed powder bed is maintained at 40~45°C, the spraying is stopped and drying continues, and then the excess powder is removed by sieving to obtain nicotine-filled granules. The nicotine-filled granules are placed in saliva-permeable pouches with the same filling amount as in Example 1. After shearing, sealing, hot pressing and ultraviolet sterilization, nicotine bags are obtained.

[0075] The nicotine-filled particles were observed using a scanning electron microscope, and the results are as follows: Figure 4 As shown, due to the excessively low inlet air temperature, the drying process was too slow, resulting in excessively wet particles that agglomerated into large clumps, leading to a low yield.

[0076] Comparative Example 3

[0077] Compared with Example 1, the difference is that the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example is adjusted to 105°C, the air velocity is 1.0 m / s, the spray rate of the adhesive solution is 15 g / min, the atomization pressure of the adhesive is 0.2 MPa, the temperature of the sprayed powder bed is maintained at 40~45°C, the spraying is stopped and drying continues, and then the excess powder is removed by sieving to obtain nicotine-filled granules. The nicotine-filled granules are placed in saliva-permeable pouches with the same filling amount as in Example 1. After shearing, sealing, hot pressing and ultraviolet sterilization, nicotine bags are obtained.

[0078] The nicotine-filled particles were observed using a scanning electron microscope, and the results are as follows: Figure 5 As shown, due to the excessively high inlet air temperature, the drying process was too fast. The adhesive droplets did not spread sufficiently on the surface of the particles before drying, resulting in a lot of fine powder, loose and brittle particles, and excessively high porosity (>50%).

[0079] Comparative Example 4

[0080] Compared with Example 1, the difference is that the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example is adjusted to 85°C, the air velocity is 0.3 m / s, the spray rate of the adhesive solution is 15 g / min, the atomization pressure of the adhesive is 0.2 MPa, the temperature of the sprayed powder bed is maintained at 40~45°C, the spraying is stopped and drying continues, and then the excess powder is removed by sieving to obtain nicotine-filled granules. The nicotine-filled granules are placed in saliva-permeable pouches with the same filling amount as in Example 1. After shearing, sealing, hot pressing and ultraviolet sterilization, nicotine bags are obtained.

[0081] The nicotine-filled particles were observed using a scanning electron microscope, and the results are as follows: Figure 6 As shown, due to the low flow rate and insufficient fluidization, channeling occurs in the bed, the particle size is extremely uneven, and there is localized over-wetting.

[0082] Comparative Example 5

[0083] Compared to Example 1, the difference lies in the following: the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example was adjusted to 85°C, the air velocity to 2.0 m / s, the spray rate of the binder solution to 15 g / min, the atomization pressure of the binder to 0.2 MPa, and the temperature of the powder bed maintained at 40~45°C. After spraying was stopped, drying continued, and then excess powder was removed by sieving. The results showed that due to the excessively high flow rate, the contact time between the particles and the spray droplets was too short, resulting in a large amount of fine powder being carried out of the system, leading to a low effective yield and difficulty in particle growth. In other words, nicotine-filled particles could not be obtained, and nicotine bags could not be prepared.

[0084] Comparative Example 6

[0085] Compared to Example 1, the difference lies in the following: the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example was adjusted to 85°C, the air velocity to 1.0 m / s, the spray rate of the binder solution to 5 g / min, the atomization pressure of the binder to 0.2 MPa, and the temperature of the powder bed sprayed onto the powder was maintained at 40~45°C. After spraying was stopped, drying continued, and then excess powder was removed by sieving. The results showed that due to the excessively low spray rate, particle growth was slow and efficiency was low. Furthermore, the long atomization time could lead to the loss of heat-sensitive components, making it impossible to prepare nicotine bags.

[0086] Comparative Example 7

[0087] Compared to Example 1, the difference lies in the following: the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example was adjusted to 85°C, the air velocity to 1.0 m / s, the spray rate of the binder solution to 40 g / min, the atomization pressure of the binder to 0.2 MPa, and the temperature of the powder bed sprayed onto the granulator was maintained at 40~45°C. After spraying was stopped, drying continued, and then excess powder was removed by sieving. The results showed that due to the excessively high spray rate, exceeding the drying capacity, the granules quickly became too wet and agglomerated, fluidization stopped, and production failed, meaning nicotine-filled granules could not be obtained, and nicotine bags could not be prepared.

[0088] Comparative Example 8

[0089] Compared to Example 1, the difference lies in the following: the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example was adjusted to 85°C, the air velocity to 1.0 m / s, the spray rate of the adhesive solution to 15 g / min, the atomization pressure of the adhesive to 0.05 MPa, and the temperature of the powder bed maintained at 40~45°C. After spraying was stopped, drying continued, and then excess powder was removed by sieving. The results showed that due to the excessively low atomization pressure and large droplet size, the spraying was uneven, resulting in a small number of large particles and a large amount of undersized fine powder, making it impossible to obtain nicotine-filled particles and thus impossible to prepare nicotine bags.

[0090] Comparative Example 9

[0091] Compared to Example 1, the difference lies in the following: the inlet air temperature of the small top-spray fluidized bed granulator in this comparative example was adjusted to 85°C, the air velocity to 1.0 m / s, the spray rate of the binder solution to 15 g / min, the atomization pressure of the binder to 0.5 MPa, and the temperature of the powder bed maintained at 40-45°C. After spraying was stopped, drying continued, and then excess powder was removed by sieving. The results showed that due to excessively high atomization pressure, the droplets were too fine and easily evaporated, making it difficult for the particles to grow effectively. This also resulted in excessive fine powder, meaning that nicotine-filled granules could not be obtained, and nicotine bags could not be prepared.

[0092] Comparative Example 10

[0093] The nicotine bag in this comparative example was prepared using the method shown in the patent document with publication number CN119837290A.

[0094] Test Example 1: Nicotine Dissolution Curve Experiment

[0095] The nicotine bags prepared in Examples 1-2 and Comparative Examples 2-4 were tested for dissolution using a dissolution apparatus-paddle method. Simulated artificial saliva was used as the dissolution medium with a pH of 6.8. The dissolution was carried out at a temperature of 37°C and a rotation speed of 80 rpm / min. The dissolution of nicotine was detected every 5 minutes using a high-performance liquid chromatograph.

[0096] The dissolution rate test results are shown in Table 1 and Figure 7 As shown, the nicotine bags prepared using the methods in Examples 1 and 2 exhibit good stability, uniform dissolution, and controllable, linear release at the endpoint, with similar release characteristics for both types of particles. However, the nicotine bag prepared using the method shown in Comparative Example 2 shows rapid burst release, with a nicotine dissolution rate exceeding 50% within 5 minutes. This release is premature, reaching 100% dissolution within 20 minutes, and cannot be sustained. The nicotine bag prepared using the method shown in Comparative Example 3 shows slow dissolution in the early stages and rapid release in the later stages. Although it reaches 100% dissolution by 30 minutes, the dissolution is delayed, with rapid dissolution in the last 5 minutes. The nicotine bag prepared using the method shown in Comparative Example 4 exhibits irregular release, reaching approximately 100% dissolution between 25 and 30 minutes. The nicotine bag prepared using Comparative Example 10 shows rapid burst release, reaching approximately 100% dissolution within about 15 minutes, and cannot be sustained.

[0097] Table 1. Statistical table of cumulative nicotine release rate in different nicotine bags

[0098] Test Example 2: Taste Test

[0099] The taste test method is as follows: a professional evaluation team (n=5) conducts the evaluation, and the nicotine pouches prepared in Examples 1-2 and Comparative Examples 2-4 are placed directly between the upper lip and the upper teeth, with a standard consumption time of 30 minutes.

[0100] The results showed that the nicotine pouches prepared by the methods shown in Examples 1 and 2 exhibited relatively mild nicotine release with no obvious throat irritation or burning sensation in the initial stage of ingestion (0-2 minutes). In the middle stage (3-15 minutes), the release was relatively stable, with a full and consistent flavor in the mouth, without any abrupt drops or decline. Even in the later stage (16-30 minutes), the unique flavor was maintained. In contrast, the nicotine pouch prepared by the method in Comparative Example 2 exhibited a noticeable throat burning sensation within 1 minute of ingestion, indicating an excessively strong initial impact. The nicotine pouch prepared by the method in Comparative Example 3 showed slow nicotine release from the initial to middle stage (5-10 minutes after ingestion), with an overly pronounced sweetness, resulting in a slow establishment of nicotine satisfaction. The nicotine pouch prepared by the method in Comparative Example 4 showed excessively rapid nicotine release from the initial to middle stage (5-20 minutes after ingestion), resulting in a relatively mild initial sensation, a sudden and noticeable throat burning sensation in the middle stage, and almost no sensation in the later stage, leading to a poor overall experience. The nicotine pouches prepared by the method in Comparative Example 10 all had a strong irritant sensation in the initial stage (5-10 minutes after ingestion), with a noticeable burning sensation in the throat. The irritant sensation dropped abruptly after about 15 minutes, and only sweetness remained in the later stage, resulting in a poor experience.

[0101] Therefore, it can be concluded that this patent provides a method for preparing nicotine pouches and nicotine-filled granules. Without other pellet cores, the method involves pre-wetting a mixture of powdered nicotine salts and additives, then precisely controlling parameters in a fluidized bed, and spraying a binder solution onto the surface of the pre-wetted premix to prepare the nicotine-filled granules. This reduces abnormalities such as adhesion, clumping, and excessive dust during granulation, thus improving the stability of the nicotine-filled granules. This not only improves production efficiency but also increases the final product yield and reduces production costs due to a higher proportion of particles within the target particle size range. Furthermore, nicotine pouches prepared using nicotine-filled granules as the filling material exhibit better nicotine dissolution, more stable nicotine release, and a full, consistent flavor in the mouth without abrupt drops or decay, resulting in a better consumer experience.

[0102] In the foregoing description of exemplary embodiments / specific implementations of this patent, various features of this patent 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 inventive aspects. However, unless expressly stated otherwise or in obvious technical contradiction or exclusion, the descriptive method of this patent should not be construed as reflecting an intention that the claimed features of the invention are more than expressly stated in each claim. 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, each claim existing independently as a separate embodiment / specific implementation of this patent.

[0103] The terms 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 this patent claim. Therefore, it should be understood that while this patent has been specifically disclosed through preferred embodiments, exemplary embodiments, and optional features, variations or modifications of the concepts disclosed herein may be adopted by those skilled in the art, and such variations and modifications are therefore considered to be within the scope of this patent as defined by the appended claims. The specific embodiments given in this specification are examples of useful embodiments of this patent, and it will be apparent to those skilled in the art that this patent can be implemented using many variations of the devices, device components, and method steps disclosed herein.

[0104] The foregoing description of specific embodiments fully discloses the general features of this patent, 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 or deviation from the general concept of this patent. 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 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.

[0105] Furthermore, the scope of this patent should not be limited to any of the exemplary embodiments described above, but only to the appended claims and their equivalents.

Claims

1. A method for preparing nicotine-filled particles, characterized in that, Includes the following steps: Step A: Mix nicotine salt powder with additive powder to obtain a powder mixture; Step B: Pre-wet the powder mixture with pure water to obtain a premix; Step C: Place the premix and the binder solution in a fluidized bed granulator to prepare the nicotine-filled granules.

2. The method for preparing nicotine-filled particles according to claim 1, characterized in that, In step B, the pure water is 1-2%, 2-3%, or 3-5% of the mass of the powder mixture.

3. The method for preparing nicotine-filled particles according to claim 1, characterized in that, In step C The concentration of the adhesive solution is 4.5-5.5%; The specific parameters of the fluidized bed granulator are as follows: inlet air temperature is 80~95℃, air velocity is 0.5~1.5 m / s, spray rate of adhesive solution is 10~30 g / min, atomization pressure of adhesive is 0.1~0.3 MPa, and the temperature of the sprayed powder bed is maintained at 40~45℃.

4. The method for preparing nicotine-filled particles according to claim 1, characterized in that, In step A The nicotine salt powder has a mass percentage of 1.0~3.0%; The additive powder comprises 92.0-94.0% by weight of filler, 3.0-5.0% by weight of sweetener, and 0.4-0.7% by weight of pH buffer. The filler includes one or a combination of two of microcrystalline cellulose, powdered cellulose, or starch; The pH buffer is used to adjust the overall pH value. The pH buffer includes a pH adjuster and / or a buffer. The pH adjuster includes one or more combinations of sodium carbonate, sodium bicarbonate, sodium phosphate, disodium hydrogen phosphate, and calcium carbonate. The buffer includes one or more combinations of carob gum, glycerin, and propylene glycol.

5. A nicotine-filled granule, characterized in that, The filler particles are prepared by the method for preparing nicotine filler particles according to any one of claims 1 to 4.

6. The nicotine-filled particles according to claim 5, characterized in that, The nicotine-filled particles have a particle size of 150~200 μm, 200~300 μm, or 300~500 μm; The porosity of the nicotine-filled particles is less than 35%.

7. A nicotine bag, characterized in that, Includes saliva-permeable pouches and nicotine-filled particles as described in any one of claims 1 to 6.

8. The nicotine bag according to claim 7, characterized in that, The amount of nicotine-filling particles added to each nicotine bag is 400-600 mg, 600-800 mg, 800-1200 mg, 1200-1500 mg, or 1500-2000 mg.

9. The nicotine bag according to claim 8, characterized in that, The saliva-permeable pouch is made of medical-grade nonwoven fabric, lyocell, modal, or Tencel; the medical-grade nonwoven fabric is one or more combinations of polypropylene fiber, polyester fiber, polyamide fiber, polytetrafluoroethylene fiber, and glass fiber.

10. The nicotine bag according to claim 9, characterized in that, The cumulative dissolution rate of nicotine in the nicotine bag reaches 100% from minute 0 to minute 30.

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