Capsule and method for preparing the same
The capsule with a core material and gelled shell, using cellulose and low molecular weight lipid, addresses encapsulation issues in hydrophilic formulations, achieving high yield and stable aerosol release in aerosol generating articles.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- SHENZHEN HUABAO COLLABORATIVE INNOVATION TECH RES INST CO LTD
- Filing Date
- 2025-02-28
- Publication Date
- 2026-05-07
AI Technical Summary
Existing capsule technologies for hydrophilic formulations face issues such as unstable encapsulation, unpleasant odors, high viscosity, brittle shells, low yield rates, and poor storage stability, especially when used as aerosol generating substrates, leading to inconsistent release and poor uniformity.
A capsule with a core material comprising a hydrophilic liquid formulation, lipophilic formulation, and structuring agent, including cellulose and/or cellulose derivatives, low molecular weight lipid, and surfactant, encapsulated by a gelled shell, which is prepared using a concentric dropper method to ensure stable encapsulation and uniformity.
The solution achieves high yield rates, stable encapsulation, and consistent aerosol release, overcoming issues of odor, viscosity, and storage stability, suitable for use in aerosol generating articles like heat-not-burn products.
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Figure PCTCN2025079828-FTAPPB-I100001 
Figure PCTCN2025079828-FTAPPB-I100002 
Figure PCTCN2025079828-FTAPPB-I100003
Abstract
Description
CAPSULE AND METHOD FOR PREPARING THE SAMEThis application claims the benefit of priority to Chinese Patent Application No. 202411548964. X, filed on October 30, 2024 with China National Intellectual Property Administration, and entitled “CAPSULE AND METHOD FOR PREPARING THE SAME” , the entire disclosure of which is incorporated herein by reference.TECHNICAL FIELD
[0001] The present disclosure relates to the technical field of material encapsulating, and more particularly, to a capsule and a method for preparing the same.BACKGROUND
[0002] Capsule with a core-shell structure can provide good protection for contents therein from influence of an external environment on composition of the contents. A traditional capsule includes a content of an oil soluble system and a shell liquid of a water soluble system. The oil soluble content is encapsulated by the water soluble shell liquid. When the system of the content contains a hydrophilic component, the shell liquid may be dissolved and cannot encapsulate.
[0003] In the prior art, a variety of capsule technologies have been developed to encapsulate hydrophilic formulations. Where, light curing dropping method is relatively mature, but a gelled shell prepared thereby contains plastic, resin, rubber and other components, and may go through a light curing process requiring a photoinitiator, photosensitizer and the like. As a result, the gelled shell prepared based on the foregoing materials is easy to retain a heavier plastic smell or special smell. Especially when the capsule is used as an aerosol generating substrate, the gelled shell is easy to release unpleasant odor and even harmful substances in a heating environment, which is not conducive to smoking experience. In an early technology, there is also a technology for preparing a hydrophilic capsule by a water-in-oil dropping method. However, in a preparation system of water-in-oil, a gelled shell is made of waxy materials, which will lead to higher viscosity of gelled shell materials, lower dropping yield, and a brittle and fragile waxy gelled shell, such that it is not conducive to industrial production and processing, and the contents are also easy to ooze out and cannot be stored for a long time. In improved three-layer dropping technology, a hydrophilic capsule is prepared by water-in-oil, and has an outermost layer coated with a layer of gelled shell, which will lead to an excessive shell thickness, a relatively low ratio of hydrophilic material, difficulty in actual use, such as pinching and exploding, and a relatively low rate of the gelled shell when releases by heat. Further, the preparation process is complex, and a liquid core is easy to break through a middle layer and contact an outer layer of a hydrophilic gelled shell, which will lead to an uncontrollable yield rate. in addition, long-term storage will also cause an internal liquid to ooze out slowly. There is also a coagulation preparation technology, for example, polylactic acid is used, stirred and solidified to form a gelled shell. Capsules prepared by this method may have a wide particle size distribution, inconsistent shapes, generally hardly generated very round spherical shapes, and uneven distribution shell thicknesses thereof. And thus, there is a large deviation in applications of the capsules, especially poor uniformity when they release by heat. There is also a hydrophilic capsule technology where sodium alginate is used as a gelled shell. However, a capsule obtained by this technology cannot be stored and applied in a dry environment, especially when a liquid core thereof is not treated, an internal hydrophilic formulation is easy to ooze out, and drying of the capsule cannot be realized.
[0004] Although the above-mentioned prior art provides preparation methods for preparing a capsule containing hydrophilic components as a content, they all have various defects. When the hydrophilic components are liquid formulations such as glycerol, propylene glycol, etc., especially when the contents of the liquid formulations are relatively large, either stable encapsulation cannot be achieved, or storage stability is poor, or there is miscellaneous odor, or uniformity is not enough, which is inconvenient to be used as an aerosol generating substrate.SUMMARY
[0005] Embodiments of the present disclosure provide a capsule and a method for preparing the same.
[0006] The capsule includes a core material and a gelled shell encapsulating the core material. The core material includes a hydrophilic liquid formulation, a lipophilic formulation and a structuring agent. The structuring agent includes cellulose and / or cellulose derivatives, and further, a low molecular weight lipid and a surfactant. The core material is a paste, a colloid or a solid-liquid mixture. The capsule is commonly known as seamless capsule and is typically spherical.
[0007] According to some embodiments, the surfactant has an HLB value of 2 to 10.
[0008] According to some embodiments, the surfactant has an HLB value of 4 to 7.
[0009] According to some embodiments, the hydrophilic liquid formulation accounts for 5 wt%to 60 wt%of a weight of the core material.
[0010] According to some embodiments, the hydrophilic liquid formulation accounts for 15 wt%to 50 wt%of a weight of the core material.
[0011] According to some embodiments, the lipophilic formulation accounts for 20 wt%to 80 wt%of a weight of the core material, and the structuring agent accounts for 5 wt%to 20 wt%of a weight of the core material.
[0012] According to some embodiments, the cellulose and / or cellulose derivatives and the low molecular weight lipid together account for 70 wt%to 95 wt%of a weight of the structuring agent, and the surfactant accounts for 30 wt%to 5 wt%of a weight of the structuring agent.
[0013] According to some embodiments, a weight ratio of the cellulose and / or cellulose derivatives to the low molecular weight lipid is 20: 1~1: 1.
[0014] According to some embodiments, the cellulose and / or cellulose derivatives have a viscosity of 1 mPa·s to 300 mPa·s (5 wt%solution in 80 wt%toluene and 20 wt%ethanol) , and account for 1 wt%to 10 wt%of a weight of the core material.
[0015] According to some embodiments, the cellulose and / or cellulose derivatives are at least one of cellulose acetate, nitrocellulose and ethylcellulose.
[0016] According to some embodiments, the low molecular weight lipid is at least one selected from a group consisting of animal wax, plant wax, mineral wax, synthetic wax, lecithin and derivatives thereof, plant sterol and esters thereof, fatty acid and esters thereof, triglyceride, and fatty alcohol.
[0017] According to some embodiments, the low molecular weight lipid is insect wax, beeswax, palm wax, or β-sitosterol.
[0018] According to some embodiments, the surfactant is at least one selected from a group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and amphoteric surfactants.
[0019] According to some embodiments, the surfactant is a combination of Tween and at least one of glycerol monooleate and span.
[0020] According to some embodiments, the lipophilic formulation is at least one selected from a group consisting of animal oils, vegetable oils, microbial gel and mineral oils.
[0021] According to some embodiments, the gelled shell contains a gelling agent and a curing agent.
[0022] According to some embodiments, the gelling agent is at least one selected from a group consisting of animal gel, vegetable gel, starch and modified starch, and the curing agent is a polyol.
[0023] According to some embodiments, the hydrophilic liquid formulation contains an aerosol generating substance releasable by heat.
[0024] According to some embodiments, the aerosol generating substance releasable by heat includes at least one of propylene glycol and glycerol.
[0025] According to some embodiments, propylene glycol and glycerol account for 80 wt%to 100 wt%of a total weight of the hydrophilic liquid formulation.
[0026] According to some embodiments, the core material further contains 0.1 wt%to 20 wt%of nicotine and / or a nicotine salt.
[0027] According to some embodiments, the core material further contains 0.1 wt%to 20 wt%of a flavor and / or an extract, and the extract generally refers to an animal or plant extract, preferably a plant extract, more preferably a tobacco extract.
[0028] According to some embodiments, a weight ratio of propylene glycol to glycerol is 2: 8~8: 2.
[0029] According to some embodiments, the capsule has a particle size of 0.5 mm to 8 mm.
[0030] According to some embodiments, the capsule has a particle size of 1 mm to 3 mm.
[0031] According to some embodiments, the gelled shell has a thickness of 50 μm to 150 μm.
[0032] The embodiments of the present disclosure further provide an application of the capsule described above in an aerosol generating article.
[0033] The embodiments of the present disclosure further provide a method for preparing the capsule described above. The method includes the following steps:
[0034] mixing a material containing a hydrophilic liquid formulation, a lipophilic formulation and a structuring agent to prepare a core material;
[0035] preparing a material containing a gelling agent, a curing agent and water into a shell liquid; and
[0036] encapsulating the core material with the shell liquid to prepare the capsule.
[0037] According to some embodiments, the core material and the shell liquid are dropped through a concentric dropper and dried to prepare the capsule.
[0038] The embodiments of the present disclosure further provide an aerosol generating article including an aerosol generating substrate. The aerosol generating substrate includes the capsule described above. The aerosol generating article is preferably a heat-not-burn (HNB) product, also referred to as a heated tobacco product (HTP) , low-temperature cigarette product, or generically as a heated product.
[0039] According to some embodiments, the aerosol generating article is a heat not burn product. According to some embodiments, the capsule is used as an aerosols generating substrate.
[0040] According to some embodiments, the aerosol generating article has a temperature of release by heat greater than 150 ℃.
[0041] According to some embodiments, the aerosol generating article has a temperature of release by heat of 200 ℃ to 300 ℃.
[0042] According to some embodiments, the capsule is used to provide a fragrance.
[0043] The embodiments of the present disclosure provide a capsule and a method for preparing the same. The capsule includes a core material and a gelled shell encapsulating the core material. The core material includes a hydrophilic liquid formulation, a lipophilic formulation and a structuring agent. The structuring agent includes cellulose and / or cellulose derivatives, and further, a low molecular weight lipid and a surfactant. The core material is a paste, a colloid or a solid-liquid mixture. The core material can realize stable dispersion and fixation of the hydrophilic liquid formulation in the lipophilic formulation, such that the gelled shell can stably encapsulate the core material. The present disclosure further discloses an aerosol generating article of the above-mentioned capsule, where low temperature release by heat can be realized when the capsule is used as an aerosol generating substrate.DETAILED DESCRIPTION
[0044] The capsule according to the embodiments of the present disclosure includes a core material and a gelled shell encapsulating the core material. The core material includes a hydrophilic liquid formulation, a lipophilic formulation and a structuring agent. The structuring agent includes cellulose and / or cellulose derivatives, a low molecular weight lipid and a surfactant. The core material is a paste, a colloid or a solid-liquid mixture.
[0045] Combination of cellulose and / or cellulose derivatives and the low molecular weight lipid in the capsule according to the embodiments of the present disclosure is conducive to forming a network structure beneficial to dispersion and fixation of the hydrophilic liquid formulation in the lipophilic formulation. The surfactant is conducive to forming an oil film between the core material and the gelled shell layer, thereby helping to realize the gelled shell encapsulating the core material. The core material formed by the hydrophilic liquid formulation, the lipophilic formulation and the structuring agent is a paste, a colloid or a solid-liquid mixture at room temperature (25 ℃) , which is conducive to realizing the gelled shell stably encapsulating the core material.
[0046] In some embodiments, the capsule has a yield rate above 50%. In some embodiments, the capsule has a yield rate above 60%. In some embodiments, the capsule has a yield rate above 70%. In some embodiments, the capsule has a yield rate above 80%. In some embodiments, the capsule has a yield rate above 90%. In some embodiments, the capsule has a yield rate above 95%. In some embodiments, the capsule has a yield rate of 100%.
[0047] In some embodiments, the surfactant has a Hydrophilic-Lipophilic Balance (HLB) value of 2 to 10. Further, the HLB value is 4 to 7. The foregoing ranges of the HLB value are conducive to formation of the core material in form of a paste, a colloid or a solid-liquid mixture, which is conducive to more stable encapsulation.
[0048] In some embodiments, the hydrophilic liquid formulation is water or a liquid formulation that can be uniformly dispersed in water molecules to form a solution, and specifically, may be for example, ethanol, glycerol, or propylene glycol, or the like.
[0049] In some embodiments, the hydrophilic liquid formulation accounts for 5 wt%to 60 wt%of a weight of the core material. In some embodiments, the hydrophilic liquid formulation accounts for 15 wt%to 50 wt%of a weight of the core material. In some embodiments, the hydrophilic liquid formulation accounts for 25 wt%to 45 wt%, and specifically, may account for, for example, 25wt%, 30wt%, 35wt%, 40wt%, or 45wt%, or the like, of a weight of the core material.
[0050] In some embodiments, the lipophilic formulation accounts for 20 wt%to 80 wt%of a weight of the core material. In some embodiments, the lipophilic formulation accounts for 30 wt%to 60 wt%, and specifically, may be, for example, 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%, 55 wt%, or 60wt%, or the like, of a weight of the core material.
[0051] In some embodiments, the structuring agent accounts for 5 wt%to 20 wt%of a weight of the core material. In some embodiments, the structuring agent accounts for 10 wt%to 15 wt%, and specifically, may be, for example, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or 15 wt%, or the like, of a weight of the core material.
[0052] In some embodiments, the cellulose and / or cellulose derivatives and the low molecular weight lipid together account for 70 wt%to 95 wt%of a weight of the structuring agent, and the surfactant accounts for 30 wt%to 5 wt%of a weight of the structuring agent. In some embodiments, the cellulose and / or cellulose derivatives and the low molecular weight lipid together account for 75 wt%, 80 wt%, 85 wt%, or 90 wt%, or the like, of a weight of the structuring agent.
[0053] In some embodiments, a weight ratio of the cellulose and / or cellulose derivatives to the low molecular weight lipid is 20: 1~1: 1, and specifically, may be, for example, 20: 1, 18: 1, 16: 1, 14: 1, 12: 1, 10: 1, 9: 1, 8: 1, 7: 1, 6: 1, 5: 1, 4: 1, 3: 1, 2: 1, or 1: 1, or the like.
[0054] In some embodiments, the cellulose and / or cellulose derivatives have a viscosity of 1 mPa·s to 300 mPa·s, and account for 1 wt%to 10 wt%of a weight of the core material. The viscosity is a viscosity of a solution of the cellulose and / or cellulose derivatives with a mass content of 5 wt%in a mixed solution of 80 wt%toluene and 20 wt%ethanol (EtOH) as a solvent. A too high proportion of the cellulose and / or cellulose derivatives in a weight of the core material may lead to a too great hardness formed core material, such that encapsulation may be difficult. A too low proportion of the cellulose and / or cellulose derivatives in a weight of the core material is not conducive to formation of a paste, a colloid or a solid-liquid mixture from the core material. The viscosity greater than 300 mPa·s is not conducive to droplet molding of a product. In some embodiments, the cellulose and / or cellulose derivatives are at least one of cellulose acetate, nitrocellulose and ethylcellulose.
[0055] In the capsule according to the embodiments of the present disclosure, the “low molecular weight” in the low molecular weight lipid is conventionally understandable in the technical field. In some embodiments, the low molecular weight lipid may be a lipid with a number average molecular weight below 3000. In some embodiments, the low molecular weight lipid is at least one selected from a group consisting of animal wax, plant wax, mineral wax, synthetic wax, lecithin and derivatives thereof, plant sterol and esters thereof, fatty acid and esters thereof, triglyceride, and fatty alcohol. Specifically, the animal wax may be, for example, beeswax, insect wax, Sichuan wax or spermaceti wax. Specifically, the plant wax may be, for example, palm wax, candelilla wax, rice wax, or sunflower wax, or the like. Specifically, the mineral wax may be, for example, paraffin, ozokerite, or microfine wax, or the like. Specifically, the synthetic wax may be, for example, a mixture of natural wax and a chemically synthesized resin, such as plastic wax, and the like. The plant sterol and esters thereof and the fatty acid and esters thereof may be, for example, β-sitosterol or γ-oryzanol, or the like.
[0056] In some embodiments, the surfactant is at least one selected from a group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and amphoteric surfactants. Specifically, the anionic surfactants may be, for example, sodium lauryl sulfate, triethanolamine lauryl sulfate, ammonium lauryl sulfate, sodium dodecylbenzene sulfonate, sodium stearate, semi-solidified sodium bovine fatty acid, semi-solidified hardened potassium bovine fatty acid, potassium stearate oleate, potassium castor oil, sodium alkyl naphthalene sulfonate, sodium dialkyl sulfosuccinate, sodium alkyl diphenyl ether disulfonate, diethanolamine alkyl phosphate, potassium alkyl phosphate, sodium polyoxyethylene alkyl sulfate, or sodium polyoxyethylene alkyl phenyl ether sulfate, or the like. Specifically, the cationic surfactants may be, for example, of lauryl trimethylammonium chloride, stearyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, distearyl dimethyl ammonium chloride, alkylphenedimethylammonium chloride and stearylamine oleate, stearylamine acetate or stearine acid, and the like. Specifically, nonionic surfactants may be, for example, glycerol fatty acid ester, propylene glycol fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, propylene fatty acid ester, glycerol fatty acid ester, monosaccharide fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene sorbitol tetraoleate, polyoxyethylene alkyl ether, polyoxypropylene alkyl ether, polyoxyethylene polyoxypropylene glycol, polyoxyethylene polyoxypropylene alkyl ether, organic esters of polyethylene glycol including, for example, polyethylene glycol fatty acid ester, polyoxyethylene glycol oil, and polyoxyethylene hydrogenated castor oil. In some embodiments, the nonionic surfactants are selected from a group consisting of sorbitol fatty acid ester and polyoxyethylene sorbitol fatty acid ester. Specifically, the amphoteric surfactant may be, for example, alkyl dimethylaminoacetic acid betaine, dimethylalkyl amine oxide, alkyl carboxymethyl hydroxyethyl imidazoleum betaine, lecithin, laurylaminopropionic acid, or alkyl diaminoethyl glycine, or the like.
[0057] In some embodiments, the surfactants are surfactants which are combinations of Tween and at least one of glycerol monooleate and span and have an HLB value. Specifically, the surfactants may be, for example, a combination of Tween 80 and glycerol monooleate, a combination of Tween 20 and glycerol monooleate, a combination of Tween 80 and span 80, a combination of Tween 20 and span 80, and the like.
[0058] In some embodiments, the lipophilic formulation is at least one selected from a group consisting of animal oils, vegetable oils and mineral oils. The animal oils may specifically be, for example, butter or lard, or the like. The vegetable oils may specifically be, for example, soybean oil, olive oil, corn oil, safflower oil, wheat germ oil or sunflower seed oil, or the like. The mineral oils may specifically be, for example, silicone oil or white oil, or the like.
[0059] In some embodiments, the core material further contains 0.1 wt%to 20 wt%of a flavor and / or an extract. In some embodiments, the core material further contains 3 wt%to 10 wt%of a flavor and / or an extract. The flavor includes oil soluble flavors or water soluble flavors. The flavor may be, for example, a fruit flavor, such as a lemon flavor, a mango flavor, or a sweet orange flavor, or the like. The extract generally refers to animal and plant extracts, such as musk, ambergris, and the like, preferably plant extracts, such as tea extracts, fructus monordicae extracts, and the like, and more preferably tobacco extracts, such as water extracts of tobacco, alcohol extracts of tobacco, pyrolyzates of tobacco, and the like.
[0060] In some embodiments, the gelled shell includes a gelling agent and a curing agent.
[0061] In some embodiments, the gelling agent is at least one selected from a group consisting of animal gel, vegetable gel, microbial gel, starch and modified starch. Specifically, the animal gel may be, for example, gelatin, fish gel, or chitosan, or the like. The vegetable gel may be, for example, carrageenan, sodium alginate, gellan gum, or tamarind gum, or the like.
[0062] In some embodiments, the curing agent is a polyol, and specifically, may be, for example, glycerol or sorbitol, and the like.
[0063] In some embodiments, the gelled shell further contains a reinforcing agent. In some embodiments, the reinforcing agent is a metal salt, and specifically, may be, for example, calcium chloride, potassium chloride, calcium carbonate, calcium phosphate, or monocalcium phosphate, or the like.
[0064] In some embodiments, the gelled shell further contains a sweetener. The sweetener may be, for example, mogroside, sucralose, or xylitol, or the like.
[0065] In some embodiments, the capsule may be used in medicine, food or cosmetics.
[0066] In some embodiments, the hydrophilic liquid formulation includes a hydrophilic liquid formulation that may generate aerosol, and the capsule can be used as an aerosol generating substrate. In some embodiments, the hydrophilic liquid formulation that can generate aerosol includes an aerosol generating substance releasable by heat. In some embodiments, the aerosol generating substance releasable by heat includes at least one of propylene glycol and glycerol. In some embodiments, propylene glycol and glycerol account for above 80 wt%of a total weight of the hydrophilic liquid formulation. In some embodiments, propylene glycol and glycerol account for above 85 wt%of a total weight of the hydrophilic liquid formulation. In some embodiments, propylene glycol and glycerol account for above 90 wt%of a total weight of the hydrophilic liquid formulation. In some embodiments, propylene glycol and glycerol account for above 95 wt%of a total weight of the hydrophilic liquid formulation. In some embodiments, propylene glycol and glycerol account for 100 wt%of a total weight of the hydrophilic liquid formulation.
[0067] In some embodiments, the core material further contains 0.1 wt%to 20 wt%of nicotine and / or a nicotine salt. Specifically, nicotine and / or the nicotine salt account for 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%, 7 wt%, 9 wt%, 10 wt%, 12 wt%, 14 wt%, or 16 wt%, or the like, of a weight of the core material.
[0068] In consideration of that the higher the content of propylene glycol in the core material, the higher the amount of released nicotine, and the higher the content of glycerol, an average particle size of aerosol is increased, the better the visual effect, and that both the amounts of smoke and released nicotine and the visual effect of aerosol need to be ensured, because a cigarette consumer requires both to enjoy pleasure in nicotine and to have a visual sense of smoke, in some embodiments, a weight ratio of propylene glycol to glycerol is 2: 8~8: 2, and specifically, may be, for example, 2: 8, 3: 7, 4: 6, 5: 5, 6: 4, 7: 3, or 8: 2, or the like.
[0069] In consideration of release effect of aerosol, in some embodiments, the capsule has a particle size of 0.5 mm to 8 mm. In some embodiments, the capsule has a particle size of 1 mm to 3 mm, and specifically, of, for example, 1 mm, 1.5 mm, 2 mm, 2.5 mm, or 3 mm, or the like.
[0070] In consideration of influence of a thickness of the gelled shell on strength of amount of released aerosol of the capsule, in some embodiments, the thickness of the gelled shell is 50 μm to 150 μm, and specifically, may be, for example, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, 120 μm, 130 μm, 140 μm, or 150 μm, or the like.
[0071] The embodiments of the present disclosure further provide an application of the capsule described above in an aerosol generating article. The capsule can provide a fragrance and can also be used as an aerosol generating substrate. When the aerosol generating article contains the capsule as an aerosol generating substrate, the capsule includes a core material and a gelled shell encapsulating the core material, and the core material includes at least one of propylene glycol and glycerol. Although current existing heat-not-burn cigarettes contains reconstituted tobacco with glycerol and / or propylene glycol which is an aerosol generating agent as an aerosol generating material, smoke is generated at a low heating temperature (<350 ℃) produces smoke to achieve smoking effect, and less harmful substances are released by the heat not burn tobacco products, but the actual heating temperature is also significantly lower than a heating temperature of traditional tobacco. As a result, in order to solve a problem of releasing sufficient smoke at a low temperature, it is necessary to increase the amounts of glycerol and propylene glycol. However, glycerol and propylene glycol themselves have good hygroscopicity and thus cause high hygroscopicity of the product, which brings great inconvenience to later processing and storage. Moreover, after opening a package, protection of a cigarette can not be ensured, resulting in uneven smoking of different cigarettes. In addition, a transfer of heat needs to be carried out during a period of time, such that amounts of smoke generated by a same cigarette in an early stage and a late stage are inconsistent. The aerosol generating article according to the embodiments of the present disclosure contains a core material prepared from propylene glycol and / or glycerol followed by encapsulating with a gelled shell, as an aerosol generating material of a cigarette, to overcome the above-mentioned problem of the existing heat not burning cigarettes, and to further reduce the heating temperature, and reduce the harmful substances. In some embodiments, the aerosol generating article has a temperature of release by heat greater than 150 ℃. In some embodiments, the temperature of release by heat is 200 ℃ to 300 ℃, and specifically, may be, for example, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃, 280 ℃, or 290 ℃, or the like. In some embodiments, the aerosol generating article includes the aforesaid capsule containing at least one of propylene glycol and glycerol.
[0072] The embodiments of the present disclosure further provide a method for preparing the capsule described above. The method includes the following steps:
[0073] mixing a material containing a hydrophilic liquid formulation, a lipophilic formulation and a structuring agent to prepare a core material;
[0074] preparing a material containing a gelling agent, a curing agent and water into a shell liquid; and
[0075] encapsulating the core material with the shell liquid to prepare the capsule.
[0076] In some embodiments, the lipophilic formulation is heated to 90 ℃ to 150 ℃, and the cellulose and / or cellulose derivatives and the low molecular weight lipid are added while stirring, dissolved and mixed evenly, cooled to 50 ℃ to 80 ℃. Then, the hydrophilic liquid formulation and the surfactant are added and stirred evenly, to prepare the core material.
[0077] In some embodiments, the core material is a paste, a colloid or a solid-liquid mixture at room temperature (25 ℃) , and placed at room temperature for 10h without stratification.
[0078] In some embodiments, the gelling agent is put into purified water, heated to a temperature of 60 ℃ to 90 ℃ while stirring, to form a uniform solution. Then, a curing agent is added, or a curing agent, a reinforcing agent, a sweetener and the like are added, and stirred evenly, to prepare the shell liquid.
[0079] Existing encapsulating methods can be adopted to encapsulate the core material with the shell liquid to prepare the capsule. In some embodiments, the method is a concentric tube dropping method. The core material and the shell liquid are dropped through a concentric dropper, and dried, to prepare the capsule. The core material is introduced through an inner layer pipeline. The shell liquid is introduced through an outer layer pipeline. Different thicknesses of the gelled shell can be achieved by adjusting an amount of added shell liquid.
[0080] The present disclosure will be further described below through specific examples.
[0081] Tests.
[0082] Core material state at room temperature.
[0083] The core material was added to a 100 ml test tube, placed at room temperature for 4h. And then, state of the core material was observed.
[0084] Stability.
[0085] The core material was added to a 100 ml test tube and placed at room temperature, to decide stability thereof according time. where, when the core material was placed at room temperature for more than 10h without stratification, stability thereof is decided to be better; when stratification occurred in the core material after the core material was placed for 6h to 10h, stability of the core material is decided to be good; and when stratification occurred in the core material after the core material was placed for less than 6h, stability of the core material is decided to be poor.
[0086] Particle size.
[0087] 30 capsules are detected for their diameters using a vernier caliper. An average diameter of the detected diameters is the particle size.
[0088] Yield rate.
[0089] A magnifying glass was used to observe a position relationship between the core material and the gelled shell. Ideally, the core material is in the center of the gelled shell, and the gelled shell completely encapsulates the core material and maintains a minimum thickness of 50 μm.If the core material deviates from the center of the gelled shell, and a thickness of the gelled shell around the core material is less than 10 μm, or the core material punctures the gelled shell, and the gelled shell does not completely encapsulate the core material, then the capsule is not a good product. A yield rate was calculated according to the gelled shell encapsulation of 100 capsules observed through a magnifying glass. Where, when above 90%of the capsules are good products, the yield rate is high; and when below 50%of the capsules are defective, the yield rate is low.
[0090] Thickness of the gelled shell.
[0091] The center of the capsule was divided into two parts. Then, shell thicknesses at four points of the capsule were measured, and an average value of the thicknesses on the left, right, top and bottom was calculated.
[0092] Volatilization Calculation.
[0093]
[0094] where, Ma is a weight of the capsule, Mb is a weight of the capsule after heating.
[0095] Nicotine content.
[0096] The capsule was filled into a paper tube. Then, the paper tube containing the capsule was put into a heating appliance for low temperature cigarettes, and sucked with a smoking machine, at a puff interval of 15 seconds, for 2 seconds per puff and 15 puffs. A filter was collected to test a content of nicotine.
[0097] Examples
[0098] Example 1
[0099] 40 weight parts of sunflower seed oil was heated to 100 ℃, and cellulose and / or cellulose derivatives and low molecular weight lipids of a formulation in Table 1 (a weight ratio of cellulose and / or cellulose derivatives, low molecular weight lipids and surfactants in a structuring agent at an amount of 13 weight parts in total) were added while stirring, dissolved and mixed evenly, cooled to 60 ℃. Then, add 24 weight parts of propylene glycol, 16 weight parts of glycerol, the surfactants of the formula in Table 1 below, 5 weight parts of mango flavor, 2 weight parts of a nicotine salt were added, and stirred well, to complete preparation of the core material. The core material was observed at room temperature and decided for stability, and the results are listed in Table 1 below. Table 1. Capsules prepared with different structuring agent formulations and test results thereof Continued from Table 1
[0100] It can be seen from the results in Table 1 above that, the structuring agent composed of a combination of cellulose and / or cellulose derivatives with the low molecular weight lipids and surfactants with a HLB value between 2 to 10, especially 4 to 7 and propylene glycol / glycerol as a hydrophilic formulation with high content form a core material in sunflower seed oil as a lipophilic formulation. The core material is a colloid at room temperature, has good stability, and can form a capsule with a high yield rate.
[0101] Further, based on formulations 11 and 12 in Table 1, when the structuring agent does not contain cellulose and / or cellulose derivatives or the low molecular weight lipids, the yield rate is low. In addition, according to a comparative experiment, if the structuring agent does not contain the surfactants, the yield rate is also low.
[0102] Example 2
[0103] 40 weight parts of sunflower seed oil was heated to 100 ℃, and raw materials were added according to formula 7 in Table 1, dissolved and mixed evenly, and cooled to 60 ℃. 40 weight parts in total of propylene glycol and glycerol (PG / VG) with a weight ratio as described in Table 2 below, 5 weight parts of mango flavor, and 2 weight parts of a nicotine salt were added, stirred evenly, to complete preparation of a core material.
[0104] 5 weight parts of carrageenan and 3 weight parts of gellan gum were put into 82 weight parts of purified water, and heated to a temperature of 60 ℃ to 90 ℃ while stirring, to form a uniform solution. Then, 10 weight parts of glycerol were added to the solution and stirred evenly, to prepare a shell liquid.
[0105] The core material (inner layer) and the shell liquid were dropped into a liquid coolant (medium chain triglycerides (MCT) ) through a concentric dropper at a temperature controlled at 10 ℃ to 25 ℃, to form a wet capsule. Then, the wet capsule was stored at -10 ℃ to 10 ℃ for 10 hours, and dried at 20 ℃ to 30 ℃ and 20%to 50%humidity, to prepare a capsule article with a particle size of 2 mm and a shell thickness of 70 μm.
[0106] The capsule article was filled into a paper tube. Then, the paper tube containing the capsule article was put into a heating appliance for low temperature cigarettes, to be heated and sucked, at a puff interval of 15 seconds, for 2 seconds per puff and 15 puffs. The heating appliance was adjusted to set different heating temperatures for suction. Volatilization of different propylene glycol (PG) / glycerol (VG) was tested at different temperatures and listed in Table 2 below. Table 2. Comparison of volatilization of different propylene glycol (PG) / glycerol (VG) at different temperatures
[0107] It can be seen from the results in Table 2 above that, the volatilization of aerosol increases with increase of the heating temperature, and the volatilization at temperatures ranging from 220 ℃ to 300 ℃ changes a little, which indicates that the volatilization is basically the same at a lower suction temperature of 220 ℃ to 260 ℃. With increase of a glycerol content, the aerosol volatilization will decrease, but at a suction temperature of 220 ℃ to 260 ℃ and the glycerol content below 60 wt%, the aerosol volatilization can be maintained above 30%. Further, nicotine contents in aerosol of aerosol generating articles (including 0.22 g capsules) made of capsules with different propylene glycol (PG) / glycerol (VG) ratios were tested at 240 ℃ after suction, and the results are listed in Table 3 below. Table 3. Nicotine contents in aerosol of different propylene glycol (PG) / glycerol (VG) at 240 ℃
[0108] It can be seen from the results in Table 3 above that, the higher the propylene glycol content, the higher the amount of released nicotine. When propylene glycol is above 40 wt%, a higher amount of released nicotine can be maintained. In addition, according to well-known technology, the higher the glycerol content, the better the visual effect of the aerosol. In consideration of the volatilization of aerosol, amount of released nicotine and the visual effect, when a ration of propylene glycol to glycerol is between 2: 8 to 8: 2, especially between 4: 6 to 6: 4, the effect is better.
[0109] Example 3
[0110] Capsule articles with particle sizes of 1 mm, 2 mm, 3 mm, 4 mm, 5 mm were respectively prepared using a method same as in Example 2 except the particle sizes. The volatilization of different propylene glycol (PG) / glycerol (VG) was tested at a heating temperature of 240 ℃, and the results are listed in Table 4 below. Table 4. Comparison of volatilization of different propylene glycol (PG) / glycerol (VG) and different particle sizes
[0111] It can be seen from the results in Table 4 above that, the volatilization of different ratios of propylene glycol to glycerol is close when the particle sizes of the capsule articles are ranging from 1 mm to 3 mm, and an amount of generated aerosol decreases with increase of particle size. If the particle size is too small, content of encapsulated propylene glycol and glycerol is low, and the amount of generated aerosol is also low.
[0112] Example 4
[0113] Capsule articles with a particle size of 2.5 mm, different shell thicknesses and different propylene glycol (PG) / glycerol (VG) as shown in Table 5 below were respectively prepared using a method same as in Example 2 except the particle sizes and shell thicknesses. The volatilization and strength of the capsules were tested at a heating temperature of 240 ℃ and decided, and the results are listed in Table 5 below. Table 5. Comparison of volatilization and capsule strength of different propylene glycol (PG) / glycerol (VG) and different shell thicknesses
[0114] It can be seen from the results in Table 5 above that, although the capsule articles with a shell thickness less than 50 μm have a good amount of released aerosol, these capsule articles are fragile and may crack in a process of loading into a paper tube, and is thus not easy to preserve. The capsule articles with a shell thickness greater than 150 μm are not easy to break during the heating process and have a small amount of released aerosol.
[0115] Although the present disclosure is disclosed as above, the present disclosure is not limited hereto. Various changes and modifications can be made by those skilled in the art without departing from the spirit and scope of the present disclosure. Therefore, the scope of protection of the present disclosure shall be subject to the scope limited by the claims.
Claims
1.A capsule, characterized by comprising a core material and a gelled shell encapsulating the core material, wherein, the core material comprises a hydrophilic liquid formulation, a lipophilic formulation and a structuring agent, the structuring agent comprises cellulose and / or cellulose derivatives, and further, a low molecular weight lipid and a surfactant, and the core material is a paste, a colloid or a solid-liquid mixture.2.The capsule according to claim 1, characterized in that the surfactant has an HLB value of 2 to 10.3.The capsule according to claim 2, characterized in that the surfactant has an HLB value of 4 to 7.4.The capsule according to claim 1, characterized in that the hydrophilic liquid formulation accounts for 5 wt%to 60 wt%of a weight of the core material.5.The capsule according to claim 4, characterized in that the hydrophilic liquid formulation accounts for 15 wt%to 50 wt%of a weight of the core material.6.The capsule according to claim 1, characterized in that the lipophilic formulation accounts for 20 wt%to 80 wt%of a weight of the core material, and the structuring agent accounts for 5 wt%to 20 wt%of a weight of the core material.7.The capsule according to claim 1, characterized in that the cellulose and / or cellulose derivatives and the low molecular weight lipid together account for 70 wt%to 95 wt%of a weight of the structuring agent, and the surfactant accounts for 30 wt%to 5 wt%of the weight of the structuring agent.8.The capsule according to claim 1, characterized in that a weight ratio of the cellulose and / or cellulose derivatives to the low molecular weight lipid is 20: 1~1: 1.9.The capsule according to claim 1, characterized in that the cellulose and / or cellulose derivatives have a viscosity of 1 mPa·s to 300 mPa·s, and account for 1 wt%to 10 wt%of a weight of the core material.10.The capsule according to claim 1, characterized in that the cellulose and / or cellulose derivatives are at least one of cellulose acetate, nitrocellulose and ethylcellulose.11.The capsule according to claim 1, characterized in that the low molecular weight lipid is at least one selected from a group consisting of animal wax, plant wax, mineral wax, synthetic wax, lecithin and derivatives thereof, plant sterol and esters thereof, fatty acid and esters thereof, triglyceride, and fatty alcohol.12.The capsule according to claim 1, characterized in that the surfactant is at least one selected from a group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and amphoteric surfactants.13.The capsule according to claim 1, characterized in that the lipophilic formulation is at least one selected from a group consisting of animal oils, vegetable oils and mineral oils.14.The capsule according to claim 1, characterized in that the gelled shell contains a gelling agent and a curing agent.15.The capsule according to claim 14, characterized in that the gelling agent is at least one selected from a group consisting of animal gel, vegetable gel, microbial gel, starch and modified starch, and the curing agent is a polyol.16.The capsule according to claim 1, characterized in that the hydrophilic liquid formulation contains an aerosol generating substance releasable by heat.17.The capsule according to claim 16, characterized in that the aerosol generating substance releasable by heat comprises at least one of propylene glycol and glycerol.18.The capsule according to claim 17, characterized in that propylene glycol and glycerol account for 80 wt%to 100 wt%of a total weight of the hydrophilic liquid formulation.19.The capsule according to claim 16, characterized in that the core material further contains 0.1 wt%to 20 wt%of nicotine and / or a nicotine salt.20.The capsule according to claim 16, characterized in that the core material further contains 0.1 wt%to 20 wt%of a flavor and / or an extract.21.The capsule according to claim 17, characterized in that a weight ratio of propylene glycol to glycerol is 2: 8~8: 2.22.The capsule according to claim 1, characterized in that the capsule has a particle size of 0.5 mm to 8 mm.23.The capsule according to claim 22, characterized in that the capsule has a particle size of 1 mm to 3 mm.24.The capsule according to claim 1, characterized in that the gelled shell has a thickness of 50 μm to 150 μm.25.An application of the capsule according to any one of claims 1 to 24 in an aerosol generating article.26.A method for preparing the capsule according to any one of claims 1 to 24, characterized by comprising the following steps:mixing a material containing the hydrophilic liquid formulation, the lipophilic formulation and the structuring agent to prepare the core material;preparing a material containing a gelling agent, a curing agent and water into the shell liquid; andencapsulating the core material with the shell liquid to prepare the capsule.27.The method for preparing the capsule according to claim 26, characterized in that the core material and the shell liquid are dropped through a concentric dropper and dried to prepare the capsule.28.An aerosol generating article, characterized by comprising an aerosol generating substrate, and the aerosol generating substrate comprises the capsule according to any one of claims 16 to 21.29.The aerosol generating article according to claim 28, characterized by having a temperature of release by heat greater than 150 ℃.30.The aerosol generating article according to claim 29, characterized by having a temperature of release by heat of 200 ℃ to 300 ℃.
Citation Information
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