CN113662236B - Microcapsule, preparation method thereof and application of microcapsule to heating of non-combustible cigarettes - Google Patents
Microcapsule, preparation method thereof and application of microcapsule to heating of non-combustible cigarettes Download PDFInfo
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- CN113662236B CN113662236B CN202111030589.6A CN202111030589A CN113662236B CN 113662236 B CN113662236 B CN 113662236B CN 202111030589 A CN202111030589 A CN 202111030589A CN 113662236 B CN113662236 B CN 113662236B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
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Abstract
The invention discloses a microcapsule, which comprises a wall material and a core material, wherein the wall material is a mixture of gelatin and Arabic gum, and the core material is menthol. The invention also discloses a preparation method of the microcapsule and application of the microcapsule to heating of non-combustible cigarettes.
Description
Technical Field
The invention belongs to the technical field of tobacco, and particularly relates to a microcapsule, a preparation method thereof and application of the microcapsule in heating non-combustible cigarettes.
Background
The heating non-combustion cigarette is a novel tobacco category which generates smokable aerosol by heating tobacco substances through an electronic heating device, and the potential health risk of the heating non-combustion cigarette is greatly reduced through the product attribute of heating rather than combustion on the basis of providing smoking feeling of a burning type cigarette of a consumer, so that a new consumer choice is provided for the consumer.
In order to improve the smoking quality of the cigarette which is not combusted by heating, develop a controlled release technology to solve the release control of nicotine and aroma, develop an innovative technology of a low-temperature adsorption embedding slow release technology, form a key technical system for improving the smoking quality and highlighting the style characteristics, enrich aroma, improve taste, highlight the style and improve quality, provide technical support for the development of the cigarette which is not combusted by heating, and have important practical value and guiding significance for the construction and innovation of a novel cigarette product flavoring system. The microcapsule technology is to wrap a functional core material into a micro particle form by utilizing natural or synthetic wall material substances, and can delay the volatilization and deterioration process of the aroma component after the aroma component is embedded by the microcapsule technology, thereby realizing the purposes of slow release and stability.
Patent CN108618190A discloses that applying tobacco essence microcapsule with beta-cyclodextrin as wall material in tobacco tar of electronic cigarette improves the problem of smoking fragrance and nicotine weakening of electronic cigarette, prolongs the storage time of tobacco juice of electronic cigarette, and improves the sensory quality of smoking. In patent CN112522031A, a core material coated with a composite wall material of cyclodextrin and carboxymethylcellulose salt is a water-soluble flavor, and the prepared microcapsule is used for gum base type chewing tobacco, wherein the slow release property and storage stability of the flavor are obviously improved.
Disclosure of Invention
The patent discloses a microcapsule, the wall material of the microcapsule is a mixture of gelatin and Arabic gum, and the core material is menthol. When the microcapsule is used for heating non-combustible cigarettes, the slow release property and the storage stability of the microcapsule are obviously improved, roasted nuts, bread and/or cocoa flavor are contained in smoke, and the comfort of the smoke fragrance is improved.
The technical scheme of the invention is as follows:
a microcapsule comprises a wall material and a core material, wherein the wall material is a mixture of gelatin and Arabic gum, and the core material is menthol.
Preferably, the mass ratio of the core material to the wall material is 1: 4-1: 8, and the mass ratio of the gelatin to the Arabic gum in the wall material is 1: 10-10: 1.
The second aspect of the invention discloses a preparation method of the microcapsule, which comprises the following steps:
(1) dissolving menthol in water, adding an emulsifier, and uniformly mixing to obtain a core material solution;
(2) dissolving a mixture of gelatin and Arabic gum in water to obtain a wall material solution;
(3) uniformly mixing the wall material solution and the core material solution according to a certain proportion to obtain a mixed solution;
(4) adding water into the mixed solution for dilution, dropwise adding acid liquor to adjust the pH value, maintaining the temperature and stirring to ensure that the complex coacervate is completely reacted in a form;
(5) cooling, adding alkali liquor, adjusting pH to neutral, standing for settling;
(6) and freeze-drying the obtained solid product to remove residual liquid to obtain the microcapsule.
Preferably, the emulsifier of step (1) is tween-80, which is used in an amount of 2 to 6wt% of the amount of menthol.
Preferably, the concentration of the wall material solution in the step (2) is 2wt% -8wt%, and the mass ratio of the gelatin to the Arabic gum is 1: 10-10: 1.
Preferably, the mass ratio of the core material to the wall material in the step (3) is 1: 4-1: 8.
Preferably, the pH value of the step (4) is 3-6, the stirring speed is 200-800rpm, the temperature is 30-60 ℃, and the reaction time is 1-3 hours.
Preferably, the acid solution in step (4) is an acetic acid solution, and the alkali solution in step (5) is a sodium hydroxide solution.
In a third aspect of the invention, the application of the microcapsule in heating non-combustion cigarettes is disclosed.
Preferably, the heat not burn cigarette has the use of roasted nuts, bread and/or savoury.
The invention has the beneficial effects that:
1. the microcapsule uses a mixture of gelatin and Arabic gum as a wall material and menthol as a core material. When the microcapsule is used for heating non-burning cigarettes, smoke has roasted nuts, bread and/or savory flavor, so that the comfort of the smoke is improved; through the analysis of the flue gas, the flue gas contains more valeraldehyde. Menthol is directly used for heating non-combustible cigarettes without roasting nuts, bread and/or flavors; through the analysis of the smoke, the smoke does not contain valeraldehyde. This effect is an unexpected effect obtained by the present invention.
2. According to the preparation method, by optimizing the raw material proportion and the reaction conditions, the obtained microcapsules are spherical, the particle size range is 1.7-5.0 mu m, the dispersion is uniform, the number of the microcapsules is large, and the yield can reach 63.6%.
Drawings
Fig. 1 is an SEM image of the composite wall material of the comparative example.
Fig. 2 is an SEM image of the menthol microcapsule obtained in example 1.
FIG. 3 is an infrared spectrum of a blank complex coacervate wall material, menthol, and menthol microcapsules; wherein (A) is blank complex coacervate wall material, (B) is menthol, and (C) is microcapsule menthol.
Figure 4 is a TGA plot of blank complex coacervate wall material, core material menthol and menthol microcapsules.
Fig. 5 shows the particle size and distribution of the menthol microcapsules obtained in example 1.
Detailed Description
In order to further understand and appreciate the structural features and effects achieved by the present invention, the present invention will be described in detail with reference to the following embodiments and the accompanying drawings.
Example 1: the preparation of the microcapsule comprises the following steps:
(1) dissolving 10g of menthol in water, adding 0.42g of emulsifier Tween-80, and uniformly mixing to obtain a core material solution;
(2) 60g of a mixture of gelatin and Arabic gum with the mass ratio of 1: 1 is dissolved in water to obtain a wall material solution;
(3) uniformly mixing the wall material solution obtained in the step (2) with the core material solution obtained in the step (1) to obtain a mixed solution;
(4) adding water into the mixed solution to dilute the mixed solution so that the wall material concentration is 6wt%, dropwise adding an acetic acid solution to adjust the pH value to 4, and reacting for 2 hours at 45 ℃ and at a stirring speed of 600 rpm;
(5) cooling to room temperature, adding sodium hydroxide solution to adjust the pH value to be neutral, and standing for sedimentation;
(6) and (3) freeze-drying the obtained solid product at-30 ℃ to remove residual liquid to obtain the microcapsule. The appearance of the obtained microcapsules was yellow loose particles with a yield of 63.6%.
Comparative example 1: same as example 1, but without menthol as core.
FIG. 1 is an SEM image of a comparative composite wall material; fig. 2 is an SEM image of the menthol microcapsule obtained in example 1. As can be seen from fig. 1 and 2, the blank complex coacervate wall material of the comparative example and the menthol microcapsule of example 1 have different microscopic shapes, and the blank complex coacervate wall material has an irregular continuous lamellar structure, indicating that it is not formed into a wrapped state. The menthol microcapsules of the embodiment have a smooth globular microstructure, a part of fine spheres are adhered to the surfaces of a plurality of larger spheres, and the particle size of the spheres is about 2-4 mu m, which shows that the menthol is wrapped by the wall material of the gelatin-Arabic gum to form the microcapsules.
Fig. 3 is an infrared spectrum of a blank complex coacervate wall material, core material menthol, and menthol microcapsules of example of comparative example. As can be seen from fig. 3, the infrared spectra of the blank complex coacervate wall material, the core material menthol and the menthol microcapsule have obvious differences in the pattern and the characteristic peak position; blank complex coacervation wall material at 3259, 2953, 1614em -1 The characteristic infrared absorption peaks of the menthol microcapsule respectively move to 3280, 2924 and 1605cm -1 The peak intensity also increased, indicating that a new phase was formed; core material menthol is 2916, 2839, 1460 and 1439cm -1 The characteristic infrared absorption peak of the compound is obviously weakened in the menthol microcapsule and is overlapped with the characteristic peak of the wall material, which is caused by the fact that the wall material is blocked in vibration after the menthol is embedded; micro-glueAnd a new characteristic peak is not found in the capsule map, which indicates that the complex coacervation reaction does not involve the generation of other chemical bonds, and further indicates that the complex coacervation reaction is only the electrostatic interaction between the wall material and the core material and does not generate other chemical reactions. The above changes fully show that the wall material of the invention can effectively embed the core material menthol to form a new microcapsule structure.
Fig. 4 is a TGA curve of blank complex coacervate wall material, core material menthol, and menthol microcapsules obtained in the examples of the comparative examples. As can be seen from FIG. 4, the thermal weight loss process of menthol as core material is mainly between 25 deg.C and 187 deg.C, and the mass loss is close to 100%, and is mainly the weight loss caused by the volatilization of menthol, and the initial turning temperature is about 175 deg.C, the maximum volatilization temperature is 171 deg.C, and the corresponding maximum weight loss rate T is lmax = 1.1%/deg.c, and is substantially unchanged after 187 deg.c. The thermal weight loss process of the blank complex coacervation wall material is divided into several stages: at the temperature of 25-175 ℃, the weight loss is mainly caused by residual free moisture in the sample, low-boiling-point volatile substances attached to the surface of the sample and the like, the mass loss is 6.3 percent, and a maximum weight loss rate is realized at the temperature of 70 ℃; in the temperature range of 175-380 ℃, the wall material is decomposed and gasified due to the damage of electrostatic acting force between the gelatin and the Arabic gum, the mass loss is 60.5 percent, and the maximum weight loss rate is realized at 328 ℃; at 380-600 ℃, the mass loss of a small amount of residual undecomposed wall materials is 11.4 percent after the further decomposition, and the decomposition is actually close to the end sound and is carried out smoothly, so that no obvious maximum or maximum weight loss rate occurs. The thermal weight loss process of the menthol microcapsule comprises the following stages: the weight loss is mainly caused by the residual free moisture in the sample and low-boiling-point volatile substances attached to the surface of the sample between 25 ℃ and 112 ℃, the mass loss is 5.5 percent, and a maximum weight loss rate exists at 50 ℃; in the temperature range of 112-380 ℃, a maximum weight loss rate exists at 260 ℃ and a maximum weight loss rate exists at 328 ℃, which respectively correspond to the release of a part of core materials in the product along with the rise of temperature and the destruction, dissociation and gasification of the wall material structure of the gelatin and Arabic gum compound, wherein the mass loss is 60.4%; at 380-600 deg.c, the residual un-decomposed wall material is further decomposedMeanwhile, a less obvious maximum weight loss rate exists at about 400 ℃, which corresponds to the release of the residual core material at a higher temperature, and the mass loss of the core material is 19.8%. The comparison shows that the important temperature parameter difference in the second stage indicates that the stability of the microcapsule menthol and the wall material or the core material in the heating process is obviously different.
Fig. 5 shows the particle size and distribution of the menthol microcapsules obtained in example 1. As can be seen from FIG. 5, the particle size range of the menthol microcapsules obtained in the examples is mostly between 1.7 μm and 5.0 μm, which belongs to micron-sized microcapsules, and the number average particle size statistic value is 2.62 μm; the particle size of the microcapsule is close to normal distribution, the particle size range is about 3.3 mu m, and the particle size distribution is narrow.
Carrying out quantitative research by adopting a mass difference method to obtain the release data of the core material; the results of the slow release property measurement of the menthol microcapsules are shown in table 1 below.
TABLE 1 sustained Release Properties of menthol microcapsules
As can be seen from table 1, the menthol microcapsules remained yellow solid powder after standing for 90 days, and the appearance was almost unchanged. After 90 days, the mass of the menthol microcapsules slowly dropped from the initial 1.000g to 0.947g with prolonged storage time, and the retention of menthol was 56.4%, indicating that the encapsulated menthol was in a relatively slow release process. In sharp contrast thereto: under the same conditions, the menthol reference substance is completely volatilized after 20 days. Therefore, the menthol microcapsule of the present example has good storage stability and sustained release property.
The prepared microcapsules and tobacco sheets are fully and uniformly mixed according to the mass ratio of 9: 91 and added into a cigarette which is not burnt by heating for manual smoking, and sensory quality evaluation is carried out according to a standard method GB 5606.4-2005. Meanwhile, PY-GCMS thermal cracking is adopted to carry out the characterization of the content of smoke components in the temperature range (200-400 ℃) for heating the non-combustible cigarette; GCMS is utilized to research the release conditions of the mouth-to-mouth smoking components of the microcapsule-loaded tobacco product and a control sample, the component composition difference is analyzed, the core material release data is obtained, and finally, expert artificial sensory quality evaluation is carried out to evaluate the application effect of the microcapsule-loaded tobacco product and the control sample. The reference sample is prepared by fully and uniformly mixing menthol and tobacco sheets according to the mass ratio of 1: 99 and is used for heating the non-burning cigarettes; the menthol content in both the test sample and the reference sample remained the same.
The pumping results were: the tobacco rod containing menthol microcapsules which is not combusted by heating has roasted nuts, bread and/or a savory flavor; whereas the reference sample had only the taste of menthol.
The results of the expert's smoke panel are shown in table 2 below:
TABLE 2 result of comparative smoking evaluation of tobacco smoke which is not combusted by heating and its reference sample
As can be seen from Table 2, after the microcapsule menthol is added into the non-combustible cigarette, the fragrance, harmony, miscellaneous odor, irritation and aftertaste of the cigarette smoke are all improved, the effect on the fragrance and the aftertaste of the cigarette smoke is obvious, the specific expression is that the fragrance is longer, and the fragrance is better retained along with the increase of the number of suction openings.
The analysis of the smoke of the cigarette subjected to non-combustion by heating through Y-GCMS thermal cracking is shown in the following table 3:
TABLE 3 thermal cracking products of microcapsule-loaded, heated, non-combustible tobacco rods and reference samples
The heated nonflammable tobacco material added with menthol microcapsules was thermally cracked at 50-300 ℃ for a total of 28 substances as shown in Table 3. The main substances (content greater than 1.5%) are carbon dioxide, methylglyoxal, valeraldehyde, glycerol, menthol, nicotine, etc. The reference sample of the cigarette without burning by heating added with menthol powder was subjected to thermal cracking at 50-300 deg.C to detect 37 substances, as shown in Table 3, the main substances (content greater than 1.5%) were carbon dioxide, methylglyoxal, glycerol, menthol, nicotine, palmitic acid, etc. As can be seen from table 3, compared with the reference sample, the types of products cracked from the tobacco branches which are not burned by heating and added with the menthol microcapsules are relatively less, but the percentage contents of characteristic aroma substances menthol and nicotine are improved, wherein pentanal only exists in the tobacco cracked gas added with the menthol microcapsules, and the substance has roasted nuts, bread and/or cocoa flavor and also has a promoting effect on the aroma of the smoke; this effect was unexpected in this patent. In addition, the tobacco pyrolysis gas added with the menthol microcapsules is also caused by the loss of some non-fragrant components such as siloxane and phthalate series chromatographic column fixing liquid.
The above description is only a specific embodiment of the present invention, but not a limitation of the present invention, and those skilled in the art can modify and modify the basic idea of the present invention without departing from the basic idea of the present invention.
Claims (6)
1. Use of a microcapsule for heating a non-combustible cigarette to impart a roasted nut, bread and/or flavourable flavour to the heated non-combustible cigarette, wherein the microcapsule comprises a wall material and a core material, the wall material being a mixture of gelatin and acacia gum, the core material being menthol; the preparation method of the microcapsule comprises the following steps:
(1) dissolving menthol in water, adding an emulsifier, and uniformly mixing to obtain a core material solution;
(2) dissolving a mixture of gelatin and Arabic gum in water to obtain a wall material solution;
(3) uniformly mixing the wall material solution and the core material solution according to a certain proportion to obtain a mixed solution;
(4) adding water into the mixed solution for dilution, dropwise adding acid liquor to adjust the pH value, maintaining the temperature and stirring to ensure that the complex coacervate completely reacts;
(5) cooling, adding alkali liquor, adjusting pH to neutral, standing and settling;
(6) freeze-drying the obtained solid product to remove residual liquid to obtain the microcapsule;
the microcapsules are used for heating non-combustible cigarettes, and the smoke contains valeraldehyde, so that the heating non-combustible cigarettes can bake nuts, bread and/or cocoa flavor.
2. Use according to claim 1, characterized in that the emulsifier of step (1) is tween-80, which is used in an amount of 2-6wt% of the amount of menthol.
3. The use according to claim 1, wherein the concentration of the wall material solution in the step (2) is 2wt% -8wt%, and the mass ratio of the gelatin to the Arabic gum is 1: 10-10: 1.
4. The use according to claim 1, wherein the mass ratio of the core material to the wall material in step (3) is 1: 4 to 1: 8.
5. Use according to claim 1, wherein the pH value of step (4) is 3-6, the stirring rate is 200-800rpm, the temperature is 30-60 ℃, and the reaction time is 1-3 hours.
6. The use according to claim 1, wherein the acid solution of step (4) is an acetic acid solution and the alkali solution of step (5) is a sodium hydroxide solution.
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