CN113729269A - Smoke agent for moisture absorption prevention cigarettes as well as preparation method and application thereof - Google Patents
Smoke agent for moisture absorption prevention cigarettes as well as preparation method and application thereof Download PDFInfo
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- CN113729269A CN113729269A CN202010474978.7A CN202010474978A CN113729269A CN 113729269 A CN113729269 A CN 113729269A CN 202010474978 A CN202010474978 A CN 202010474978A CN 113729269 A CN113729269 A CN 113729269A
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- moisture absorption
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 87
- 239000000779 smoke Substances 0.000 title claims abstract description 71
- 238000010521 absorption reaction Methods 0.000 title claims description 35
- 230000002265 prevention Effects 0.000 title claims description 14
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 85
- 239000000463 material Substances 0.000 claims abstract description 38
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 30
- 230000000391 smoking effect Effects 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 239000003094 microcapsule Substances 0.000 claims abstract description 19
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- 239000000839 emulsion Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 238000004945 emulsification Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 8
- 229920002492 poly(sulfone) Polymers 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000004695 Polyether sulfone Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 229920006393 polyether sulfone Polymers 0.000 claims description 4
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- GTTSNKDQDACYLV-UHFFFAOYSA-N Trihydroxybutane Chemical compound CCCC(O)(O)O GTTSNKDQDACYLV-UHFFFAOYSA-N 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims description 2
- 239000011147 inorganic material Substances 0.000 claims description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 2
- MDDPTCUZZASZIQ-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]alumane Chemical compound [Al+3].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] MDDPTCUZZASZIQ-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 29
- 239000011257 shell material Substances 0.000 description 14
- 235000011187 glycerol Nutrition 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 241000208125 Nicotiana Species 0.000 description 5
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 5
- 239000002775 capsule Substances 0.000 description 5
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000001804 emulsifying effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229940083575 sodium dodecyl sulfate Drugs 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 239000012454 non-polar solvent Substances 0.000 description 3
- 239000007762 w/o emulsion Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004505 smoke cartridge Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D1/00—Cigars; Cigarettes
- A24D1/20—Cigarettes specially adapted for simulated smoking devices
Abstract
The invention discloses a smoking agent for moisture-absorption-preventing cigarettes as well as a preparation method and application thereof. The preparation process comprises the following steps: dissolving a smoke agent for cigarettes, inorganic acid and a surfactant in water to obtain a solution A, and dissolving the surfactant in a nonpolar organic solvent to obtain a solution B; adding the solution A into the solution B for emulsification under the stirring condition to obtain emulsion; the microcapsule shell precursor material is dripped into the emulsion, the stirring reaction is carried out, the obtained product is subjected to surface hydrophobic treatment, the preparation method is simple, the cost is low, the condition is mild, the large-scale production is facilitated, and the prepared smoke agent for the moisture-absorption-preventing cigarette has good moisture-absorption-preventing performance on the premise of not influencing normal smoking when the smoke agent is added into a cigarette which is not heated and combusted.
Description
Technical Field
The invention relates to a smoking material, in particular to a smoking agent with a moisture absorption prevention function for cigarettes, and also relates to a preparation method and application thereof, belonging to the technical field of novel smoking materials.
Background
Due to the continuous push of global smoking control, the pressure of traditional cigarettes is increasing, and new tobacco products are gradually becoming a research focus, wherein the cigarette is particularly concerned when not burning. The cigarette is heated and does not burn, the tobacco components are taken as main raw materials to prepare the cigarette bullet, and then the cigarette bullet is heated (300-. In order to make the cigarette produce enough smoke when being smoked, 10-30% of smoke agent is added in the manufacturing process of the cigarette cartridge, and the main component of the smoke agent is glycerol (glycerin). Although glycerol has a good smoking effect and does not have a negative effect on the taste of cigarettes, it has a strong hygroscopicity, thus adversely affecting the production and storage of cigarette cartridges of non-combustible cigarettes. In order to solve the practical problem faced in the production and application of the heating non-combustion cigarette, Chinese patent (CN210043197U) proposes to adjust the moisture content of the heating non-combustion cigarette through a composite filter stick containing a tobacco material, Chinese patent (CN110881684A) proposes to load a smoking material with a functional material, and Chinese patent (CN108451054A) reports to reduce the hygroscopicity of a smoke cartridge core material by coating a hydrophobic material on a tobacco sheet. Although the proposal proposed by the Chinese patent (CN210043197U) can reduce the moisture content of the smoke, the problem of moisture absorption of the smoke cartridge cannot be solved, the problem of adsorption quantity of the smoke agent carried by the functional material proposed by the Chinese patent (CN110881684A) also exists, and certain disadvantages exist in the cigarette production process when the hydrophobic material is coated.
Disclosure of Invention
In order to solve the problems of strong cigarette hygroscopicity, unfavorable storage and the like caused by using a large amount of smoke agents in a cigarette cartridge for heating a non-combustible cigarette, the first object of the invention is to provide the smoke agent for the moisture-absorption-preventing cigarette, which utilizes an inorganic shell material capsule subjected to hydrophobic treatment to encapsulate the smoke agent, so that the direct contact between the smoke agent and a solvent and air can be reduced, the normal smoke effect is not influenced, and the problem of high moisture absorption caused by the smoke agent in the cigarette which is not combusted during heating is solved.
The second purpose of the invention is to provide a method for preparing the smoke agent for the moisture absorption preventing cigarette under mild conditions, simple process and low cost.
The third purpose of the invention is to provide the application of the smoke agent for the moisture-absorption-preventing cigarette in heating the non-burning cigarette, and the smoke agent for the moisture-absorption-preventing cigarette can effectively solve the technical problem that the existing heating non-burning cigarette is strong in moisture absorption and difficult to store due to the adoption of the smoke agent.
In order to achieve the technical purpose, the invention provides a smoking agent for preventing moisture absorption, which is formed by encapsulating the smoking agent for cigarettes in a hydrophobic microcapsule shell.
The smoke agent for cigarette in the prior art is mainly a micromolecular polyalcohol compound, has strong hygroscopicity and is volatile in the storage process. The smoke agent for preventing the moisture absorption of the cigarettes provided by the invention not only can well prevent the smoke agent from absorbing the moisture, but also can prevent the volatilization loss of the smoke agent in the storage process, and meanwhile, the smoke agent is encapsulated by adopting the hydrophobic microcapsule shell without influencing the normal smoking effect of the smoke agent, so that the technical problem that the smoke agent for the cigarettes is strong in moisture absorption and difficult to store is well solved
As a preferable scheme, the hydrophobic microcapsule shell is composed of an inorganic oxide shell and a hydrophobic layer modified on the surface of the inorganic oxide shell.
Preferably, the inorganic oxide shell is made of at least one inorganic material selected from titanium dioxide, silicon dioxide and aluminum trioxide. The materials have good stability and safety, meet the addition requirements of cigarettes, and have low cost, no pollution and easy obtainment.
Preferably, the hydrophobic layer is made of at least one hydrophobic material selected from polysulfone, polyarylsulfone and polyethersulfone. The high polymer materials have good hydrophobicity and good thermal stability, are modified on the surface of an inorganic oxide material, and further improve the hydrophobicity of the microcapsule shell.
Preferably, the smoking agent for the cigarette is at least one of glycerol, propylene glycol, ethylene glycol, butanediol and butanetriol. The preferable smoking agent for cigarette is at least one of glycerol, propylene glycol and butanediol.
As a preferable scheme, the mass ratio of the smoke agent for the cigarette to the hydrophobic microcapsule shell is 9: 1-1: 1. The preferable mass ratio is 9:1 to 7: 1.
The invention also provides a preparation method of the smoking agent for the moisture-absorption-preventing cigarette, which comprises the following steps:
1) dissolving a smoke agent for cigarettes, inorganic acid and a surfactant in water to obtain a solution A, and dissolving the surfactant in a nonpolar organic solvent to obtain a solution B;
2) adding the solution A into the solution B for emulsification under the stirring condition to obtain emulsion;
3) dropwise adding a microcapsule shell precursor material into the emulsion, stirring for reaction, and carrying out solid-liquid separation, washing and drying on an obtained reaction product to obtain a solid particle material;
4) adding the solid particle material into a solution containing the hydrophobic material, stirring for reaction, filtering, separating and drying to obtain the hydrophobic material.
As a preferable scheme, the volume ratio of the smoking agent for the cigarette to water and the nonpolar organic solvent is 1-10: 1: 10-50. In the preferred ratio range, capsule formation is facilitated, and if the ratio is not controlled well, it is liable to cause inefficient coating of the fuming agent or it is difficult to form a microcapsule structure.
In a preferred embodiment, the nonpolar organic solvent is n-hexane and/or cyclohexane. These non-polar solvents are insoluble in water and facilitate the subsequent formation of an emulsion.
In a preferred embodiment, the inorganic acid is at least one of hydrochloric acid, sulfuric acid, and nitric acid. The inorganic acid mainly plays a catalytic role, and catalyzes the precursor to be hydrolyzed to generate silicon dioxide, titanium dioxide and aluminum oxide.
Preferably, the concentration of the inorganic acid in the solution A is 0.1-6.5M.
As a preferable scheme, the surfactant is at least one of sodium dodecyl sulfonate, sodium dodecyl sulfate, span 80, Tween 80 and hexadecyl trimethyl ammonium bromide. The surfactant is mainly used for promoting the smoke agent to form micro liquid drops or micro emulsion liquid drops in a two-phase system, and then inorganic oxide generated by precursor hydrolysis is deposited on the surface of the liquid drops to coat the liquid drops to obtain (micro) capsules.
As a preferable scheme, the concentration of the surfactant in the solution A is 0.01-0.1 g/mL; the concentration of the surfactant in the solution B is 0.005-0.05 g/mL.
As a preferable mode, the microcapsule shell precursor material contains at least one of n-butyl titanate, titanium tetrachloride, tetramethoxysilane, tetraethoxysilane, aluminum tert-butoxide, and aluminum sec-butoxide. The microcapsule shell precursor material may be added in the form of a stock solution, or may be added by dissolving it in a nonpolar organic solvent.
As a preferable scheme, the microcapsule shell precursor material is dripped into the emulsion at the temperature of 25-35 ℃, stirred and reacted, and after dripping is finished, the stirring and reaction are continued for 18-30 hours.
As a preferable scheme, the concentration of the hydrophobic material in the solution containing the hydrophobic material is 0.1-0.5 g/mL. The solution containing the hydrophobic material is obtained by dissolving at least one hydrophobic material selected from polysulfone, polyarylsulfone and polyethersulfone in dichloromethane and/or DMF.
Preferably, in the step 4), the stirring reaction is carried out for 0.5 to 3 hours.
The specific preparation method of the smoke agent for preventing the moisture absorption cigarette provided by the invention comprises the following steps: dissolving a smoking agent for cigarettes in water containing a certain amount of inorganic acid and surfactant at 25-70 ℃, and cooling to 15-30 ℃ to obtain a solution A; dissolving a certain amount of surfactant in a non-polar solvent to obtain a solution B; then adding the solution A into the solution B, and stirring and emulsifying at a certain rotating speed at room temperature to obtain stable emulsion; dropwise adding a microcapsule shell precursor material into the emulsion at 25-35 ℃; and after the addition, continuously stirring and reacting for 24 hours, filtering, washing solid particles by using a corresponding nonpolar solvent and ethanol, drying, adding the obtained solid particles into dichloromethane and/or dimethylformamide dissolved with hydrophobic high polymer materials, stirring for 0.5-3 hours, filtering and separating, and finally drying to obtain the smoke agent for the moisture-absorption-preventing cigarettes.
The invention also provides application of the smoking agent for the moisture-absorption-preventing cigarette, which is applied to heating non-combustion cigarettes.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1) the capsule of the smoke agent for the moisture-proof cigarette is added into a main material (thin sheet or cut tobacco) of a cigarette bullet which is heated and does not burn the cigarette, and is exposed in a 60% humidity environment, the water absorption amount of the smoke agent for the moisture-proof cigarette is not more than 3% of the smoke agent amount for the moisture-proof cigarette, and the capsule of the smoke agent for the moisture-proof cigarette can prolong the storage time compared with the common smoke agent for the cigarette, can normally smoke at high temperature and does not influence the atomization effect of the smoke agent.
2) The smoke agent for the moisture-absorption-preventing cigarette has the advantages of simple preparation process, easily obtained raw materials, mild conditions and contribution to industrial production.
Drawings
FIG. 1 is a scanning electron microscope image of a smoke agent for moisture-absorption-preventing cigarettes;
FIG. 2 is a thermogravimetric analysis comparison graph of a smoke agent for a moisture-absorption-preventing cigarette and a smoke agent for a common cigarette.
Detailed Description
The invention is further illustrated by the following examples, which are intended to better understand the contents of the study of the invention and are not intended to limit the scope of the invention.
Example 1
5mL of glycerin and 0.05g of sodium lauryl sulfate were added to 2.2mL of an aqueous solution of hydrochloric acid of 2.5M, dissolved with stirring at 60 ℃ and cooled to 25 ℃ to obtain solution A. 0.3g of span 80 is dissolved in 30mL of cyclohexane to obtain solution B. And adding the solution A into the solution B, emulsifying at 3000RPM for 1 minute to obtain a water-in-oil emulsion, heating to 35 ℃, and slowly dropping 5mL of tetraethoxysilane stock solution into the emulsion. And after the addition, continuously stirring and reacting for 24 hours at 35 ℃, filtering, washing filter residues twice by using cyclohexane, washing the filter residues by using ethanol for 1 time, drying the filter residues for 12 hours at 40 ℃, adding the obtained solid particles into a polysulfone dimethylformamide solution with the concentration of 0.5g/mL, stirring for 1.5 hours, filtering, washing twice, and drying the solid particles for 12 hours at 80 ℃ to obtain the smoke agent for the moisture absorption preventing cigarette.
The appearance of the smoke agent for the moisture absorption preventing cigarette is shown in figure 1, and as can be seen from the figure, the smoke agent is micron-sized spherical particles. And the size is more uniform.
Thermogravimetric analysis of the smoke agent and the glycerol for the moisture-absorption-preventing cigarette is shown in figure 2, and from figure 2, it can be seen that the atomization temperatures of the microcapsule smoke agent and the pure smoke agent are not obviously different, so that the effective component of the smoke agent is wrapped by a means which does not influence the atomization effect of the smoke agent.
Example 2
4mL of glycerin, 1mL of propylene glycol and 0.01g of sodium dodecyl sulfate were added to 1mL of an aqueous solution of hydrochloric acid concentration 0.5M, and the mixture was dissolved with stirring at 70 ℃ and then cooled to 15 ℃ to obtain solution A. 0.1g of Tween 80 was dissolved in 10mL of cyclohexane to obtain solution B. Adding the solution A into the solution B, cooling to 15 ℃, emulsifying for 5 minutes at 1000RPM to obtain water-in-oil emulsion, heating to 25 ℃, and dropwisely adding 3.75mL of methyl orthosilicate stock solution into the emulsion slowly. And after the addition, continuously stirring and reacting for 24 hours at 25 ℃, filtering, washing filter residues twice by using cyclohexane, washing the filter residues by using ethanol for 1 time, drying the filter residues for 12 hours at 40 ℃, adding the obtained solid particles into polysulfone dimethylformamide solution with the concentration of 0.3g/mL, stirring for 2 hours, filtering, washing twice by using water, and drying the solid particles for 12 hours at 80 ℃ to obtain the smoke agent for the moisture absorption preventing cigarette.
Example 3
8mL of glycerin, 2mL of butanediol and 1g of sodium dodecyl sulfate were added to 1mL of an aqueous solution of hydrochloric acid having a concentration of 1M, and the mixture was dissolved with stirring at 25 ℃ to obtain solution A. 2.5g of sodium dodecylsulfate was dissolved in 50mL of cyclohexane to obtain solution B. Adding the solution A into the solution B, emulsifying at room temperature at 10000RPM for 1 minute to obtain water-in-oil emulsion, heating to 30 ℃, and dropwisely adding 3.75mL of tetraethoxysilane stock solution into the emulsion. And after the addition, continuously stirring and reacting for 24 hours at 25 ℃, filtering, washing filter residue twice by using cyclohexane, washing the filter residue 1 time by using ethanol, drying the filter residue for 12 hours at 40 ℃, adding the obtained solid particles into polysulfone dimethylformamide solution with the concentration of 0.5g/mL, stirring for 1 hour, filtering, washing twice by using water, and drying the solid particles for 12 hours at 80 ℃ to obtain the smoke agent for the moisture absorption preventing cigarette.
The smoking agent for the moisture-proof cigarette prepared in the above examples and the tobacco sheet were mixed according to the addition ratio of 20%, and then exposed to the air for 15 days in a 60% humidity environment, and the moisture absorption performance of the smoking agent was evaluated by weighing the sample mass, and the experimental results are as follows:
Claims (19)
1. a smoking agent for moisture-absorption-preventing cigarettes is characterized in that: the cigarette smoke agent is encapsulated in the hydrophobic microcapsule shell.
2. The smoking agent for preventing moisture absorption cigarette as claimed in claim 1, wherein: the hydrophobic microcapsule shell is composed of an inorganic oxide shell and a hydrophobic layer modified on the surface of the inorganic oxide shell.
3. The smoking agent for preventing moisture absorption cigarette as claimed in claim 2, wherein: the inorganic oxide shell is made of at least one inorganic material of titanium dioxide, silicon dioxide and aluminum trioxide.
4. The smoking agent for preventing moisture absorption cigarette as claimed in claim 2, wherein: the hydrophobic layer is made of at least one hydrophobic material of polysulfone, polyarylsulfone and polyethersulfone.
5. The smoking agent for preventing moisture absorption cigarette as claimed in claim 1, wherein: the smoke agent for the cigarette is at least one of glycerol, propylene glycol, ethylene glycol, butanediol and butanetriol.
6. The agent for preventing smoking for moisture absorption according to any one of claims 1 to 5, wherein: the mass ratio of the smoke agent for the cigarette to the hydrophobic microcapsule shell is 9: 1-1: 1.
7. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to any one of claims 1 to 6, which is characterized by comprising the following steps: the method comprises the following steps:
1) dissolving a smoke agent for cigarettes, inorganic acid and a surfactant in water to obtain a solution A, and dissolving the surfactant in a nonpolar organic solvent to obtain a solution B;
2) adding the solution A into the solution B for emulsification under the stirring condition to obtain emulsion;
3) dropwise adding a microcapsule shell precursor material into the emulsion, stirring for reaction, and carrying out solid-liquid separation, washing and drying on an obtained reaction product to obtain a solid particle material;
4) adding the solid particle material into a solution containing the hydrophobic material, stirring for reaction, filtering, separating and drying to obtain the hydrophobic material.
8. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7, wherein the method comprises the following steps: the volume ratio of the smoke agent for the cigarette to the water and the nonpolar organic solvent is 1-10: 1: 10-50.
9. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 8, wherein the method comprises the following steps: the nonpolar organic solvent is n-hexane and/or cyclohexane.
10. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 8, wherein the method comprises the following steps: the inorganic acid is at least one of hydrochloric acid, sulfuric acid and nitric acid.
11. The method for preparing the smoke agent for the moisture absorption preventing cigarette according to claim 7 or 10, wherein the method comprises the following steps: the concentration of the inorganic acid in the solution A is 0.1-6.5M.
12. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7, wherein the method comprises the following steps: the surfactant is at least one of sodium dodecyl sulfate, span 80, Tween 80 and cetyl trimethyl ammonium bromide.
13. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7 or 12, wherein the method comprises the following steps: the concentration of the surfactant in the solution A is 0.01-0.1 g/mL; the concentration of the surfactant in the solution B is 0.005-0.05 g/mL.
14. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7, wherein the method comprises the following steps: the microcapsule shell precursor material contains at least one of n-butyl titanate, titanium tetrachloride, tetramethoxysilane, tetraethoxysilane, aluminum tert-butoxide and aluminum sec-butoxide.
15. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7, wherein the method comprises the following steps: and (3) dropwise adding the precursor material of the microcapsule shell into the emulsion at the temperature of 25-35 ℃, stirring for reaction, and continuing stirring for reaction for 18-30 hours after dropwise adding.
16. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7, wherein the method comprises the following steps: the concentration of the hydrophobic material in the solution containing the hydrophobic material is 0.1-0.5 g/mL.
17. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 16, wherein the method comprises the following steps: the solution containing the hydrophobic material is obtained by dissolving at least one hydrophobic material selected from polysulfone, polyarylsulfone and polyethersulfone in dichloromethane and/or DMF.
18. The method for preparing the smoke agent for the moisture absorption prevention cigarette according to claim 7, wherein the method comprises the following steps: in the step 4), the stirring reaction time is 0.5-3 hours.
19. The use of the smoke agent for preventing moisture absorption cigarette as claimed in any one of claims 1 to 6, wherein: is applied to heating non-combustion cigarettes.
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