CN111096469A - Polylactic acid-based flavor slow-release material, composite sheet, preparation method of composite sheet and application of composite sheet in heating non-combustible tobacco products - Google Patents
Polylactic acid-based flavor slow-release material, composite sheet, preparation method of composite sheet and application of composite sheet in heating non-combustible tobacco products Download PDFInfo
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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
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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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
- A24B15/281—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
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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
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
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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
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
Abstract
The invention belongs to the technical field of heating non-combustion cigarettes, and particularly discloses a polylactic acid-based flavor slow-release material for heating non-combustion tobacco products. The invention also provides a composite sheet compounded with the slow release material. In addition, the invention also provides a preparation method of the slow-release material and the composite sheet and an application method of the slow-release material and the composite sheet in heating non-combustible cigarettes. The invention innovatively discovers that the material is applied to a heating non-combustible tobacco product, and can overcome the technical problems that the fragrance of the first chewing tobacco product is too strong, the fragrance of the second chewing tobacco product is basically volatilized, the specific quality and style characteristics of the product are difficult to endow and the like caused by the fact that the fragrance is quickly released in the perfuming technology of the heating non-combustible tobacco product. The invention can obviously improve the fragrance slow-release effect of the product, improve the sensory quality of smoking and endow the product with stable quality and style characteristics.
Description
Technical Field
The invention relates to a method for slowly releasing the fragrance of a heating non-combustible tobacco product and application thereof, belonging to the technical field of novel slow release of the fragrance of the tobacco product.
Background
The heating non-combustion tobacco product (low-temperature tobacco) is a novel tobacco product with the flavor characteristics closest to the traditional cigarette, has lower harmful chemical components and biological toxicity in the smoke, and is the development focus of the tobacco industry of various countries in the world at present.
However, since the tobacco heating part is always in a heating state in the smoking process of the tobacco product which is not heated and is not combusted, the release of the flavor substances is caused, especially the release of the additional flavor substances with strong volatility is not uniform, the additional flavor substances are usually volatilized completely at the first mouth and the second mouth, the smoking taste is difficult to keep uniform before and after, and the quality stability and the product taste style are difficult to ensure. Thus, flavor delivery technology remains one of the short boards that have limited the development of products that do not burn tobacco when heated.
At present, some researches are carried out in the aspect of flavor slow-release control technology at home and abroad, and the main methods comprise: (1) adding fragrance precursor, and heating at high temperature or burning for cracking to generate fragrance substance. (2) The microcapsules are added. The coating of the essence is realized by coating and other technical means, and the essence are released by the rupture or degradation of the capsule wall. (3) Adding an adsorbent, and adsorbing the essence and the spice by utilizing the porous structure of the adsorbent.
However, the above-described flavor-release method is not suitable for heating a non-combustible tobacco product. The heating temperature is generally below 350 ℃, which is far lower than the combustion temperature of the traditional cigarette, so that some aroma precursors cannot be cracked to generate aroma substances, or the aroma substances wrapped in the microcapsule wall materials cannot be released because the cracking temperature of the microcapsule wall materials cannot be reached, or the aroma substances cannot be slowly and uniformly released only depending on the adsorption capacity of the adsorbent.
Chinese patent publication No. CN102821628A provides a supramolecular complex perfume immobilization and controlled release technology, which utilizes non-covalent bond interaction between supramolecular compounds and flavors to realize controlled release of flavors and fragrances. The patent mainly relates to simple perfume raw materials such as menthol and lemon oil, and does not describe the perfume slow-release effect of essence or perfume base with complex components.
Disclosure of Invention
In order to solve the defects that the aroma of the heating non-combustible tobacco product is not uniformly released and stable quality and style characteristics of the product are difficult to endow, the invention innovatively provides a polylactic acid-based aroma slow-release material (also called aroma slow-release material) for heating non-combustible tobacco products, and aims to remarkably improve the aroma slow-release effect of the product, improve the smoking sensory quality and endow the product with stable quality and style characteristics.
The second purpose of the invention is to provide a preparation method of the polylactic acid-based flavor slow-release material.
A third object of the present invention is to provide a polylactic acid-based flavor-sustained-release composite sheet (the present invention is also simply referred to as a composite sheet) comprising the polylactic acid-based flavor-sustained-release material.
The fourth purpose of the invention is to provide a preparation method of the composite sheet.
The fifth purpose of the invention is to provide an application method of the polylactic acid-based flavor slow-release material and/or the composite sheet added to the heating end of a heating non-combustible tobacco product.
A sixth object of the present invention is to provide a tobacco rod having a flavor-releasing function for heating a nonflammable tobacco product.
The seventh object of the present invention is to provide a tobacco product which does not burn upon heating and which is compounded with the tobacco rod having a flavor-releasing function.
A polylactic acid-based flavor slow-release material for heating non-combustible tobacco products comprises a polylactic acid base material and a flavor material for tobacco compounded in the polylactic acid base material.
The invention innovatively discovers that the material for the cigarette flavor is applied to a heating non-combustible tobacco product by adopting polylactic acid as a base material (carrier) and embedding, dispersing and inlaying the polylactic acid in the base material, can overcome the technical problems that the first flavor is too strong, the second flavor is almost completely volatilized, the specific quality and style characteristics of the product are difficult to endow and the like in the direct perfuming of the heating non-combustible tobacco product, and is favorable for developing the heating non-combustible tobacco product with good sensory quality and distinct style characteristics.
Preferably, the polylactic acid substrate is made of at least one of levorotatory polylactic acid (PLLA), dextrorotatory polylactic acid (PDLA), racemic polylactic acid (PDLLA) and meso-polylactic acid (meso-PLA); racemic polylactic acid is preferred.
The molecular weight of the polylactic acid is not less than 5 ten thousand, preferably 5 to 150 ten thousand. Preferably, the polylactic acid with the molecular weight is more beneficial to the slow release of the fragrance and is more beneficial to the preparation of the fragrance slow-release material.
In the polylactic acid-based flavor slow-release material, the mass percentage of the polylactic acid is 20-70%.
Preferably, the flavor material for the cigarette is at least one of monomer synthetic flavor, natural flavor raw material, essence base or essence.
The technical method is particularly suitable for volatile or semi-volatile additional fragrant substances, especially strong volatile fragrant substances. For example, it is particularly suitable for low-grade ester flavoring substances with volatilization temperature below 200 ℃. In addition, the method is also particularly suitable for cigarette flavor materials with complex components, such as cigarette surface flavor essence.
Preferably, the tobacco flavor material can be a characteristic flavor which is added into a non-combustion tobacco product by heating and is separately emphasized or highlighted, such as furanone, menthol, ethyl maltol and the like; further preferably, the tobacco flavoring essence and the surface essence containing the characteristic fragrance note can be used.
Preferably, the content of the flavor material for the cigarette is less than or equal to 40 percent by mass, and more preferably less than or equal to 35 percent by mass (based on the mass of the polylactic acid-based flavor slow-release material).
Preferably, the polylactic acid-based flavor release material is further compounded with an adsorbent and/or a filler. In the polylactic acid-based flavor slow-release material, the adsorbent and/or the filling material are embedded, dispersed or embedded in the polylactic acid base material. Researches show that the adsorbent and/or the filling material can adsorb, disperse and load cigarette flavor materials, modify the polylactic acid-based flavor slow-release material, and adjust the properties of the polylactic acid-based flavor slow-release material such as hardness, density, strength and the like.
According to the invention, the adsorbent and/or the filling material are/is added into the polylactic acid base material, and the flavor slow-release effect of the flavor material in the heating non-combustion tobacco product can be unexpectedly improved by utilizing the embedding effect of the polylactic acid.
Preferably, the cigarette flavor material is adsorbed in the adsorbent and/or the filling material.
Preferably, the adsorbent is one or more of activated carbon, diatomite, molecular sieve and cyclodextrin.
Preferably, the mass percentage of the adsorbent in the polylactic acid-based flavor release material is not higher than 40 wt.%.
Preferably, the filling material is one or more of tobacco powder, starch and vegetable gum.
Preferably, the vegetable gum is at least one of guar gum, carrageenan and fenugreek gum.
Preferably, the filling material accounts for not more than 40 wt.% of the polylactic acid-based flavor release material.
Preferably, the polylactic acid-based flavor-releasing material has a layered structure.
The invention also innovatively provides a preparation method of the polylactic acid-based flavor slow-release composite material, polylactic acid and flavor materials for cigarettes are dissolved by using a solvent to obtain a raw material solution, and then the solvent is removed to obtain the polylactic acid-based flavor slow-release material.
Preferably, the raw material solution further comprises an adsorbent and/or a filler.
Preferably, the polylactic acid and the flavor materials for cigarettes are dissolved by a solvent to obtain a viscous liquid or dough-like material, and the viscous liquid or dough-like material is uniformly stirred and coated into a sheet shape or made into a noodle shape to obtain the polylactic acid-based flavor slow-release material.
The preferred preparation method comprises the following steps: dissolving polylactic acid by using a solvent, adding an essence perfume (a cigarette flavor material), selectively adding an adsorbent and/or a filling material, fully stirring to uniformly disperse the mixture to form a viscous polylactic acid solution or a dough-like material, then preparing a sheet or a noodle by adopting a coating method, removing the solvent, cutting the sheet or the noodle into threads, sheets or granules, and mixing the threads, sheets or granules with a tobacco material end (a heating end) of a tobacco product which is not combusted by heating, so as to realize the slow and uniform release of the essence perfume in a heating range of 150 plus 300 ℃.
In the present invention, the solvent is a solvent capable of dissolving polylactic acid, and is preferably a solvent having a boiling point of not higher than 100 ℃.
Preferably, the solvent is a solvent comprising halogenated hydrocarbons such as dichloromethane, chloroform, etc., or lower esters such as ethyl acetate, ethyl lactate, etc.
In the invention, the method for removing the solvent can be room temperature volatilization, hot air drying at 30-50 ℃, low-temperature evaporation or freeze drying.
The invention also provides a polylactic acid-based flavor slow-release composite sheet for heating non-combustible tobacco products, which comprises the polylactic acid-based flavor slow-release material layer and a polylactic acid layer compounded on the surface of the polylactic acid-based flavor slow-release material layer.
The invention innovatively discovers that compared with the polylactic acid-based flavor slow-release material, the composite sheet formed by compounding the polylactic acid-based flavor slow-release material and the polylactic acid has better flavor slow-release effect and more uniform flavor release.
Preferably, the polylactic acid-based flavor sustained-release composite sheet is a two-layer sheet in which a polylactic acid layer and a polylactic acid-based flavor sustained-release material layer are combined. That is, the polylactic acid layer is compounded on one plane of the polylactic acid-based flavor release material layer.
More preferably, the polylactic acid-based flavor sustained-release composite sheet is a three-layer sandwich sheet comprising a polylactic acid layer, a polylactic acid-based flavor sustained-release material layer and a polylactic acid layer in sequence. That is, the polylactic acid layer is compounded on the upper plane and the lower plane of the polylactic acid-based flavor slow-release material layer.
Preferably, the polylactic acid-based flavor sustained-release composite sheet is a multilayer composite sheet having four or more layers in which a polylactic acid layer and a polylactic acid-based flavor sustained-release material layer are sequentially combined.
To be suitable for use in an application, the polylactic acid based flavour release material may be cut into various shapes for application to heated non-combustible tobacco products, including but not limited to filaments, tablets, granules.
The invention also provides a preparation method of the polylactic acid-based flavor slow-release composite sheet, which comprises the steps of preparing a raw material solution and a polylactic acid solution, sequentially coating the solutions according to the structure of the composite sheet, and removing the solvent to obtain the polylactic acid-based flavor slow-release composite sheet.
For example, polylactic acid is dissolved in a solvent, the solvent is removed to form a polylactic acid layer, then a raw material solution is prepared according to the preparation method of the fragrance sustained-release material, the raw material solution is compounded on the polylactic acid layer, and the solvent is removed to obtain the polylactic acid-based fragrance sustained-release composite sheet. And repeating the steps according to the composite sheet structure to obtain the required composite sheet.
The invention also provides an application of the polylactic acid-based flavor slow-release material and/or the polylactic acid-based flavor slow-release composite sheet, which is used for preparing a tobacco rod of a heating non-combustible tobacco product.
The tobacco rod is the portion that heats the heated end of the nonflammable tobacco product and produces the tobacco aroma. According to the application, the polylactic acid-based flavor slow-release material and/or the composite sheet are/is added to a tobacco rod (a tobacco material end, namely a heating end) of the heating non-combustible tobacco product, so that the flavor of the heating non-combustible tobacco product is slowly released. The flavor slow-release method for the tobacco product which is not burnt by heating and uses the polylactic acid as the base material to fix the flavors and fragrances is applied to the tobacco product which is not burnt by heating and has good effects of improving the flavor quality of the product and endowing style characteristics.
Preferably, the application is to mix at least one of the polylactic acid-based flavor release material and the polylactic acid-based flavor release composite sheet with tobacco materials (such as cut tobacco) to prepare a unit tobacco rod.
Preferably, at least one of the polylactic acid-based flavor-releasing material and the polylactic acid-based flavor-releasing composite sheet is formed into a thread form, and the thread form is mixed with a tobacco material (e.g., cut tobacco) and rolled into a cigarette-form heated non-burning tobacco product.
The invention also provides a tobacco rod of a heating non-combustion tobacco product with a flavor slow-release function, which comprises tobacco materials and at least one of the polylactic acid flavor slow-release material and the polylactic acid-based flavor slow-release composite sheet.
The tobacco rod is a unit rod or a binary and multi-element composite rod.
The adding percentage content of at least one of the polylactic acid-based flavor slow-release material and the polylactic acid-based flavor slow-release composite sheet of the tobacco rod is 1-10%.
The invention also provides a heating non-combustible tobacco product with a fragrance slow-release function, which comprises a filter stick and the tobacco stick which are connected in a tipping mode.
Has the advantages that:
1. the preparation method of the fragrance slow-release sheet is simple, and the application forms of the fragrance slow-release sheet in heating ends of heating non-combustible tobacco products are various. The polylactic acid is used as a nontoxic biodegradable covering material, can block natural volatilization of the essence and the spice at normal temperature, and is convenient to store and transport; can be softened gradually in the heating process, thereby slowly and uniformly releasing the essence and the spice.
2. The invention is not only suitable for simple fragrant raw materials, but also has the most outstanding advantages that the invention can be suitable for essence and fragrant base with complex components, can well improve the richness of the fragrance of the smoke of the heating non-combustible tobacco product, improve the quality stability of the heating non-combustible tobacco product and lay the technical foundation of endowing the product with style characteristics by using the essence and the spice.
Drawings
Fig. 1 is a TG curve of essence a.
FIG. 2 is a TG curve of polylactic acid.
Fig. 3 is a TG curve of the polylactic acid flavor-sustained release sheet.
FIG. 4 is a constant temperature TG curve of polylactic acid fragrance sustained-release sheet at 220 deg.C
The specific implementation scheme is as follows:
the invention is further described with reference to specific examples. The following examples are intended to illustrate the invention without further limiting it.
Example 1
The essence A is a common conventional cigarette essence, and is applied to a heating non-combustible tobacco product, wherein the contained fragrance components mainly comprise ethyl acetate, ethyl butyrate, 2-methyl ethyl butyrate, ethyl isovalerate, furfural, hexyl hexanoate, 3-methyl-pyrazine, 2-ethyl-3-methyl pyrazine, benzaldehyde, acetophenone, megastigmatrienone, geranyl acetone, β -damascenone, menthol, methyl phenylacetate, a tobacco extract, a fig extract, an apple extract, jujube, vanilla bean tincture, benzoin cream, a liquorice fluid extract and the like.
In order to promote the essence A to be slowly and uniformly released in the heating stage, the L-polylactic acid is used as a thin sheet base material to fix the essence A and is applied to the heating end for heating the non-combustible tobacco product. The specific implementation method comprises the following steps: 2g of L-polylactic acid (molecular weight 60 ten thousand, type DG-L400, Jinan Dai Ting Dian bioengineering Co., Ltd.) was weighed and about 30ml of methylene chloride solution was added to completely dissolve the polylactic acid. Then adding 2g of essence A, and fully stirring to uniformly disperse the essence in the solution; coating the above liquid on a flat plate, evaporating at room temperature to remove solvent, making into sheet, cutting into filaments with length of about 20mm, and blending into tobacco material of thin cigarette-shaped non-combustible tobacco product.
FIG. 2 is a thermogravimetric curve of L-polylactic acid, and it is found by analysis that L-polylactic acid has stable quality below 320 ℃ and rapidly loses weight from 340 ℃. FIG. 3 is a thermogravimetric curve of the L-polylactic acid fragrance sustained-release composite material loaded with essence A, wherein the material can achieve a good sustained-release effect at a programmed temperature of 150-300 ℃, the weight loss rate is 22%, and the main temperature range of essence volatilization is 150-300 ℃; FIG. 4 is a constant temperature thermogravimetric curve of the L-polylactic acid fragrance sustained-release composite material at 220 ℃, the temperature rises to 220 ℃ in 1min and starts to be in a constant temperature state, the sheet has a slow and uniform weight loss trend, the weight loss rate in 15min is about 9%, and the time for continuously losing weight and releasing fragrance reaches more than 20 min.
The smoking test result of the tobacco product which is not combusted by heating shows that the tobacco product which is not combusted by heating after the sheet is added has better fragrance persistence and uniform mouth-to-mouth release, and obvious fragrance can be sensed from the first mouth to the sixth mouth and the seventh mouth, which are consistent with the instrument simulation test result. Meanwhile, researches show that the higher the content of the fragrant materials, the more the fragrance materials are dissociated, the more the loss in the processing process is, and the lower the utilization efficiency is. The aroma characteristics are prominent when the addition amount of the aroma materials is large. The specific addition ratio depends on the application, and when the other fragrances are modified, the ratio may be less than 1% or even lower.
In conclusion, the invention is suitable for the formula of the essence and the spice with complex fragrance components, compared with the direct injection perfuming, the polylactic acid fragrance slow-release sheet added can achieve the effect of slow and uniform weight loss at the temperature of 150-300 ℃, and meets the requirement of heating slow release of a non-combustible tobacco product.
Example 2
In another optimized embodiment, the flavor slow-release sheet is prepared by adding polylactic acid solution after the flavor and the spice are adsorbed by the adsorbent and is applied to the heating end of a non-combustion tobacco product, and the specific steps are as follows: sieving the activated diatomite with a 40-mesh sieve, drying in an oven at 500 ℃ for 12h, and cooling at room temperature for later use; mixing the essence A and 40-mesh diatomite according to a ratio of 1: 1, uniformly stirring, and then placing in a room temperature environment for balancing for 0.5 h; adding equal amount of L-polylactic acid (molecular weight 60 ten thousand, type DG-L400 of Jinan Dai big Dipper bioengineering Co., Ltd.) into the above balance system, adding 15 times volume of dichloromethane solution to dissolve polylactic acid, and stirring thoroughly until the absorbing material and essence perfume are uniformly dispersed in viscous liquid; uniformly coating the liquid on a flat plate, and removing the solvent by adopting a hot air drying method at 30 ℃ to obtain the flaky slow-release composite material; it is cut into particles with a diameter of about 2mm and blended into tobacco material of a non-combustible heated tobacco product.
The result of the smoke panel test and the thermogravimetric analysis show that the adsorbent-containing L-polylactic acid sustained-release sheet can achieve the effect of slow and uniform weight loss at the temperature of 150-300 ℃, the mouth-to-mouth release uniformity of the essence and the spice is better, the sustained and uniform release time reaches more than 25min, and the weight loss rate is 7% within 15 min. Meets the requirement of heating the non-combustible tobacco product for slow release.
Example 3
The essence A is fixed by using racemic polylactic acid as a base material, and cyclodextrin is added as an adsorbent. The specific implementation steps are as follows: weighing 2g of cyclodextrin, uniformly mixing with 2g of essence A, and balancing at room temperature for 0.5 h; adding 2g ester-terminated racemic polylactic acid (OH-PDLLA-COOR, molecular weight 19 ten thousand, type DG-DL150, manufactured by Jinan Dai handle & Dipper bioengineering Co., Ltd.), dissolving with about 20ml ethyl acetate solution to form viscous liquid, and stirring thoroughly to disperse uniformly; coating the liquid on a flat plate, and removing the solvent by adopting a room-temperature volatilization method to obtain a flaky slow-release composite material with the thickness of about 0.5 mm; the sheet was cut into strands of approximately 20mm length and blended at a rate of 2% into tobacco material of a heated non-combustible smoking article.
Test results show that the racemic polylactic acid flavor slow-release sheet added with cyclodextrin can remarkably improve the mouth-to-mouth release uniformity of essence and flavor in a heating non-combustible tobacco product, is beneficial to the slow and uniform release of the essence and flavor at the temperature of 150-300 ℃, the sustained release time reaches more than 25min, and the weight loss rate within 15min is 7%. Meets the requirement of heating and slow release at the burning end of the tobacco product which is not burned. Meanwhile, the racemic polylactic acid can be dissolved by adopting ethyl acetate, and the ethyl acetate is used as a high-volatility common fragrant raw material, so that the quick drying of the composite material is facilitated, and the fruity fragrance can be increased. Therefore, the polylactic acid is preferably a racemic polylactic acid.
Example 4
According to the method of the embodiment 3, the adsorbent is replaced by the H β molecular sieve, and the prepared flavor slow-release sheet is shredded and then blended into the tobacco material of the heating non-combustible tobacco product, so that the flavor slow-release sheet has good slow-release effect, the flavor and the fragrance can be slowly and uniformly released at the temperature of 150-300 ℃, the sustained-release time reaches more than 25min, and the weight loss rate within 15min is 6.5%.
Example 5
In another optimization scheme, the slow-release sheet has a double-layer structure, the first layer is a polylactic acid sheet, the second layer is a slow-release sheet added with active carbon, the essence B is used as the slow-release essence, and the essence B mainly comprises the following fragrance components of ethyl acetate, ethyl propionate, ethyl butyrate, ethyl isovalerate, ethyl caproate, furfural, 3-methylpyrazine, amyl valerate, benzyl alcohol, ethyl caprylate, benzyl acetate, ethyl caprate, megastigmatrienone, β -damascenone, dihydrodamascenone, geranylacetone, clary sage oil, lemon oil, tobacco extract, cocoa extract, vanilla bean tincture, iris extractum, licorice fluid extractum and the like, and the specific implementation steps are as follows:
1. weighing 2g ester-terminated racemic polylactic acid (OH-PDLLA-COOR, molecular weight 19w), adding 20ml ethyl acetate, and completely dissolving to obtain viscous polylactic acid solution;
2. pouring 10ml of the liquid into a flat plate, and removing the solvent by room-temperature volatilization to form a polylactic acid sheet with the thickness of about 0.5 mm;
3. 1g of essence B and 1g of 150-mesh active carbon are uniformly mixed and then are placed in a room temperature environment for balancing for 1 hour. And (3) adding 10ml of polylactic acid solution in the step (1), fully stirring until the solution is uniformly dispersed, coating the solution on the polylactic acid sheet formed in the step (2), and volatilizing at room temperature to remove the solvent to form the slow-release composite material with a double-layer structure.
4. The double-layer structure slow-release agent is cut into pieces with the width of about 2mm, and the pieces are blended into tobacco materials of a tobacco product which is not burnt when being heated in a proportion of 3%.
The test result shows that the double-layer structure racemic polylactic acid slow-release composite material can obviously improve the uniformity of the gradual release of the essence and the spice in the heating non-combustible tobacco product, the release uniformity is further improved on the basis of the example 1, the essence and the spice can be slowly and uniformly released at the temperature of 150-300 ℃, the weight loss rate is 6 percent within 15min, and the sustained release time in the heating non-combustible tobacco product can reach eight or nine mouths.
Example 6
On the surface of the sustained-release composite material with the double-layer structure formed in the example 5, the method of the example 5 is adopted, and then the composite material with the double-layer structure is compounded, namely the sustained-release composite material with the four-layer structure in which the polylactic acid and the composite material are distributed in a staggered manner is formed. The result shows that the slow release effect of the structural composite material is further improved on the basis of the embodiment 5, the weight loss rate is about 6% within 15min, and the sustained release time can reach more than nine mouths.
Example 7
In another embodiment, tobacco powder is added as a filling material, and a slow-release material is prepared by adopting a noodle press method, and the specific implementation method is as follows: 40g of ester-terminated racemic polylactic acid (OH-PDLLA-COOR, molecular weight 19w) was weighed and added to about 400ml of ethyl acetate solution to completely dissolve the polylactic acid and form a viscous liquid. Adding 20g of essence B and 10g of tobacco powder, and stirring and kneading to uniformly disperse the essence B in the dough-like material. Feeding the dough-like material into a household noodle maker, customizing the size of an outlet aperture to be 1mm, extruding the material from a fine hole in an extrusion mode to form a noodle shape, removing the solvent by adopting a room temperature volatilization method, drying, cutting into the length of about 20mm, and blending the length of about 20mm into the tobacco material of a heating non-combustion tobacco product in a proportion of 3%.
The test result shows that the tobacco powder is added to enhance the tobacco fragrance of the heating non-combustible tobacco product, and the characteristics of the slow release material such as tensile strength, hardness and the like can be adjusted, so that the tobacco product can be conveniently rolled, the essence and the spice at the heating end can slowly and uniformly lose weight at the temperature of 150-300 ℃, the sustained release time reaches more than 25min, the weight loss rate is 8% within 15min, and the requirement of heating the heating non-combustible tobacco product for slow release is met.
Example 8
According to the method of the embodiment 7, the filling material is replaced by the porous starch, and the prepared noodle-shaped flavor slow-release material is applied to the heating end of the non-burning tobacco product, so that the slow-release effect is good, the essence and the spice at the heating end can be slowly and uniformly released at the temperature of 300 ℃ for more than 25min, and the weight loss rate is 7% within 15 min.
Example 9
The guar gum is used as a filling material to prepare the fragrance sustained-release material, and the specific implementation steps are as follows: weighing 10g of ester-terminated racemic polylactic acid (OH-PDLLA-COOR, molecular weight 61w), and adding about 200ml of ethyl lactate solution to completely dissolve the polylactic acid into polylactic acid solution; weighing 2.5g of guar gum, dissolving with cold water, and adding a polylactic acid solution to increase the viscosity of the polylactic acid solution; then adding 20g of essence B, and fully stirring to uniformly disperse the essence and the spice; after leaving the volatile solvent for a period of time, the above materials were converted into dough, extruded into noodle-like sustained-release materials in the manner of example 6, the solvent was removed by evaporation at a low temperature of 30 ℃, cut into about 20mm lengths and blended into tobacco materials of a tobacco product which was not heated to burn in a proportion of 3%.
The test result shows that the addition of the guar gum is beneficial to increasing the viscosity of the solution, and the characteristics of the slow-release material such as tensile strength, hardness and the like can be adjusted, so that the essence and the spice at the heating end can be slowly and uniformly released at the temperature of 150-300 ℃. The sustained release time reaches 30min, and the weight loss rate within 15min is 9%.
Example 10
According to the method of the embodiment 2, the concentrated tea aroma essence, the adsorbent diatomite and the racemic polylactic acid (OH-PDLLA-COOR, molecular weight 115w, Jinan DG-DL500) are compounded according to the proportion of 1: 1, the mixture is made into a flaky slow-release composite material, then the flaky slow-release composite material is cut into threads, the flaky slow-release composite material is mixed with tobacco materials according to the proportion of 10 percent and rolled into cigarettes, and sensory evaluation tests are carried out, and the result shows that the product shows very thick and outstanding tea aroma characteristics and can continuously and uniformly release more than ten mouthfuls of tea aroma; when the adding proportion of the composite material is reduced to 1 percent, the light tea fragrance is shown, and seven or eight mouths can be released continuously and uniformly. Therefore, the adding proportion of the composite material is determined according to the actual application condition, and when the fragrance of certain characteristic essence is weak or important points need to be highlighted, the adding proportion of the composite material can be increased; when the aroma characteristics of certain essences are obvious or the emphasis on the aroma characteristics is not required to be obvious, the adding proportion of the composite material can be properly reduced.
Through comparison between the example 1 and the examples 2-5, the adsorbent with the porous structure is added, so that the adsorption and fixation effects on the essence and the spice can be enhanced, and the essence release time is prolonged; compared with the L-polylactic acid, the racemic polylactic acid is adopted, so that the solvent is better in safety and can enhance the fragrance of fruit fragrance; as shown by comparing example 2 with examples 4 to 5, the composite material of the multilayer structure compounded with the polylactic acid has better slow release effect than a single layer and more uniform fragrance release; compared with the examples 7-9, the filler material, especially the tobacco powder, added in the example 2 is found to enhance the tobacco fragrance of the product, and is also beneficial to adjusting the characteristics of the composite material, such as tensile strength, hardness and the like, so that the composite material can be more easily and uniformly mixed with tobacco materials and rolled into cigarettes; compared with the examples 4-5, the composite material with the multilayer structure has better slow release effect than a single layer; by way of examples 1-10 we have found that the larger the molecular weight of the polylactic acid, the more solvent is needed for complete dissolution.
The present invention is not limited to the above embodiments, and it is within the scope of the present invention to use polylactic acid as a base material to fix flavors and fragrances and to apply the polylactic acid to a non-combustible tobacco product by heating.
Claims (27)
1. A polylactic acid-based flavor slow-release material for heating non-combustible tobacco products is characterized by comprising a polylactic acid base material and a tobacco flavor material compounded in the polylactic acid base material.
2. The polylactic acid-based flavor-sustained-release material according to claim 1, wherein the polylactic acid is at least one of a levorotatory polylactic acid, a dextrorotatory polylactic acid, a racemic polylactic acid, and a meso-polylactic acid;
the molecular weight of the polylactic acid is not less than 5 ten thousand, preferably 5 to 150 ten thousand.
3. The polylactic acid-based flavor-sustained-release material according to claim 2, wherein the polylactic acid is contained in an amount of 20 to 70% by mass.
4. The polylactic acid-based flavor slow-release material according to claim 1, wherein the flavor material for cigarettes is at least one of monomer synthetic flavor, natural flavor raw material, flavor base or essence.
5. The polylactic acid-based flavor release material according to claim 4, wherein the content of the flavor material for cigarettes is 40% by mass or less.
6. The polylactic acid-based flavor-sustained-release material according to claim 1, wherein an adsorbent and/or a filler is further compounded in the polylactic acid-based flavor-sustained-release material.
7. The polylactic acid-based flavor release-controlling material according to claim 6, wherein the adsorbent is one or more of activated carbon, diatomaceous earth, molecular sieves, and cyclodextrin.
8. The polylactic acid-based flavor-sustained-release material according to claim 6, wherein the adsorbent accounts for not more than 40 wt.% of the polylactic acid-based flavor-sustained-release material.
9. The polylactic acid-based flavor release material according to claim 6, wherein the filler is one or more of tobacco powder, starch, and vegetable gum.
10. The polylactic acid-based flavor release material according to claim 9, wherein the vegetable gum is at least one of guar gum, carrageenan and fenugreek gum.
11. The polylactic acid-based flavor-sustained-release material according to claim 6, wherein the filler accounts for not more than 40 wt.% of the polylactic acid-based flavor-sustained-release material.
12. A preparation method of the polylactic acid-based flavor slow-release material as claimed in claims 1 to 11, characterized by dissolving polylactic acid and flavor materials for cigarettes with a solvent to obtain a raw material solution, and then removing the solvent to obtain the polylactic acid-based flavor slow-release composite material.
13. The method according to claim 12, wherein the raw material solution further contains an adsorbent and/or a filler.
14. The method according to any one of claims 12 to 13, wherein the solvent is a solvent which can dissolve polylactic acid and has a boiling point of not higher than 100 ℃.
15. The method according to claim 14, wherein the solvent is at least one of dichloromethane, chloroform, ethyl lactate, and ethyl acetate.
16. A polylactic acid-based flavor-sustained-release composite sheet for use in a tobacco product which does not burn when heated, comprising the polylactic acid-based flavor-sustained-release material layer according to any one of claims 1 to 11 and a polylactic acid layer compounded on the surface thereof.
17. The polylactic acid-based flavor-sustained-release composite sheet according to claim 16, which is a double-layered sheet in which a polylactic acid layer and a polylactic acid-based flavor-sustained-release material layer are combined.
18. The polylactic acid-based flavor-sustained-release composite sheet according to claim 16, which is a three-layer-sandwiched sheet comprising a polylactic acid layer, a polylactic acid-based flavor-sustained-release material layer and a polylactic acid layer in this order.
19. The polylactic acid-based flavor-sustained-release composite sheet according to claim 16, which is a multilayer composite sheet comprising four or more layers in which a polylactic acid layer and a polylactic acid-based flavor-sustained-release material layer are sequentially laminated.
20. The method for producing a polylactic acid-based flavor sustained-release composite sheet according to any one of claims 16 to 19, wherein a raw material solution and a polylactic acid solution are prepared, and the solution and the solvent are sequentially applied and removed in the sheet structure to obtain the polylactic acid-based flavor sustained-release composite sheet.
21. Use of the polylactic acid-based flavor-sustained-release material according to any one of claims 1 to 14 and/or the polylactic acid-based flavor-sustained-release composite sheet according to any one of claims 16 to 19 for producing a tobacco rod for a tobacco product that does not burn when heated.
22. The use according to claim 21, wherein the tobacco material is mixed with at least one of the polylactic acid-based flavor-sustained-release material and the polylactic acid-based flavor-sustained-release composite sheet to produce a unitary tobacco rod.
23. The use according to claim 22, wherein at least one of the polylactic acid-based flavor-releasing material, the polylactic acid-based flavor-releasing composite sheet is formed into a thread form, and is mixed with tobacco shreds and rolled into a cigarette-form heated non-combustible tobacco product.
24. A tobacco rod for a heating non-burning tobacco product having a flavor-releasing function, comprising a tobacco material and at least one of the polylactic acid-based flavor-releasing material according to any one of claims 1 to 11 and the polylactic acid-based flavor-releasing composite sheet according to any one of claims 16 to 19.
25. A tobacco rod for a non-combustible smoking article having a flavor-releasing function, according to claim 24, wherein said tobacco rod is a unit rod or a composite rod of two or more units.
26. The tobacco rod according to any one of claims 24 or 25, wherein at least one of the polylactic acid-based flavor-sustained-release material and the polylactic acid-based flavor-sustained-release composite sheet is added in an amount of 1 to 10% by weight.
27. A heated non-combustible smoking article having a flavour release function, comprising a tipping filter rod and a tobacco rod according to any one of claims 24 to 26.
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