CN119679197A - Preparation method and application of tobacco refined product - Google Patents
Preparation method and application of tobacco refined product Download PDFInfo
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- CN119679197A CN119679197A CN202411982121.0A CN202411982121A CN119679197A CN 119679197 A CN119679197 A CN 119679197A CN 202411982121 A CN202411982121 A CN 202411982121A CN 119679197 A CN119679197 A CN 119679197A
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Abstract
本申请公开一种烟草精制物的制备方法及应用。该制备方法包括以下步骤：S1，将烟草浸膏通过乙醇水溶液溶解稀释，获得烟草溶液；S2，向烟草溶液中加入H型β分子筛，搅拌过滤得到烟草滤液；S3，将烟草滤液经大孔吸附树脂柱动态吸附，并使用乙醇水溶液梯度洗脱，得到烟草洗脱液；S4，将烟草洗脱液减压浓缩得到浓缩液，浓缩液再经调配处理得到烟草精制物。本申请技术方案，通过以上步骤设置，可在步骤S2中基于H型β分子筛吸附去除大量的亚硝胺，以及在步骤S3和步骤S4中进一步辅助去除少量的亚硝胺，以最终得到亚硝胺含量低的烟草精制物。该烟草精制物应用于电子烟产品中时，得益于亚硝胺含量低，可以极大减小对人体的损害，提升安全性。
The present application discloses a preparation method and application of a tobacco refined product. The preparation method comprises the following steps: S1, dissolving and diluting tobacco extract by ethanol-water solution to obtain tobacco solution; S2, adding H-type β molecular sieve to the tobacco solution, stirring and filtering to obtain tobacco filtrate; S3, dynamically adsorbing the tobacco filtrate by a macroporous adsorption resin column, and gradient eluting with ethanol-water solution to obtain tobacco eluate; S4, decompressing and concentrating the tobacco eluate to obtain a concentrated solution, and the concentrated solution is further blended to obtain a tobacco refined product. The technical solution of the present application, through the above steps, can remove a large amount of nitrosamines based on H-type β molecular sieve adsorption in step S2, and further assist in removing a small amount of nitrosamines in steps S3 and S4, so as to finally obtain a tobacco refined product with a low nitrosamine content. When the tobacco refined product is used in electronic cigarette products, thanks to the low nitrosamine content, it can greatly reduce the damage to the human body and improve safety.
Description
Technical Field
The application relates to the technical field of electronic cigarettes, in particular to a preparation method and application of a tobacco refined product.
Background
The atomized liquid of electronic cigarette is also called as electronic cigarette oil, and refers to a liquid mixture which can be atomized into inhalable aerosol by an electronic cigarette tool, and the main components of the atomized liquid are Vegetable Glycerin (VG), 1, 2-Propanediol (PG), nicotine salt and edible essence and spice additive. The variety and the dosage of the essence and the spice are reasonably selected, so that the electronic tobacco tar can present various tastes, such as various tastes of tobacco, fruits, herbs, foods, beverages and the like.
The tobacco extract is an important fragrant raw material in tobacco-flavor electronic tobacco tar, and can present natural tobacco aroma. However, in tobacco extracts, nitrosamines (TSNAs) have strong carcinogenicity, mainly contain NNK, NNN, NAB and other strong carcinogens, and seriously harm physical and mental health of users of electronic cigarettes.
Disclosure of Invention
The application provides a preparation method and application of a tobacco refined product, and aims to solve the problem that the existing tobacco extract has high nitrosamine content and endangers physical and mental health of users of electronic cigarettes.
In order to achieve the above object, the present application provides a method for preparing a tobacco refined product. The preparation method comprises the following steps:
S1, dissolving and diluting tobacco extract by using an ethanol water solution to obtain a tobacco solution;
S2, adding a powdery H-type beta molecular sieve into the tobacco solution, stirring and filtering to obtain tobacco filtrate;
s3, dynamically adsorbing the tobacco filtrate by a macroporous adsorption resin column, and performing gradient elution by using an ethanol aqueous solution to obtain a tobacco eluent;
s4, concentrating the tobacco eluent under reduced pressure to obtain concentrated solution, and blending the concentrated solution to obtain the refined tobacco product.
In some embodiments, the tobacco extract comprises a flue-cured tobacco extract, a aromatic tobacco extract, a burley tobacco extract, and a cigar extract.
In some embodiments, in step S1, the volume fraction of the aqueous ethanol solution is 0-30%, and the volume ratio of the total amount of the non-volatile components in the obtained tobacco solution is 1-10%.
In some embodiments, the added mass of the H-type beta molecular sieve is 0.5-3% of the mass of the tobacco solution, and the molar ratio of SiO 2 to Al 2O3 in the H-type beta molecular sieve is 20-45:1.
In some embodiments, in step S2, the stirring temperature is 10-40 ℃, the stirring time is 0.5-2 hours, and the stirring speed is 300-800 r/min.
In some embodiments, the macroporous adsorption resin has a specific surface area of 450-550 m 2/g and an average pore diameter of 10-100 nm.
In some embodiments, in the gradient elution, the volume fraction of the aqueous ethanol solution is 0-95%, and the elution flow rate is 1-3 BV/h.
In some embodiments, the reduced pressure concentration is performed at a pressure of 30 to 100mbar and a temperature of 40 to 60 ℃.
In some embodiments, the compounding process comprises adding propylene glycol to the concentrate and mixing well;
wherein the adding mass of the propylene glycol is 0.1-0.5 times of the mass of the concentrated solution.
The application also provides application of the tobacco refined product in electronic cigarettes.
The application provides a preparation method and application of a tobacco refined product. The preparation method comprises the following steps of S1, dissolving and diluting tobacco extract through an ethanol aqueous solution to obtain a tobacco solution, S2, adding an H-type beta molecular sieve into the tobacco solution, stirring and filtering to obtain a tobacco filtrate, S3, dynamically adsorbing the tobacco filtrate through a macroporous adsorption resin column, and carrying out gradient elution through the ethanol aqueous solution to obtain a tobacco eluent, S4, concentrating the tobacco eluent under reduced pressure to obtain a concentrated solution, and carrying out blending treatment on the concentrated solution to obtain a tobacco refined product. According to the technical scheme, through the arrangement of the steps, a large amount of nitrosamine can be removed based on the adsorption of the H-type beta molecular sieve in the step S2, and a small amount of nitrosamine is further removed in the step S3 and the step S4, so that the refined tobacco with low nitrosamine content is finally obtained. When the tobacco refined product is further applied to electronic cigarette products, the tobacco refined product benefits from low nitrosamine content, so that the harm to human bodies can be greatly reduced, and the safety is improved.
Drawings
For a clearer description of embodiments of the application or of solutions in the prior art, the drawings that are necessary for the description of the embodiments or of the prior art will be briefly described, it being apparent that the drawings in the description below are only some embodiments of the application, from which, without the inventive effort, other drawings can be obtained for a person skilled in the art, in which:
fig. 1 is a schematic structural view of a method for producing a tobacco refined product according to an embodiment of the present application.
Fig. 2 is a state diagram of the electronic cigarette after use, and fig. 2 (a) is a schematic diagram of the electronic cigarette paste core state after use of the electronic cigarette atomized liquid prepared from the tobacco refined product according to the comparative example of the present application, and (b) is a schematic diagram of the electronic cigarette non-paste core state after use of the electronic cigarette atomized liquid prepared from the tobacco refined product according to the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Referring to the flow chart shown in fig. 1, the application provides a preparation method of a tobacco refined product. The preparation method comprises the following steps:
and S1, dissolving and diluting the tobacco extract by using an ethanol aqueous solution to obtain a tobacco solution.
The tobacco extract is a concentrate obtained by a series of extraction processes of tobacco, and contains various components in the tobacco, such as nicotine, tar, aroma substances, organic acid, alkaloid and the like. These ingredients are present in the tobacco extract in a dissolved or suspended state. The ethanol aqueous solution is a solution prepared by mixing ethanol and water according to a certain proportion, and can be used as a solvent to dissolve and dilute the tobacco extract.
In the step, according to the proportion of the non-volatile components in the tobacco extract, the proportion of the non-volatile components in the tobacco solution obtained by dissolution dilution can be controlled by controlling the ethanol content in the ethanol aqueous solution. Specifically, the volume fraction of the ethanol aqueous solution is set in a range of 0-30%, so that the ethanol aqueous solution with the corresponding volume fraction is added based on the tobacco extract, and the total volume of the nonvolatile components in the tobacco solution formed by final dissolution and dilution is 1-10%. Thus, when the non-volatile components in the tobacco solution are in a certain proportion, the operation of removing the nitrosamine in the subsequent step is facilitated. It can be understood that the concentration range of the non-volatile component is 1-10%, which indicates that the dissolution of the tobacco extract is relatively sufficient, the competition adsorption phenomenon of the non-volatile component is relatively less, the specific adsorption of the subsequent H-type beta molecular sieve to nitrosamine is facilitated, and the balance of the adsorption quality and the separation efficiency of the subsequent macroporous adsorption resin column is facilitated when the concentration range of the non-volatile component is 1-10%.
A dissolving and diluting operation for tobacco extract is as follows:
Selecting tobacco extract, putting the tobacco extract into a beaker, then adding an ethanol water solution with corresponding volume fraction, and stirring and dissolving to obtain the tobacco solution with the non-volatile components. The tobacco extract can be dissolved and diluted by stirring, the stirring parameters can be set to be 10-40 ℃, the stirring speed is 300-800 r/min, and the stirring time is 0.5-1.0 hour. Whereas the measurement of the total amount of non-volatile components can be determined with reference to YC/T145.9-2012.
In some embodiments, the tobacco extract includes flue-cured tobacco extract, aromatic tobacco extract, burley tobacco extract, and cigar extract. The different types of extractum have unique flavor and chemical components. By selecting different extract types, the tobacco refined product with unique flavor and taste can be correspondingly created.
And S2, adding the H-type beta molecular sieve into the tobacco solution, stirring and filtering to obtain tobacco filtrate.
The H-type Beta molecular sieve is also called hydrogen-type Beta molecular sieve or Beta zeolite, has a unique three-dimensional twelve-membered ring pore canal system, and has huge adsorption capacity for nitrosamine.
In this step, an appropriate amount of the H-type beta molecular sieve is added to the tobacco solution, and the H-type beta molecular sieve is allowed to react with the tobacco solution sufficiently to adsorb nitrosamine under a proper temperature and stirring condition. And then separating the H-type beta molecular sieve from the tobacco solution through filtering operation to obtain tobacco filtrate with a large amount of nitrosamine removed.
The dosage of the H-type beta molecular sieve is 0.5-3% of the mass of the tobacco solution, and the dosage of the molecular sieve is reasonably controlled on the premise of ensuring the adsorption efficiency so as to reduce the production cost. And further in the H-type beta molecular sieve, the molar ratio between SiO 2 and Al 2O3 is 20-45:1. The molar ratio of SiO 2 to Al 2O3 refers to the number ratio of silicon atoms to aluminum atoms in the H-type beta molecular sieve, the ratio determines the framework structure and the pore size of the molecular sieve, and higher SiO 2 and Al 2O3 have larger pore sizes and higher silicon-aluminum ratio, so that a larger specific surface area and more adsorption sites can be provided, and the adsorption capacity of nitrosamine is enhanced. Meanwhile, the excessively high silicon-aluminum ratio is controlled to prevent the surface of the H-type beta molecular sieve from being excessively hydrophobic, so that the adsorption affinity of the H-type beta molecular sieve to nitrosamine is reduced. Therefore, the adsorption removal effect of the H-type beta molecular sieve on nitrosamine can be optimized in the silicon-aluminum ratio range.
After the H-type beta molecular sieve is added into the tobacco solution, the stirring parameters comprise the stirring temperature of 10-40 ℃, the stirring time of 0.5-2.0 hours and the stirring rotating speed of 300-800 r/min. The stirring process under the parameters can ensure that the tobacco solution is fully contacted with the H-type beta molecular sieve, promote the adsorption of nitrosamine in a free state, ensure the full dispersion of the solid phase of the H-type beta molecular sieve and improve the adsorption efficiency.
Further, the filtration may be carried out by filtration under reduced pressure through a 0.45 μm polypropylene filter. The polypropylene filter membrane is a commonly used microporous filter membrane, has good chemical stability and high mechanical strength, can effectively intercept most of solid particles, bacteria, viruses and other microorganisms in the tobacco solution, and simultaneously allows small molecular substances and dissolved tobacco components to pass through. And then the polypropylene filter membrane is adopted to filter the H-type beta molecular sieve which can intercept and adsorb nitrosamine, thus obtaining tobacco filtrate with much nitrosamine removed.
And S3, dynamically adsorbing the tobacco filtrate by a macroporous adsorption resin column, and performing gradient elution by using an ethanol aqueous solution to obtain a tobacco eluent.
In the step, the dynamic adsorption based on macroporous adsorption resin refers to the process that tobacco filtrate to be separated passes through an adsorption column at a certain flow rate so that target components (such as aroma components) in the tobacco filtrate and the resin are adsorbed. The specific operation comprises the steps of loading pretreated macroporous adsorption resin into an adsorption column (the volume of a column bed is 1-5 BV), ensuring uniformity and compactness of a resin layer, pumping tobacco filtrate into the adsorption column at a proper flow rate (1-3 BV/h), enabling components in the filtrate to be dynamically adsorbed with the resin, and adjusting conditions such as flow rate, temperature and the like according to requirements in the adsorption process so as to optimize the adsorption effect.
And eluting by using solvents with different concentrations sequentially at proper eluting flow rates (1-3 BV/h) so as to gradually wash off the components adsorbed on the resin. Among them, aqueous ethanol is a commonly used eluent, and the eluting power is gradually increased with the increase of the ethanol solubility. The volume fraction of the ethanol water solution used for elution is 0-95%. It can be understood that after the dynamic adsorption is completed, the low-concentration ethanol aqueous solution is used for eluting first to remove impurities and components easily desorbed from the resin, and then the concentration of the ethanol aqueous solution is gradually increased for gradient elution.
It should be noted that in the eluting process, the eluent is collected after eluting corresponding to each concentration of the eluent, and preferably, the eluent after eluting with ethanol of a certain concentration is selected to be mixed as a raw material for subsequent preparation. If the water washing part or the low-concentration ethanol elution part is omitted, the high-concentration ethanol elution part is collected, because the paste core substances are generally easy to concentrate on the water washing part or the low-concentration ethanol elution part, the risk of paste core of the electronic cigarette can be reduced in the actual use process of the tobacco refined product manufactured after the removal, and the stability is improved. And a small amount of nitrosamine is contained in the removed portion, so that the nitrosamine content in the eluate can be further removed. Preferably, the eluent with the volume fraction of 30-70% of the ethanol aqueous solution is mixed.
And S4, concentrating the tobacco eluent under reduced pressure to obtain concentrated solution, and blending the concentrated solution to obtain the refined tobacco product.
In this step, the concentrated solution of the tobacco active ingredient with higher concentration is obtained by concentrating under reduced pressure to remove most of the solvent (such as water and ethanol) in the tobacco eluent. It is noted that during the evaporation of the solvent at reduced pressure concentration, small amounts of nitrosamines may also be carried away to further reduce the nitrosamines content.
The heating evaporation may be performed under a condition lower than normal pressure using a device such as reduced pressure distillation or rotary evaporator. The reduced pressure can reduce the boiling point of the solvent, so that the evaporation process is carried out at a lower temperature, and the thermosensitive components in the tobacco are protected. Specifically, in this embodiment, the pressure of vacuum concentration adopts a step-by-step decompression mode, because the eluent has high ethanol concentration at the beginning and low boiling point, the evaporation efficiency can be ensured by relatively low temperature and vacuum degree, and as evaporation is performed, the ethanol concentration gradually decreases, the boiling point gradually increases, and the vacuum degree needs to be increased to ensure the evaporation efficiency. In the process of decompression concentration, the parameters are set to be that the pressure is 30-100 mbar and the temperature is 40-60 ℃.
Further blending to obtain the required tobacco refined product. The preparation process includes adding propylene glycol into the concentrated solution and mixing. Wherein the adding mass of the propylene glycol is 0.1-0.5 times of the mass of the concentrated solution. The propylene glycol is used as a common solvent and a humectant on one hand, can be used as a carrier to help dissolve and disperse active ingredients in tobacco, and simultaneously increases the wettability and taste of the product, so that the product is convenient for subsequent use, and has a bacteriostatic effect on the other hand, and can realize a preservative effect.
In conclusion, the nitrosamine content of the refined tobacco product prepared by the preparation method provided by the application is greatly removed, and a large amount of impurities such as easily burnt cores and the like are removed, so that aroma components are enriched. Furthermore, in further application, after the tobacco refined product prepared based on the application is prepared into the electronic cigarette atomized liquid, the problems of safety and stability existing when the tobacco extract is directly applied to electronic cigarette oil can be solved, peculiar smell is weakened, tobacco aroma is stronger, and user experience can be further improved.
The application further provides specific examples for preparing different types of tobacco refinements. Comprising the following steps:
Example 1
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 10 percent is added, and the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 6.30 percent according to YC/T145.9-2012 measurement. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2781.2g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing the pressure from 100mbar to 30mbar at 45 ℃ by using a rotary evaporator, concentrating until no condensate is present, obtaining 31.1g of concentrated solution, adding 6.2g of propylene glycol into the obtained concentrated solution, mixing and shaking uniformly to obtain refined burley tobacco.
Example 2
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with volume fraction of 1% is added, stirring and dissolving are carried out, thus obtaining the burley tobacco solution, and the total content of non-volatile components is 6.33% by referring to YC/T145.9-2012. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2775.4g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 45deg.C by rotary evaporator, concentrating until no condensate is present to obtain concentrated solution 30.2g, adding 6.0g propylene glycol into the obtained concentrated solution, mixing, and shaking to obtain refined burley tobacco product.
Example 3
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 5 percent is added, the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 6.31 percent according to YC/T145.9-2012 measurement. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2779.6g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 45deg.C by rotary evaporator, concentrating until no condensate is present to obtain concentrated solution 30.7g, adding 6.1g propylene glycol into the obtained concentrated solution, mixing, and shaking to obtain refined burley tobacco product.
Example 4
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 10 percent is added, and the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 6.30 percent according to YC/T145.9-2012 measurement. 45g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2773.5g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 45deg.C by rotary evaporator, concentrating until no condensate is present to obtain concentrated solution 30.9g, adding 6.2g propylene glycol into the obtained concentrated solution, mixing, and shaking to obtain refined burley tobacco product.
Example 5
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 10 percent is added, and the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 6.30 percent according to YC/T145.9-2012 measurement. 60g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 60:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2766.7g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 45deg.C by rotary evaporator, concentrating until no condensate is present to obtain concentrated solution 30.6g, adding 6.1g propylene glycol into the obtained concentrated solution, mixing, and shaking to obtain refined burley tobacco product.
Example 6
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 10 percent is added, and the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 6.30 percent according to YC/T145.9-2012 measurement. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 20:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2783.7g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing the pressure from 100mbar to 30mbar at 45 ℃ by using a rotary evaporator, concentrating until no condensate is present, obtaining 31.2g concentrate, adding 6.2g propylene glycol into the concentrate, mixing, and shaking to obtain refined burley tobacco.
Example 7
300G of burley tobacco extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 10 percent is added, and the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 6.30 percent according to YC/T145.9-2012 measurement. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 40:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2774.3g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 45deg.C by rotary evaporator, concentrating until no condensate is present to obtain 30.4g concentrate, adding 6.0g propylene glycol into the concentrate, mixing, and shaking to obtain refined burley tobacco product.
Example 8
300G of burley tobacco extract is taken and added into a 5L beaker, 5700g of ethanol water solution with the volume fraction of 10% is added, and the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 3.15% by referring to YC/T145.9-2012. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 5780.0g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 45deg.C by rotary evaporator, concentrating until no condensate is present to obtain 29.4g concentrate, adding 5.9g propylene glycol into the concentrate, mixing, and shaking to obtain refined burley tobacco product.
Example 9
300G of burley tobacco extract is taken and added into a 5L beaker, 4200g of ethanol water solution with the volume fraction of 10% is added, the burley tobacco solution is obtained by stirring and dissolving, and the total content of nonvolatile components is 4.20% by referring to YC/T145.9-2012. 30g of H-type beta molecular sieve is added into the obtained burley tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the burley tobacco solution is placed in a 20 ℃ water bath to be stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 4278.5g of tobacco filtrate.
And (3) taking 1300g of macroporous adsorption resin for dynamic adsorption, wherein the selected macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., the main material is crosslinked polystyrene, the specific surface area is 530m 2/g, the average pore diameter is 95 nm), and referring to the method of the manufacturer, loading the column for pretreatment, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 1BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing the pressure from 100mbar to 30mbar at 45 ℃ by using a rotary evaporator, concentrating until no condensate is present, obtaining 29.8g of concentrated solution, adding 6.0g of propylene glycol into the obtained concentrated solution, mixing and shaking uniformly to obtain refined burley tobacco.
Example 10
400G of Zimbabwe tobacco extract is taken and added into a 5L beaker, 3600g of ethanol water solution with the volume fraction of 20% is added, and then the Zimbabwe tobacco solution is obtained by stirring and dissolving, and the total amount of non-volatile components is 7.21% by referring to YC/T145.9-2012. Adding 40g of H-type beta molecular sieve into the obtained Zimbabwe tobacco solution, wherein the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 40:1, stirring for 2.0 hours at 500r/min in a water bath at 40 ℃, and decompressing and filtering by using a 0.45 mu m polypropylene filter membrane to obtain 3785.2g of Zimbabwe tobacco filtrate.
Taking 1320g of macroporous adsorption resin for dynamic adsorption, namely selecting macroporous adsorption resin YKDH332,332 with medium polarity (Tianjin allowed resin science and technology Co., ltd., main structure is crosslinked polystyrene, specific surface area is 450m 2/g, average pore diameter is 14 nm), and referring to the method of the manufacturer, loading the mixture into a column for pretreatment, wherein the volume of a column bed is about 2L. The tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by 1BV distilled water, 1BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol and 2BV95% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing pressure from 100mbar to 30mbar at 50deg.C by rotary evaporator, concentrating until no condensate is present to obtain 111.8g concentrate, adding 33.5g propylene glycol into the concentrate, mixing, and shaking to obtain Zimbabwe tobacco refined product.
Example 11
300G of aromatic tobacco extract is taken and added into a 10L stainless steel barrel, 5700g of ethanol water solution with the volume fraction of 30% is added, and the aromatic tobacco solution is obtained by stirring and dissolving, and the total amount of non-volatile components is 3.45% by referring to YC/T145.9-2012. 30g of H-type beta molecular sieve is added into the obtained aromatic tobacco solution, the silicon-aluminum ratio (SiO 2/Al2O3) in the H-type beta molecular sieve is 25:1, then the aromatic tobacco solution is placed in a water bath at 30 ℃ and stirred at 600r/min for 1.0 hour, and the aromatic tobacco solution is subjected to reduced pressure filtration through a 0.45 mu m polypropylene filter membrane to obtain 5836.4g of tobacco filtrate.
1320G of macroporous adsorption resin is adopted for adsorption [ in the embodiment, the macroporous adsorption resin is YKDH332 medium-polarity macroporous adsorption resin (Tianjin let-off resin technology Co., ltd., the main structure is crosslinked polystyrene, the specific surface area is 550m 2/g, the average pore diameter is 50 nm), and the column pretreatment is carried out by referring to the method of the manufacturer, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 3 BV/h, and then is dynamically eluted with 2BV distilled water, 2BV50% ethanol, 2BV70% ethanol and 2BV95% ethanol at the flow rate of 2 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing the pressure from 100mbar to 30mbar at 45 ℃ by using a rotary evaporator, concentrating until no condensate exists, obtaining 37.0g of concentrated solution, adding 3.7g of propylene glycol, and uniformly mixing to obtain the aromatic tobacco refined product.
Example 12
300G of cigar extract is taken and added into a 5L beaker, 2700g of ethanol water solution with the volume fraction of 5 percent is added, and the cigar solution is obtained by stirring and dissolving, and the total amount of non-volatile components is 6.95 percent according to YC/T145.9-2012. 45g of H-type beta molecular sieve is added into the cigar solution, the silicon-aluminum ratio (SiO 2/Al2O3) of the H-type beta molecular sieve is 40:1, then the cigar solution is placed in a water bath at 30 ℃ and stirred at 400r/min for 1.5 hours, and a 0.45 mu m polypropylene filter membrane is used for decompression filtration to obtain 2801.0g of tobacco filtrate.
1300G of macroporous adsorption resin is adopted for adsorption [ in the embodiment, macroporous adsorption resin is YKDH331 medium-polarity macroporous adsorption resin (Tianjin allowed resin technology Co., ltd., main structure is crosslinked polystyrene, specific surface area is 500m 2/g, average pore diameter is 14 nm), and the column pretreatment is carried out by referring to a manufacturer method, and the volume of a column bed is about 2L. The obtained tobacco filtrate is loaded and adsorbed at the flow rate of 1 BV/h, and then is dynamically eluted by using 1BV distilled water, 2BV30% ethanol, 2BV50% ethanol, 1BV70% ethanol and 1BV90% ethanol at the flow rate of 1 BV/h. Discarding distilled water eluent, mixing the other eluents, gradually reducing the pressure from 100mbar to 30mbar at 60 ℃ by using a rotary evaporator, concentrating until no condensate exists, obtaining 104g of concentrated solution, adding 31.2g of propylene glycol, and uniformly mixing to obtain cigar refined product.
The above are only some examples of the present application, and it is within the scope of the claimed application to prepare the tobacco refined product obtained. Wherein, based on the tobacco refined product prepared in the above example, effect verification is performed, comprising:
Effect verification experiment 1
Referring to the method for measuring the nitrosamine peculiar to the tobacco in the electronic atomized liquid of annex F of the technical Specification for electronic atomized liquid safety of T/CECC002-2021, the concentrations of nitrosamine in the tobacco solution, tobacco filtrate and tobacco refined product in the above 12 examples were measured by using a Wat-S4RM0970 liquid chromatograph-tandem mass spectrometer, respectively. And respectively calculating the TSNA concentration in the tobacco extract, the removal rate of TSNA of the molecular sieve adsorption section and the macroporous resin purification section and the total TSNA removal rate according to the formulas (1), (2), (3) and (4).
c = c1 × d (1)
η1 ＝ (m1c1-m2c2)/m1c1 × 100% (2)
η2 ＝ (m2c2-m3c3)/m1c1 × 100% (3)
η = η1 + η2 (4)
In the four formulas, c and c 1、c2、c3 are respectively the sum of the concentrations of four tobacco-specific nitrosamines in tobacco extract, tobacco solution, tobacco filtrate and tobacco refined product, the unit is mg/g, d is dilution factor, no unit is given, m 1、m2、m3 is the mass of the tobacco solution, the tobacco filtrate and the tobacco refined product, the unit is g, eta 1、η2 and eta are respectively the TSNA removal rate of a molecular sieve adsorption section, the TSNA removal rate of a macroporous resin purification section and the total TSNA removal rate, and the unit is percent. The mass, TSNA concentration and removal rate of each feed are shown in Table 1.
TABLE 1
According to the embodiment, through molecular sieve adsorption and macroporous resin purification treatment, the TSNA concentration in the refined tobacco is obviously reduced compared with that of the tobacco extract, namely c 3 < c, and the use safety of the electronic atomized liquid is improved. In addition, from the viewpoint of eta 1、η2, the beta molecular sieve adsorption section has remarkable removal effect on TSNA, and the removal rate of the TSNA is further increased through macroporous resin purification and subsequent concentration processes.
Effect verification experiment 2
The tobacco extract and the obtained tobacco refined product in each example were respectively formulated into an electronic cigarette atomized liquid, and were used as comparative examples and examples, respectively. In the electronic cigarette atomized liquid, the mass fraction of the tobacco extract or the tobacco refined product is 10%, the mass fraction of the Vegetable Glycerin (VG) is 40%, and the rest 50% is Propylene Glycol (PG). A8-station electronic cigarette smoking machine is used for carrying out core pasting test, and the specific method comprises the steps of carrying out sensory evaluation on whether core pasting is carried out before the machine is started, then carrying out machine pumping, wherein the pumping capacity of each mouth is 35mL, stopping pumping for 2 seconds and 10 seconds, carrying out sensory evaluation after each time of pumping for 100 mouths, and confirming whether core pasting phenomenon is caused or not, and carrying out total pumping for 500 mouths. The paste core test results are shown in table 2.
TABLE 2
As shown in the results of Table 2, the tobacco refined product has no core pasting phenomenon at the mouth of 500 times, and is obviously improved compared with the tobacco extract before refining. This is because not only TSNA is further discarded in the macroporous resin dynamic elution process, but also most of highly polar saccharides, proteins and other easily-caused core-pasting impurities can be eluted from the distilled water elution stage, so that the risk of core pasting is reduced. The states of the stuck core state and the non-stuck core state are schematically shown in fig. 2.
In addition to the TSNA test and the paste core test, a tissue professional evaluator performed sensory evaluation on the atomized liquid with 1% tobacco extract and 1% tobacco extract added, respectively. The sensory evaluation results of the tobacco extract and the tobacco purified product are shown in Table 3.
TABLE 3 Table 3
The evaluation results are consistent, and compared with the tobacco extract, the obtained tobacco refined product has the advantages of reduced sweet taste, obviously increased aroma intensity and more outstanding tobacco aroma characteristics, and is beneficial to the result that the aroma-causing components are enriched due to the removal of impurities in the tobacco extract.
The above description of the preferred embodiments of the present application should not be taken as limiting the scope of the application, but rather should be understood to cover all modifications, variations and adaptations of the present application using its general principles and the following detailed description and the accompanying drawings, or the direct/indirect application of the present application to other relevant arts and technologies.
Claims (10)
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