Preparation method and application of tobacco refined product

Abstract

The invention discloses a preparation method and application of a tobacco refined product. The preparation method comprises the following steps: S1, dissolving and diluting a tobacco extract with 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 tobacco filtrate; s3, dynamically adsorbing the tobacco filtrate through a macroporous adsorption resin column, and carrying out gradient elution by using an ethanol water solution to obtain a tobacco eluent; and S4, concentrating the tobacco eluent under reduced pressure to obtain a concentrated solution, and blending the concentrated solution to obtain the tobacco refined substance. According to the technical scheme, through the steps, a large amount of nitrosamine can be adsorbed and removed based on the H-type beta molecular sieve in the step S2, a small amount of nitrosamine can be further removed in the step S3 and the step S4 in an auxiliary mode, and finally the tobacco refined matter with the low nitrosamine content is obtained. When the tobacco refined substance is applied to an electronic cigarette product, due to the low nitrosamine content, damage to a human body can be greatly reduced, and safety is improved.

Description

Technical Field

[0001] The present application relates to the technical field of electronic cigarettes, and in particular to a preparation method and application of a tobacco refined product. Background Art

[0002] Electronic cigarette atomizer liquid, also known as electronic cigarette oil, refers to a liquid mixture that can be atomized into an inhalable aerosol by electronic cigarette smoking devices. Its main ingredients are vegetable glycerin (VG), 1,2-propylene glycol (PG), nicotine salt, and edible flavors and fragrance additives. Reasonable selection of flavors and fragrances can make electronic cigarette oil present a variety of flavors, such as tobacco, fruit, herb, food, beverages and other flavors.

[0003] Among them, tobacco extract is an important flavor raw material in tobacco-flavored e-cigarette oil, which can present the natural tobacco flavor. However, in tobacco extract, nitrosamines (TSNA) are highly carcinogenic, mainly including strong carcinogens such as NNK, NNN, and NAB, which seriously endanger the physical and mental health of e-cigarette users. Summary of the invention

[0004] The present application provides a preparation method and application of a tobacco refined product, aiming to solve the problem that the existing tobacco extract has a high content of nitrosamines, which harms the physical and mental health of electronic cigarette users.

[0005] To achieve the above-mentioned purpose, the present application proposes a method for preparing a tobacco refined product. The preparation method comprises the following steps:

[0006] S1, dissolving and diluting tobacco extract by ethanol aqueous solution to obtain tobacco solution;

[0007] S2, adding powdered H-type β molecular sieve to the tobacco solution, stirring and filtering to obtain tobacco filtrate;

[0008] S3, dynamically adsorbing the tobacco filtrate through a macroporous adsorption resin column, and gradient eluting with an ethanol-water solution to obtain a tobacco eluate;

[0009] S4, concentrating the tobacco eluate under reduced pressure to obtain a concentrated solution, and then blending the concentrated solution to obtain a tobacco refined product.

[0010] In some embodiments, the tobacco extract includes flue-cured tobacco extract, oriental tobacco extract, burley tobacco extract and cigar tobacco extract.

[0011] In some embodiments, in step S1, the volume fraction of the ethanol aqueous solution is 0-30%, and the volume fraction of the total amount of non-volatile components in the obtained tobacco solution is 1-10%.

[0012] In some embodiments, the added mass of the H-type β molecular sieve is 0.5-3% of the mass of the tobacco solution; and the molar ratio between SiO2 and Al2O3 in the H-type β molecular sieve is 20-45:1.

[0013] In some embodiments, in step S2, the stirring temperature is 10-40°C, the stirring time is 0.5-2h, and the stirring speed is 300-800r / min.

[0014] In some embodiments, the specific surface area of ​​the macroporous adsorption resin is 450-550 m 2 / g, and the average pore size is 10-100nm.

[0015] In some embodiments, in gradient elution, the volume fraction of the ethanol aqueous solution is 0-95%, and the elution flow rate is 1-3 BV / h.

[0016] In some embodiments, during the reduced pressure concentration, the pressure is 30-100 mbar and the temperature is 40-60°C.

[0017] In some embodiments, the blending process includes: adding propylene glycol to the concentrate and mixing uniformly;

[0018] Wherein, the added mass of the propylene glycol is 0.1 to 0.5 times the mass of the concentrated solution.

[0019] The present application also proposes an application of the above tobacco refined product in an electronic cigarette.

[0020] The technical solution of the present application proposes 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 remove 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 further applied to electronic cigarette products, thanks to the low nitrosamine content, it can greatly reduce the harm to the human body and improve safety. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the prior art descriptions are briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative work, among which:

[0022] Figure 1 It is a structural schematic diagram of a method for preparing a tobacco refined product according to an embodiment of the present application.

[0023] Figure 2 This is the state diagram of the electronic cigarette after use in this application. Figure 2 In the figure, (a) is a schematic diagram of the state of the electronic cigarette with a sticky core after the tobacco refined material of the comparative example of the present application is used to prepare the electronic cigarette atomizer, and (b) is a schematic diagram of the state of the electronic cigarette with a sticky core after the tobacco refined material of the present application is used to prepare the electronic cigarette atomizer. DETAILED DESCRIPTION

[0024] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0025] See also Figure 1 As shown in the flow diagram, the present application proposes a method for preparing a tobacco refined product. The preparation method comprises the following steps:

[0026] Step S1, dissolving and diluting tobacco extract with ethanol aqueous solution to obtain tobacco solution.

[0027] Tobacco extract is a concentrate obtained after a series of extraction processes. It contains a variety of ingredients in tobacco, such as nicotine, tar, flavor substances, organic acids, alkaloids, etc. These ingredients exist in the tobacco extract in a dissolved or suspended state. The ethanol-water solution is a solution made by mixing ethanol and water in a certain proportion, which can be used as a solvent to dissolve and dilute the tobacco extract.

[0028] In this step, according to the proportion of non-volatile components in the tobacco extract, the proportion of non-volatile components in the tobacco solution obtained by dissolving and diluting 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 the range of 0 to 30%, so that the volume fraction of the total amount of non-volatile components in the tobacco solution finally dissolved and diluted is 1 to 10%. In this way, when the non-volatile components in the tobacco solution occupy a certain proportion, it is convenient to remove nitrosamines in the subsequent steps. It can be understood that the non-volatile components are in the concentration range of 1 to 10%, indicating that the tobacco extract is relatively fully dissolved, and the competitive adsorption phenomenon produced by the non-volatile components is relatively small, which is conducive to the subsequent specific adsorption of nitrosamines by the H-type β molecular sieve, and the non-volatile components are in the concentration range of 1 to 10%, which is conducive to balancing the adsorption quality and separation efficiency of the subsequent macroporous adsorption resin column.

[0029] A dissolving and diluting operation for tobacco extract is:

[0030] Select tobacco extract, put it into a beaker, then add ethanol aqueous solution of corresponding volume fraction, stir and dissolve to obtain tobacco solution with the above concentration of non-volatile components. Stirring can accelerate the dissolution and dilution of tobacco extract, and the stirring parameters can be set to stirring temperature of 10-40°C, stirring speed of 300-800r / min, and stirring time of 0.5-1.0 hour. The total amount of non-volatile components can be measured with reference to YC / T 145.9-2012.

[0031] In certain embodiments, tobacco extracts include flue-cured tobacco extracts, aromatic tobacco extracts, burley tobacco extracts and cigar extracts. Different types of extracts have unique flavors and chemical compositions. By selecting different extract types, a tobacco refined product with unique flavor and mouthfeel can be created accordingly.

[0032] Step S2, adding H-type β molecular sieve to the tobacco solution, stirring and filtering to obtain tobacco filtrate.

[0033] H-type β molecular sieve, also known as hydrogen-type Beta molecular sieve or Beta zeolite, has a unique three-dimensional twelve-membered ring pore system and has a huge adsorption capacity for nitrosamines.

[0034] In this step, the purpose is to add an appropriate amount of H-type β molecular sieve to the tobacco solution, and under appropriate temperature and stirring conditions, allow the H-type β molecular sieve to fully react with the tobacco solution to adsorb nitrosamines. Subsequently, the H-type β molecular sieve is separated from the tobacco solution by filtering to obtain a tobacco filtrate from which a large amount of nitrosamines have been removed.

[0035] Among them, the amount of H-type β molecular sieve is 0.5-3% of the mass of the tobacco solution. Under the premise of ensuring the adsorption efficiency, the amount of molecular sieve is reasonably controlled to reduce the production cost. And further in the H-type β molecular sieve, the molar ratio between SiO2 and Al2O3 is 20-45:1. Among them, the molar ratio of SiO2 and Al2O3 refers to the ratio of the number of silicon atoms and aluminum atoms in the H-type β molecular sieve. This ratio determines the skeleton structure and pore size of the molecular sieve. Higher SiO2 and Al2O3 have larger pores and higher silicon-aluminum ratios, which can provide larger specific surface area and more adsorption sites, and enhance the adsorption capacity of nitrosamines. At the same time, controlling the excessively high silicon-aluminum ratio prevents the surface of the H-type β molecular sieve from being too hydrophobic, reducing its adsorption affinity for nitrosamines. Therefore, within the silicon-aluminum ratio range, the adsorption and removal effect of the H-type β molecular sieve on nitrosamines can be optimized.

[0036] After adding H-type β molecular sieve to the tobacco solution, the stirring parameters are set as follows: stirring temperature 10-40°C, stirring time 0.5-2.0 hours, stirring speed 300-800 r / min. The stirring process under these parameters can make the tobacco solution fully contact with the H-type β molecular sieve, promote the adsorption of free nitrosamines; at the same time, ensure that the H-type β molecular sieve solid phase is fully dispersed, and improve the adsorption efficiency.

[0037] Furthermore, the filtering process can be: using a 0.45 μm polypropylene filter membrane to filter under reduced pressure. The polypropylene filter membrane is a commonly used microporous filter membrane with good chemical stability and high mechanical strength, which can effectively intercept most of the solid particles, bacteria, viruses and other microorganisms in the tobacco solution, while allowing small molecules and dissolved tobacco components to pass through. The polypropylene filter membrane is then used to filter the H-type β molecular sieve that can intercept and adsorb nitrosamines to obtain a tobacco filtrate in which nitrosamines are largely removed.

[0038] Step S3, dynamically adsorbing the tobacco filtrate through a macroporous adsorption resin column, and gradient eluting with an ethanol-water solution to obtain a tobacco eluate.

[0039] In this step, dynamic adsorption based on macroporous adsorption resin refers to the process in which the tobacco filtrate to be separated passes through the adsorption column at a certain flow rate, so that the target components (such as aroma components) in the tobacco filtrate are adsorbed by the resin. The specific operation includes: loading the pre-treated macroporous adsorption resin into the adsorption column (the column bed volume is 1 to 5 BV), and ensuring that the resin layer is uniform and tight, pumping the tobacco filtrate into the adsorption column at an appropriate flow rate (1 to 3 BV / h), so that the components in the filtrate are dynamically adsorbed by the resin, and during the adsorption process, the flow rate and temperature and other conditions can be adjusted as needed to optimize the adsorption effect.

[0040] Further, different concentrations of solvents are used to elute in sequence at an appropriate elution flow rate (1 to 3 BV / h) to gradually wash off the components adsorbed on the resin. Among them, ethanol aqueous solution is a commonly used eluent, and as the solubility of ethanol increases, the elution ability gradually increases. The volume fraction of ethanol aqueous solution used for elution in the present application is set to 0 to 95%. It can be understood that after the dynamic adsorption is completed, a low concentration of ethanol aqueous solution is first used for elution to remove impurities and components that are easily desorbed from the resin, and then the concentration of the ethanol aqueous solution is gradually increased for gradient elution.

[0041] It is worth noting that in the elution process, the eluate needs to be collected after elution corresponding to each concentration of eluent. Preferably, the eluate after elution with a certain concentration of ethanol is selected and mixed as the subsequent preparation raw material. For example, the water-washed part or the low-concentration ethanol elution part is discarded, and the high-concentration ethanol elution part is collected. This is because the substances that are easy to cause the core to stick are generally concentrated in the water-washed or low-concentration alcohol elution part. The tobacco refined product produced after discarding it can reduce the risk of electronic cigarette core sticking during actual use and improve stability. Moreover, a small amount of nitrosamines is contained in the discarded part, so that the nitrosamine content in the eluate can be further removed. Preferably, the eluate is mixed with ethanol-water solution at a volume fraction of 30 to 70%.

[0042] Step S4, the tobacco eluate is concentrated under reduced pressure to obtain a concentrated solution, and the concentrated solution is further blended to obtain a tobacco refined product.

[0043] In this step, the purpose is to remove most of the solvents (such as water and ethanol) in the tobacco eluate by decompression concentration, thereby obtaining a concentrated solution of a higher concentration of tobacco active ingredients. It is worth noting that in the solvent evaporation process of the decompression concentration, a small amount of nitrosamines can also be taken away to further reduce the content of nitrosamines.

[0044] Wherein, equipment such as vacuum distillation or rotary evaporator can be used to heat and evaporate under conditions below normal pressure. Decompression can reduce the boiling point of the solvent, so that the evaporation process is carried out at a lower temperature, protecting the heat-sensitive components in the tobacco. Specifically, in the present embodiment, the pressure of vacuum concentration adopts a step-by-step decompression method, because the ethanol concentration of the eluent is high at the beginning, the boiling point of the system is low, and a relatively low temperature and vacuum degree can ensure the evaporation efficiency. As the evaporation proceeds, the ethanol concentration gradually decreases, and the boiling point gradually increases, and the vacuum degree needs to be increased to ensure the evaporation efficiency. During the process of decompression concentration, the parameters are set as follows: the pressure is 30-100mbar, and the temperature is 40-60°C.

[0045] The desired tobacco refined product is further obtained through blending treatment. The blending treatment includes: adding propylene glycol to the concentrate and mixing evenly. Among them, the added mass of propylene glycol is 0.1 to 0.5 times the mass of the concentrate. On the one hand, propylene glycol is a commonly used solvent and humectant, which can be used as a carrier to help dissolve and disperse the active ingredients in tobacco, while increasing the wetness and taste of the product, making it convenient for subsequent use; on the other hand, it has an antibacterial effect and can achieve an antiseptic effect.

[0046] In summary, the nitrosamine content of the tobacco refined material prepared by the above preparation method of the present application is greatly removed, and a large number of impurities such as easy to stick to the core are removed, so that the aroma components are enriched. Furthermore, in further applications, after the tobacco refined material prepared based on the present application is formulated into an electronic cigarette atomizer, it can improve the safety and stability problems existing when the tobacco extract is directly applied to the electronic cigarette oil, and the odor is reduced, and the tobacco aroma is more intense, which can further improve the user experience.

[0047] The present application further proposes specific embodiments for preparing different types of tobacco refined products, including:

[0048] Example 1

[0049] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.30% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2781.2g of tobacco filtrate.

[0050] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar at 45°C using a rotary evaporator, and concentrated until there is almost no condensate, to obtain 31.1g of concentrated solution; 6.2g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0051] Example 2

[0052] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 1% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.33% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2775.4g of tobacco filtrate.

[0053] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar using a rotary evaporator at 45°C, and concentrated until there is almost no condensate, to obtain 30.2g of concentrated solution; 6.0g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0054] Example 3

[0055] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 5% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.31% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2779.6g of tobacco filtrate.

[0056] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar using a rotary evaporator at 45°C, and concentrated until there is almost no condensate, to obtain 30.7g of concentrated solution; 6.1g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0057] Example 4

[0058] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.30% according to YC / T145.9-2012. 45g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2773.5g of tobacco filtrate.

[0059] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar at 45°C using a rotary evaporator, and concentrated until there is almost no condensate, to obtain 30.9g of concentrated solution; 6.2g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0060] Example 5

[0061] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.30% according to YC / T145.9-2012. 60g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 60:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2766.7g of tobacco filtrate.

[0062] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar using a rotary evaporator at 45°C, and concentrated until there is almost no condensate, to obtain 30.6g of concentrated solution; 6.1g of propylene glycol is added to the obtained concentrated solution, and the mixture is mixed and shaken to obtain the refined burley tobacco.

[0063] Example 6

[0064] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.30% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 20:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2783.7g of tobacco filtrate.

[0065] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar using a rotary evaporator at 45°C, and concentrated until there is almost no condensate, to obtain 31.2g of concentrated solution; 6.2g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0066] Example 7

[0067] 300g of burley tobacco extract was added to a 5L beaker, and 2700g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 6.30% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 40:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2774.3g of tobacco filtrate.

[0068] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar at 45°C using a rotary evaporator, and concentrated until there is almost no condensate, to obtain 30.4g of concentrated solution; 6.0g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0069] Example 8

[0070] 300g of burley tobacco extract was added to a 5L beaker, and 5700g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 3.15% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 5780.0g of tobacco filtrate.

[0071] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar using a rotary evaporator at 45°C, and concentrated until there is almost no condensate, to obtain 29.4g of concentrated solution; 5.9g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0072] Example 9

[0073] 300g of burley tobacco extract was added to a 5L beaker, and 4200g of 10% ethanol aqueous solution was added, and the burley tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was determined to be 4.20% according to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained burley tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 20°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 4278.5g of tobacco filtrate.

[0074] 1300g of macroporous adsorption resin was taken for dynamic adsorption. [The macroporous adsorption resin selected was YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main material was cross-linked polystyrene, with a specific surface area of ​​530m 2 / g, average pore size 95nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 4BV10% ethanol, 2BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 1BV95% ethanol are used in sequence for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar at 45°C using a rotary evaporator, and concentrated until there is almost no condensate, to obtain 29.8g of concentrated solution; 6.0g of propylene glycol is added to the obtained concentrated solution, and the mixture is shaken to obtain the refined burley tobacco.

[0075] Example 10

[0076] 400g of Zimbabwe tobacco extract was added to a 5L beaker, and 3600g of 20% ethanol aqueous solution was added, and the Zimbabwe tobacco solution was obtained by stirring. The total amount of non-volatile components was 7.21% as determined by referring to YC / T145.9-2012. 40g of H-type β molecular sieve was added to the obtained Zimbabwe tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 40:1. The solution was stirred for 2.0 hours at 500r / min in a 40°C water bath, and 3785.2g of Zimbabwe tobacco filtrate was obtained by vacuum filtration with a 0.45μm polypropylene filter membrane.

[0077] 1320 g of macroporous adsorption resin was used for dynamic adsorption. [The selected macroporous adsorption resin is YKDH332 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main structure is cross-linked polystyrene, the specific surface area is 450m 2 / g, average pore size 14nm), refer to the manufacturer's method for column pretreatment, the column bed volume is about 2L. 】The tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then 1BV distilled water, 1BV30% ethanol, 1BV50% ethanol, 1BV70% ethanol, 2BV95% ethanol are used for dynamic elution at a flow rate of 1BV / hour. The distilled water eluent is discarded, and the remaining eluents are mixed. The pressure is gradually reduced from 100mbar to 30mbar at 50°C using a rotary evaporator, and concentrated until there is almost no condensate, and 111.8g of concentrated solution is obtained; 33.5g of propylene glycol is added to the obtained concentrated solution, and the mixture is mixed and shaken to obtain Zimbabwe tobacco refined material.

[0078] Embodiment 11

[0079] 300g of aromatic tobacco extract was added to a 10L stainless steel barrel, and 5700g of 30% ethanol aqueous solution was added, and the aromatic tobacco solution was obtained by stirring and dissolving. The total amount of non-volatile components was 3.45% as determined by referring to YC / T145.9-2012. 30g of H-type β molecular sieve was added to the obtained aromatic tobacco solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 25:1. Then, the solution was placed in a 30°C water bath and stirred at 600r / min for 1.0 hour, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 5836.4g of tobacco filtrate.

[0080] Take 1320g of macroporous adsorption resin for adsorption. [In this embodiment, the macroporous adsorption resin is YKDH332 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main structure is cross-linked polystyrene, specific surface area 550m 2 / g, average pore size 50nm), column pretreatment according to the manufacturer's method, column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 3BV / hour, and then dynamically eluted with 2BV distilled water, 2BV50% ethanol, 2BV70% ethanol, and 2BV95% ethanol at a flow rate of 2BV / hour. Discard the distilled water eluent, mix the remaining eluents, use a rotary evaporator at 45°C, gradually reduce the pressure from 100mbar to 30mbar, and concentrate until there is almost no condensate, to obtain 37.0g of concentrated liquid, add 3.7g of propylene glycol, mix evenly to obtain refined aromatic tobacco.

[0081] Example 12

[0082] 300g of cigar extract was added to a 5L beaker, and 2700g of 5% ethanol aqueous solution was added, and the cigar solution was obtained by stirring and dissolving. The total amount of non-volatile components was 6.95% as determined by referring to YC / T145.9-2012. 45g of H-type β molecular sieve was added to the obtained cigar solution, and the silicon-aluminum ratio (SiO2 / Al2O3) in the H-type β molecular sieve was 40:1. Then, the solution was placed in a 30°C water bath and stirred at 400r / min for 1.5 hours, and filtered under reduced pressure with a 0.45μm polypropylene filter membrane to obtain 2801.0g of tobacco filtrate.

[0083] 1300 g of macroporous adsorption resin was taken for adsorption. [In this embodiment, the macroporous adsorption resin is YKDH331 medium polar macroporous adsorption resin (Tianjin Yunkai Resin Technology Co., Ltd., the main structure is cross-linked polystyrene, specific surface area 500m 2 / g, average pore size 14nm), pre-treatment on the column according to the manufacturer's method, the column bed volume is about 2L. 】The obtained tobacco filtrate is adsorbed at a flow rate of 1BV / hour, and then dynamically eluted with 1BV distilled water, 2BV30% ethanol, 2BV50% ethanol, 1BV70% ethanol, and 1BV90% ethanol at a flow rate of 1BV / hour. Discard the distilled water eluent, mix the remaining eluents, use a rotary evaporator at 60°C, gradually reduce the pressure from 100mbar to 30mbar, and concentrate until there is almost no condensate, to obtain 104g of concentrated liquid, add 31.2g of propylene glycol, and mix evenly to obtain cigar tobacco refined product.

[0084] The above are only some embodiments of the present application. Within the parameter range of the present application, the tobacco refined products prepared are all within the protection scope of the present application. Among them, the tobacco refined products prepared based on the above embodiments are verified for their effects, including:

[0085] Effect verification experiment 1

[0086] With reference to Appendix F of T / CECC002-2021 "Technical Specifications for Safety of Electronic Atomization Liquids" for the determination method of tobacco-specific nitrosamines in electronic atomization liquids, the concentrations of nitrosamines in tobacco solutions, tobacco filtrates, and tobacco refined products in the above 12 examples were determined using a Watt-S4RM0970 liquid chromatography-tandem mass spectrometer. The TSNA concentration in tobacco extract, the TSNA removal rates in the molecular sieve adsorption section and the macroporous resin purification section, and the total TSNA removal rate were calculated according to formulas (1), (2), (3), and (4).

[0087] c = c1 × d (1)

[0088] η1 = (m1c1-m2c2) / m1c1 × 100% (2)

[0089] η2 = (m2c2-m3c3) / m1c1 × 100% (3)

[0090] η = η1 + η2 (4)

[0091] In the above four formulas, c, c1, c2, c3 are the sum of the concentrations of four tobacco-specific nitrosamines in tobacco extract, tobacco solution, tobacco filtrate and tobacco refined products, respectively, in mg / g; d is the dilution factor, without unit; m1, m2, m3 are the masses of tobacco solution, tobacco filtrate and tobacco refined products, respectively, in g; η1, η2, η are the TSNA removal rate of the molecular sieve adsorption section, the TSNA removal rate of the macroporous resin purification section, and the total TSNA removal rate, respectively, in %. The mass of each feed liquid, TSNA concentration and removal rate are shown in Table 1.

[0092] Table 1

[0093]

[0094]

[0095] From the above examples, it can be seen that after molecular sieve adsorption and macroporous resin purification, the TSNA concentration in the tobacco refined product is significantly lower than that in the tobacco extract, that is, c3 < c, which improves the safety of electronic atomization liquid. In addition, from the perspective of η1 and η2, the β molecular sieve adsorption stage has a significant removal effect on TSNA, and after macroporous resin purification and subsequent concentration process, the TSNA removal rate is further increased.

[0096] Effect verification experiment 2

[0097] The tobacco extract and the obtained tobacco refined product in each embodiment are respectively formulated into electronic cigarette atomization liquid, and are used as comparative examples and embodiments respectively. In the electronic cigarette atomization liquid, the mass fraction of tobacco extract or tobacco refined product is 10%, the mass fraction of vegetable glycerin (VG) is 40%, and the remaining 50% is propylene glycol (PG). An 8-station electronic cigarette smoking machine is used for the core sticking test. The specific method is: sensory evaluation before the machine is on whether the core is sticky, and then the machine is pumped, the suction capacity of each puff is 35mL, and the puff is stopped for 10 seconds after 2 seconds of puffing. After each 100 puffs, a sensory evaluation is performed to confirm whether the core sticking phenomenon occurs, and a total of 500 puffs are sucked. The results of the core sticking test are shown in Table 2.

[0098] Table 2

[0099]

[0100]

[0101] From the results in Table 2, it can be seen that the tobacco extract did not have a sticky core after 500 puffs, which is significantly improved compared to the tobacco extract before refining. This is because in the dynamic elution process of the macroporous resin, not only TSNA is further discarded, but also most of the impurities with high polarity such as sugars and proteins that are easy to cause sticking can be eluted from the distilled water elution stage, thereby reducing the risk of sticking. The state of sticking and not sticking is shown in the figure below. Figure 2 shown.

[0102] In addition to the TSNA test and the core paste test, professional smoking testers were also organized to conduct sensory evaluation on the atomized liquids with 1% tobacco extract and 1% tobacco refined products added respectively. The sensory evaluation results of tobacco extract and tobacco refined products are shown in Table 3.

[0103] Table 3

[0104]

[0105]

[0106] The evaluation results unanimously agreed that the obtained tobacco refined product had a weaker sweetness than tobacco extract, a significantly increased aroma intensity, and a more prominent tobacco aroma characteristic, which was due to the removal of impurities in the tobacco extract and the enrichment of the aroma components.

[0107] The above description is only a partial or preferred embodiment of the present application. Neither the text nor the drawings can limit the scope of protection of the present application. All equivalent structural changes made using the contents of the present application specification and drawings under the overall concept of the present application, or direct / indirect application in other related technical fields are included in the scope of protection of the present application.

Claims

1. A method for preparing a refined tobacco product, characterized in that: The preparation method comprises the following steps: S1, dissolving and diluting tobacco extract by ethanol aqueous 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 through a macroporous adsorption resin column, and gradient eluting with an ethanol-water solution to obtain a tobacco eluate; S4, concentrating the tobacco eluate under reduced pressure to obtain a concentrated solution, and then blending the concentrated solution to obtain a tobacco refined product.

2. The method for preparing a refined tobacco product according to claim 1, characterized in that: The tobacco extract includes flue-cured tobacco extract, spice tobacco extract, burley tobacco extract and cigar tobacco extract.

3. The method for preparing a refined tobacco product according to claim 1, characterized in that: In step S1, the volume fraction of the ethanol aqueous solution is 0-30%, and the volume fraction of the total amount of non-volatile components in the obtained tobacco solution is 1-10%.

4. The method for preparing a refined tobacco product according to claim 1, characterized in that: 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 between SiO2 and Al2O3 in the H-type beta molecular sieve is 20-45:

1.

5. The method for preparing a refined tobacco product according to claim 4, characterized in that: In step S2, the stirring temperature is 10-40°C, the stirring time is 0.5-2h, and the stirring speed is 300-800r / min.

6. The method for preparing a refined tobacco product according to claim 1, characterized in that: The specific surface area of ​​the macroporous adsorption resin is 450 to 550 m 2 / g, and the average pore size is 10-100nm.

7. The method for preparing a refined tobacco product according to claim 1, characterized in that: In the gradient elution, the volume fraction of the ethanol aqueous solution is 0-95%, and the elution flow rate is 1-3 BV / h.

8. The method for preparing a refined tobacco product according to claim 1, characterized in that: During the reduced pressure concentration, the pressure is 30 to 100 mbar and the temperature is 40 to 60°C.

9. The method for preparing a refined tobacco product according to claim 8, characterized in that: The preparation process includes: adding propylene glycol to the concentrated solution and mixing uniformly; Wherein, the added mass of the propylene glycol is 0.1 to 0.5 times the mass of the concentrated solution.

10. Use of the refined tobacco product according to any one of claims 1 to 9 in an electronic cigarette.

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