Tobacco extract, atomization liquid, and preparation method therefor and use thereof

Abstract

Disclosed in the present application are a tobacco extract, an atomization liquid, and a preparation method therefor and the use thereof. The preparation method for the tobacco extract comprises the following steps: subjecting a tobacco aqueous extract solution to thermal decomposition, an electrodialysis treatment and an adsorption treatment, so as to prepare the tobacco extract.

Description

Tobacco extracts, atomizing fluids, their preparation methods and applications

[0001] Related applications

[0002] This application claims priority to Chinese patent application filed on December 30, 2024, application number 2024119750836, entitled "Tobacco Extract, Atomizing Liquid and Preparation Method Thereof and Application Thereof", the entire contents of which are incorporated herein by reference. Technical Field

[0003] This application relates to the field of electronic atomization product technology, and in particular to tobacco extracts, atomizing liquids, their preparation methods and applications. Background Technology

[0004] Traditional e-liquids almost always contain residual or come into contact with ethanol, as ethanol is a crucial solvent in the preparation process. In the extraction stage, tobacco extract preparation processes mainly include solvent extraction, supercritical fluid extraction, molecular distillation, and percolation. Ethanol is commonly used as the extraction solvent in these processes. On the one hand, based on the principle of "like dissolves like," ethanol can better extract aroma components; on the other hand, ethanol can reduce the dissolution of large-molecule pasteurizing components. In the refining stage, polysaccharides and other large molecules are the primary pasteurizing factors in e-cigarettes. Adding high-concentration ethanol can effectively remove polysaccharides and other large molecules, thereby reducing the overall pasteurizing factors in the e-liquid. Therefore, ethanol is required in both the initial extraction and subsequent refining stages.

[0005] However, some people are allergic or sensitive to ethanol. For these individuals, the presence of ethanol residue or exposure in the nebulizer fluid is a key concern. Even after post-processing, the risk of ethanol residue remains once ethanol is used in the extraction or refining stages, making tobacco extracts obtained using ethanol extraction technology unsuitable for this group.

[0006] As an alternative to ethanol, other low-polarity chemical solvents such as diethyl ether and ethyl acetate can be used. However, if these solvents are not completely removed, they will increase the safety risks of the atomized liquid products.

[0007] Therefore, how to solve the problem of ethanol residue at its source, and provide tobacco extracts that are suitable for the lifestyles of people who are allergic or sensitive to ethanol, while ensuring efficacy and safety, is a problem worthy of attention. Summary of the Invention

[0008] Based on this, this application provides tobacco extract, atomizing liquid, preparation method thereon, and application.

[0009] The first aspect of this application provides a method for preparing a tobacco extract, comprising the following steps:

[0010] The tobacco extract was prepared by thermal decomposition, electrodialysis and adsorption treatment of the tobacco aqueous extract.

[0011] A second aspect of this application provides a method for preparing a tobacco extract, comprising the following steps:

[0012] The first tobacco aqueous extract was prepared by thermal decomposition, electrodialysis and adsorption treatment.

[0013] Take the second tobacco aqueous extract for H + The second tobacco extract was prepared by adsorption using a type cation exchange resin.

[0014] The tobacco extract is prepared by mixing the first tobacco extract with the second tobacco extract.

[0015] In some embodiments, one or more of the following characteristics are satisfied:

[0016] (1) The thermal decomposition includes at least one of pressure pyrolysis and dynamic pyrolysis;

[0017] (2) The adsorption material for the adsorption treatment includes at least one of molecular sieve and activated carbon.

[0018] In some embodiments, one or more of the following characteristics are satisfied:

[0019] (1) The conditions for the electrodialysis treatment include: voltage 10V-25V; current 2A-15A; treatment time 1h-4h;

[0020] (2) The conditions for the adsorption treatment include: the amount of adsorbent material used is 5%-100% of the mass of the material to be treated; the adsorption treatment time is 1h-48h; and the adsorption treatment temperature is 15℃-65℃.

[0021] (3) The conditions for pressurized pyrolysis include: pyrolysis temperature 110℃-380℃; pyrolysis pressure 0.3MPa-1MPa; pyrolysis time 2h-6h;

[0022] (4) The conditions for dynamic pyrolysis include: pyrolysis temperature 180℃-350℃; pyrolysis time 40min-80min;

[0023] Optionally, the conditions for dynamic pyrolysis include: 180℃-240℃, 10min-20min; 240℃-280℃, 10min-20min; 280℃-320℃, 10min-20min; and 320℃-350℃, 10min-20min.

[0024] In some embodiments, one or more of the following characteristics are satisfied:

[0025] (1) The H + Type cation exchange resins include strongly acidic cation exchange resins and / or weakly acidic cation exchange resins;

[0026] (2) The H + The adsorption conditions for type I cation exchange resins include: H + The amount of cation exchange resin used is 20%-200% of the filtrate mass; the adsorption time is 0.5h-24h; and the adsorption temperature is 15℃-65℃.

[0027] A third aspect of this application provides a tobacco extract prepared by the aforementioned method.

[0028] A fourth aspect of this application provides a tobacco extract having an ethanol content of <0.1 mg / g and an NNK content of <0.05 μg / g.

[0029] A fifth aspect of this application provides a tobacco extract, comprising a first tobacco extract; the method for preparing the first tobacco extract includes the following steps:

[0030] The first tobacco aqueous extract was prepared by thermal decomposition, electrodialysis and adsorption treatment.

[0031] In some embodiments, the tobacco extract further includes a second tobacco extract; the method for preparing the second tobacco extract includes:

[0032] Take the second tobacco aqueous extract for H + The second tobacco extract was prepared by adsorption using a type cation exchange resin.

[0033] In some embodiments, the mass ratio of the first tobacco extract to the second tobacco extract is 1:(0.2-3).

[0034] A sixth aspect of this application provides an atomizing liquid comprising the aforementioned tobacco extract.

[0035] In some embodiments, the atomizing liquid further includes nicotine, a matrix, and organic acids.

[0036] In some embodiments, the atomizing liquid comprises, by mass percentage: 1%-10% tobacco extract; 0.1%-2% nicotine; 0.5%-5% organic acids; and 83%-97% matrix.

[0037] In some embodiments, one or more of the following characteristics are satisfied:

[0038] (1) The organic acid includes at least one of benzoic acid, citric acid, cinnamic acid, fumaric acid, 2-ethylbutyric acid, acetic acid, lactic acid, acetylpropionic acid, malic acid, myristic acid, oxalic acid, and succinic acid;

[0039] (2) The matrix includes glycerol and / or propylene glycol.

[0040] The seventh aspect of this application provides an electronic atomization product, including the aforementioned tobacco extract or the aforementioned atomizing liquid. Attached Figure Description

[0041] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. The drawings are only for illustrating preferred embodiments and are not intended to limit this application. Throughout the drawings, the same reference numerals denote the same parts. In the drawings:

[0042] Figure 1 is a front view of the carbon buildup in the atomizing liquid corresponding to Comparative Example 1;

[0043] Figure 2 is a front view of carbon buildup in the atomizing liquid corresponding to Comparative Example 2;

[0044] Figure 3 is a front view of the carbon buildup in the atomizing liquid corresponding to the basic embodiment 1;

[0045] Figure 4 is a front view of the carbon buildup in the atomizing liquid corresponding to Example 1;

[0046] Figure 5 is a front view of the carbon buildup in the atomizing liquid corresponding to Example 4. Detailed Implementation

[0047] To facilitate understanding of this application, a more comprehensive description of the application will be provided below with reference to specific embodiments. Preferred embodiments of the application are given below. However, the application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of this application.

[0048] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0049] In this article, the technical features described in an open-ended manner include both closed technical solutions composed of the listed features and open technical solutions that include the listed features.

[0050] In this document, the terms “second” and “first” are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated.

[0051] In this document, numerical ranges are referred to as continuous unless otherwise specified, and include the minimum and maximum values ​​of the range, as well as every value between the minimum and maximum values. Furthermore, when a range refers to an integer, it includes every integer between the minimum and maximum values ​​of the range. Additionally, when multiple ranges are provided to describe a feature or characteristic, the ranges may be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges to which they are incorporated.

[0052] In this application, unless otherwise specified, the temperature parameters are permitted to be either constant-temperature treatment or variations within a certain temperature range. It should be understood that the constant-temperature treatment allows temperature fluctuations within the precision range of the instrument control. Fluctuations are permitted within ranges such as ±5℃, ±4℃, ±3℃, ±2℃, and ±1℃.

[0053] The first aspect of this application provides a method for preparing a tobacco extract, comprising the following steps:

[0054] The tobacco extract was prepared by thermal decomposition, electrodialysis and adsorption treatment of the tobacco aqueous extract.

[0055] The aroma components in tobacco are mainly lipid-soluble compounds such as esters, acids, aldehydes, hybrid compounds, alcohols, ketones, and phenols, which are easily soluble in ethanol. Therefore, ethanol is often used as the extraction solvent for tobacco to enrich these aroma components. However, the water-soluble polysaccharides and proteins in tobacco can lead to severe carbon buildup, which is detrimental to atomization. Therefore, while using water as the extraction solvent can solve the problem of ethanol residue, the resulting tobacco extract is not suitable for electronic atomization systems.

[0056] The tobacco extract of this application is prepared by pyrolysis, electrodialysis and adsorption of tobacco aqueous solution. Pyrolysis can enrich volatile aroma components and avoid the influence of large molecules such as polysaccharides and proteins, and reduce the generation of harmful substances such as tar. Electrodialysis can effectively remove ions and adsorption treatment can further purify tobacco extract and reduce the generation of nitrosamines. In the absence of ethanol residue and ethanol contact, the atomization performance and sensory experience of tobacco extract can be guaranteed at the same time, solving the problem of safety or use limitation of tobacco extract caused by ethanol residue or ethanol contact.

[0057] A second aspect of this application provides a method for preparing a tobacco extract, comprising the following steps:

[0058] The first tobacco aqueous extract was prepared by thermal decomposition, electrodialysis and adsorption treatment.

[0059] Take the second tobacco aqueous extract for H + The second tobacco extract was prepared by adsorption using a type cation exchange resin.

[0060] The tobacco extract is prepared by mixing the first tobacco extract with the second tobacco extract.

[0061] As described above, the first tobacco extract prepared by thermal decomposition, electrodialysis and adsorption treatment of the first tobacco aqueous extract can enrich volatile aroma components and avoid the influence of large molecules such as polysaccharides and proteins, thereby reducing the production of harmful substances such as tar. Electrodialysis can effectively remove ions, and adsorption treatment can further purify the tobacco extract and reduce the production of nitrosamines. This can simultaneously ensure the atomization performance and sensory experience of the tobacco extract.

[0062] The second tobacco aqueous extract was then subjected to H... + The second tobacco extract, prepared by adsorption with a type-3 cation exchange resin, is due to H... + Type II cation exchange resin can effectively remove macromolecules and ions such as polysaccharides and proteins from tobacco aqueous extracts, and also has good atomization performance and sensory experience.

[0063] The applicant found that although through H + Cation exchange resins can be used to treat tobacco aqueous extracts, or after pyrolysis and flavor enhancement, electrodialysis and adsorption can be used to effectively remove large molecules such as polysaccharides and proteins from the tobacco aqueous extracts, as well as harmful substances such as ions. This is beneficial for preparing tobacco extracts suitable for electronic atomization systems, and their performance is not inferior to that of tobacco extracts obtained by traditional ethanol extraction processes. However, the two differ in their performance in use. Furthermore, the combined use of the first and second tobacco extracts can further improve atomization performance and sensory experience. This may be because the combination of the two extracts results in a richer composition, which is beneficial for adjusting atomization performance and sensory experience.

[0064] As a specific example, the mass ratio of the first tobacco extract to the second tobacco extract can be 1:(0.2-3), such as 1:0.2, 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, etc. By adjusting the mass ratio of the first tobacco extract to the second tobacco extract, ideal atomization performance and sensory experience can be obtained.

[0065] In some embodiments, the thermal decomposition includes at least one of pressure pyrolysis and dynamic pyrolysis.

[0066] Understandably, the aforementioned thermal decomposition can achieve the enrichment of aroma-producing components. A common flavoring process is pyrolysis, which allows aroma-producing components such as esters, acids, aldehydes, hybrid compounds, alcohols, ketones, and phenols to volatilize. By collecting the volatiles, the aroma-producing components can be enriched. There are no special limitations on the flavoring process; it is sufficient to achieve the enrichment of aroma components.

[0067] In some embodiments, the adsorption material for the adsorption treatment includes at least one of molecular sieves and activated carbon.

[0068] Understandably, adsorbent materials can be selected individually or in combination. The selected adsorbent materials have a large specific surface area, which can adsorb and remove nitrogen-containing impurities, reduce harmful substances, and improve safety.

[0069] In some embodiments, one or more of the following features are satisfied:

[0070] (1) The conditions for the electrodialysis treatment include: voltage 10V-25V; current 2A-15A; treatment time 1h-4h;

[0071] (2) The conditions for the adsorption treatment include: the amount of adsorbent material used is 5%-100% of the mass of the material to be treated; the adsorption treatment time is 1h-48h; and the adsorption treatment temperature is 15℃-65℃.

[0072] (3) The conditions for pressurized pyrolysis include: pyrolysis temperature 110℃-380℃; pyrolysis pressure 0.3MP-1MPa; pyrolysis time 2h-6h;

[0073] (4) The conditions for dynamic pyrolysis include: pyrolysis temperature of 180℃-350℃; pyrolysis time of 40min-80min.

[0074] Understandably, the removal efficiency of ions and small molecule impurities can be adjusted by modifying the conditions of electrodialysis. Specifically, the voltage can be 10V, 11V, 12V, 13V, 14V, 15V, 20V, 25V, etc.; the current can be 2A, 4A, 6A, 8A, 10A, 12A, 14A, 15A, etc.; and the treatment time can be 1h, 2h, 3h, 4h, etc. During the electrodialysis process, water needs to be added, with a water-to-material volume ratio of (5-20):1. Specifically, the water-to-material volume ratio can be 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, 20:1, etc.

[0075] Understandably, the adsorption effect of nitrogen-containing components can be achieved by adjusting the adsorption treatment conditions. Specifically, the amount of adsorbent material used is 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 100% of the mass of the material to be treated; the adsorption treatment time is 1h, 5h, 10h, 15h, 20h, 25h, 30h, 35h, 40h, 45h, 48h; and the adsorption treatment temperature can be 15℃, 25℃, 35℃, 45℃, 55℃, 65℃.

[0076] Understandably, the volatility and enrichment of aroma-enhancing components can be adjusted by modifying the conditions of the aroma-enhancing process. Specifically, for pressure pyrolysis, the pyrolysis temperature can be 110℃, 150℃, 200℃, 250℃, 300℃, 350℃, or 380℃; the pyrolysis pressure can be 0.3MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, 0.9MPa, or 1MPa; and the pyrolysis time can be 2h, 3h, 4h, 5h, or 6h, etc. For dynamic pyrolysis, it can include segmented pyrolysis. Specifically, the conditions for dynamic pyrolysis include: 180℃-240℃, 10min-20min; 240℃-280℃, 10min-20min; 280℃-320℃, 10min-20min; and 320℃-350℃, 10min-20min.

[0077] Understandably, the dynamic pyrolysis also includes a heating phase, with conditions of 0℃-180℃ for 20min-30min.

[0078] In some embodiments, one or more of the following features are satisfied:

[0079] (1) The H + Type cation exchange resins include strongly acidic cation exchange resins and / or weakly acidic cation exchange resins;

[0080] (2) The H + The adsorption conditions for type I cation exchange resins include: H + The amount of cation exchange resin used is 20%-200% of the filtrate mass; the adsorption time is 0.5h-24h; and the adsorption temperature is 15℃-65℃.

[0081] Understandable, H +The cation exchange resin can be selected as a single type or in combination. For example, the strong acid cation exchange resin can be at least one of Tulsimer T-42H, 001×7, D001H, D061, D072, D072H and NKC-9; the weak acid cation exchange resin can be at least one of D113, D151, D152, 110 and 122. + Type II cation exchange resins can effectively remove macromolecules and ions such as polysaccharides and proteins, improving atomization performance and sensory experience.

[0082] Understandably, by adjusting H + The adsorption conditions of the H-type cation exchange resin can be adjusted to improve the purification effect on tobacco aqueous solutions and achieve the enrichment of aroma components. Specifically, H... + The amount of cation exchange resin used can be 20%, 40%, 60%, 80%, 100%, 120%, 140%, 160%, 180%, 200% of the filtrate mass, etc.; the adsorption time can be 0.5h, 1h, 5h, 10h, 15h, 20h, 24h, etc.; the adsorption temperature can be 15℃, 25℃, 35℃, 45℃, 55℃, 65℃, etc.

[0083] In some embodiments, the extraction processes for the tobacco aqueous extract, the first tobacco aqueous extract, and the second tobacco aqueous extract each include independently:

[0084] The step of mixing and extracting tobacco raw materials with water.

[0085] Understandably, there are no particular limitations on the extraction conditions of the tobacco aqueous extract, the first tobacco aqueous extract, and the second tobacco aqueous extract. However, by adjusting the extraction process, the effective dissolution of aroma components can be promoted. In some embodiments, the extraction conditions include: a material-to-liquid ratio of 1:4 g / mL to 1:20 g / mL; an extraction temperature of 60℃ to 110℃; an extraction time of 1 h to 4 h; and 1 to 3 extractions. Specifically, material-to-liquid ratios can be 1:4 g / mL, 1:6 g / mL, 1:8 g / mL, 1:10 g / mL, 1:12 g / mL, 1:14 g / mL, 1:16 g / mL, 1:18 g / mL, 1:20 g / mL, etc.; extraction temperatures can be 60℃, 70℃, 80℃, 90℃, 100℃, 110℃, etc.; extraction times can be 1 h, 2 h, 3 h, 4 h, etc.; and the number of extractions can be 1, 2, or 3.

[0086] Understandably, the extraction process of tobacco aqueous extract, first tobacco aqueous extract, and second tobacco aqueous extract may include a concentration step, which can reduce H+. +The amount of type cation exchange resin used. Concentration conditions may include 50℃-70℃, 50mbar-200mbar (solids content of 55%-65%).

[0087] A third aspect of this application provides a tobacco extract prepared by the aforementioned method.

[0088] The tobacco extract of this application simultaneously guarantees both the atomization performance and sensory experience of the tobacco extract, solving the safety or usability limitations of tobacco extracts caused by ethanol residue or contact with ethanol. The tobacco extract of this application can be used in atomizing liquids, is suitable for electronic atomization systems, and exhibits excellent atomization performance that is no less than that of tobacco extracts obtained through traditional ethanol extraction processes.

[0089] A fourth aspect of this application provides a tobacco extract having an ethanol content of <0.1 mg / g and an NNK content of <0.05 μg / g.

[0090] The tobacco extract of this application has no ethanol residue or contact with ethanol, and has an extremely low NNK content, exhibiting good safety. It is suitable for electronic atomization systems, with good atomization performance that is no inferior to tobacco extracts obtained through traditional ethanol extraction processes.

[0091] A fifth aspect of this application provides a tobacco extract, comprising a first tobacco extract; the method for preparing the first tobacco extract includes the following steps:

[0092] The first tobacco aqueous extract was prepared by thermal decomposition, electrodialysis and adsorption treatment.

[0093] In some embodiments, the tobacco extract further includes a second tobacco extract; the method for preparing the second tobacco extract includes:

[0094] Take the second tobacco aqueous extract for H + The second tobacco extract was prepared by adsorption using a type cation exchange resin.

[0095] In some embodiments, the mass ratio of the first tobacco extract to the second tobacco extract is 1:(0.2-3), such as 1:0.2, 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, etc.

[0096] A sixth aspect of this application provides an atomizing liquid comprising the aforementioned tobacco extract.

[0097] The atomizing liquid of this application does not produce a burnt taste, has a rich aroma, strong layering, and a clean aftertaste. It also has less carbon buildup, a large atomization volume, and a low smoke attenuation rate, providing a good sensory experience and atomization performance. Therefore, it not only meets the requirements of the alcohol-free atomizing liquid market but also ensures the consumer's experience.

[0098] In some embodiments, the atomizing liquid further includes nicotine, a matrix, and organic acids.

[0099] In some embodiments, the atomizing liquid comprises, by mass percentage: 1%-10% tobacco extract; 0.1%-2% nicotine; 0.5%-5% organic acids; and 83%-97% matrix.

[0100] Understandably, organic acids can be used as preservatives, flavoring agents, etc., in atomizing fluids, and there is no particular limitation on their specific types. In some embodiments, the organic acid includes at least one selected from benzoic acid, citric acid, cinnamic acid, fumaric acid, 2-ethylbutyric acid, acetic acid, lactic acid, levulinic acid, malic acid, myristic acid, oxalic acid, and succinic acid.

[0101] Understandably, the matrix can be glycerol or propylene glycol, preferably a combination of glycerol and propylene glycol, wherein the glycerol can be vegetable glycerin. In the combination of glycerol and propylene glycol, the mass ratio of glycerol to propylene glycol can be 1:(0.5-2).

[0102] The seventh aspect of this application provides an electronic atomization product, including the aforementioned tobacco extract or the aforementioned atomizing liquid.

[0103] Understandably, electronic atomization products can be electronic atomizing devices used to atomize a liquid into an aerosol for users to inhale. By choosing different liquids, effects such as reducing bad breath, freshening breath, refreshing the mind, and helping to maintain a comfortable state in the mouth and throat can be achieved. The atomization method is not limited; for example, it can be resistive atomization, electromagnetic atomization, ultrasonic atomization, or two-phase flow atomization. Specifically, electronic atomizing devices can be electronic cigarettes.

[0104] It is worth noting that the raw materials used in the embodiments of this application are all ordinary commercially available products, and their sources are not specifically limited.

[0105] Comparative Example 1

[0106] Preparation of tobacco ethanol extract:

[0107] 1) Crude extraction: Take tobacco leaves and crush them to 30 mesh, add ethanol solution for crude extraction (ethanol solution volume concentration is 60%, material-liquid ratio is 1:8g / mL, temperature: 81℃, time: 2h, extract twice in the same way), filter with a 200 mesh filter, take the filtrate and concentrate (60℃, 100mbar) to obtain crude extract.

[0108] 2) Refining: Add 95 v / v% ethanol to the crude extract at a volume ratio of crude extract to ethanol of 1:3, precipitate at -20℃ for 24 h, centrifuge at -20℃ and 8000 rpm, take the supernatant and concentrate (60℃, 100 mbar) to obtain tobacco ethanol extract, denoted as tobacco extract A.

[0109] Comparative Example 2

[0110] Preparation of crude tobacco water extract:

[0111] Take tobacco leaves, crush them to 30 mesh, add water for coarse extraction (material-to-liquid ratio 1:8 g / mL, temperature: 81℃, time: 2h, extract twice using the same method), filter through a 200 mesh filter, and concentrate the filtrate (60℃, 100mbar) to obtain crude tobacco water extract, denoted as tobacco extract B.

[0112] Basic Example 1

[0113] Preparation of the second tobacco extract:

[0114] Tobacco leaves were pulverized to 30 mesh, and coarsely extracted with water (material-to-liquid ratio 1:8 g / mL, temperature: 81℃, time: 2 h, extraction twice using the same method). The extract was filtered through a 200-mesh filter, and the filtrate was concentrated (60℃, 100 mbar) to obtain crude tobacco aqueous extract. 100% H2 solution (by weight of the crude tobacco aqueous extract) was added. + The second tobacco extract was obtained by adsorbing the cation exchange resin (Tulsimer T-42H) at 25°C for 12 hours and filtering it through a 200-mesh filter. It is denoted as tobacco extract C1.

[0115] Basic Implementation Example 2

[0116] Preparation of the second tobacco extract:

[0117] Tobacco leaves were pulverized to 30 mesh, and coarsely extracted with water (material-to-liquid ratio 1:4 g / mL, temperature: 60℃, time: 3 h, extraction twice using the same method). The extract was filtered through a 200-mesh filter, and the filtrate was concentrated (60℃, 100 mbar) to obtain crude tobacco aqueous extract. 100% H2 solution (by weight of the crude tobacco aqueous extract) was added. + The second tobacco extract was obtained by adsorbing the cation exchange resin (Tulsimer T-42H) at 35°C for 6 hours and filtering it through a 200-mesh filter. It is denoted as tobacco extract C2.

[0118] Basic Example 3

[0119] Preparation of the second tobacco extract:

[0120] Tobacco leaves were pulverized to 30 mesh, and coarsely extracted with water (material-to-liquid ratio 1:6 g / mL, temperature: 75℃, time: 2 h, extraction twice using the same method). The extract was filtered through a 200-mesh filter, and the filtrate was concentrated (60℃, 80 mbar) to obtain crude tobacco aqueous extract. 100% H2O (by weight of the crude tobacco aqueous extract) was added. + The second tobacco extract was obtained by adsorbing the cation exchange resin (Tulsimer T-42H) at 50°C for 4 hours and filtering it through a 200-mesh filter. It is designated as tobacco extract C3.

[0121] Example 1

[0122] Preparation of the first tobacco extract:

[0123] 1) Take tobacco leaves and crush them to 30 mesh, add water for coarse extraction (material-liquid ratio 1:8g / mL, temperature: 81℃, time 2h, extract twice in the same way), filter with a 200 mesh filter, take the filtrate and concentrate (60℃, 100mbar) to obtain crude tobacco water extract.

[0124] 2) Refining: The crude tobacco water extract was subjected to pressure pyrolysis under the following conditions: pyrolysis at 0.5 MPa and 140℃ for 3 hours, and the pyrolytes were collected. The pyrolytes were then subjected to electrodialysis treatment using an electrodialysis device under the following conditions: water to material volume ratio of 10:1, voltage of 12V, current of 6A, treatment for 3 hours, filtration through a 200-mesh filter, concentration (60℃, 100mbar), and after concentration, 10wt% zeolite (A5) was added for adsorption treatment for 4 hours, filtration through a 600-mesh filter, and concentration (60℃, 60mbar) to obtain the first tobacco extract, denoted as tobacco extract D1.

[0125] Example 2

[0126] Preparation of the first tobacco extract:

[0127] 1) Take tobacco leaves and crush them to 30 mesh, add water for coarse extraction (material-liquid ratio 1:10 g / mL, temperature: 60℃, time 2h, extract twice in the same way), filter with a 200 mesh filter, take the filtrate and concentrate (60℃, 100mbar) to obtain crude tobacco water extract.

[0128] 2) Refining: The crude tobacco water extract was subjected to pressure pyrolysis under the following conditions: pyrolysis at 0.6 MPa and 145℃ for 3 hours, and the pyrolytes were collected. The pyrolytes were then subjected to electrodialysis treatment using an electrodialysis device under the following conditions: water to material volume ratio of 10:1, voltage of 12V, current of 6A, treatment for 2 hours, filtration through a 200-mesh filter, concentration (60℃, 100mbar), and after concentration, 10wt% zeolite (A5) was added for adsorption treatment for 4 hours, filtration through a 600-mesh filter, and concentration (60℃, 60mbar) to obtain the first tobacco extract, denoted as tobacco extract D2.

[0129] Example 3

[0130] Preparation of the first tobacco extract:

[0131] 1) Take tobacco leaves and crush them to 30 mesh, add water for coarse extraction (material-liquid ratio 1:12 g / mL, temperature: 80℃, time 2h, extract twice in the same way), filter with a 200 mesh filter, take the filtrate and concentrate (60℃, 100mbar) to obtain crude tobacco water extract.

[0132] 2) Refining: The crude tobacco water extract was subjected to pressure pyrolysis under the following conditions: pyrolysis at 0.7 MPa and 150℃ for 3 hours, and the pyrolytes were collected. The pyrolytes were then subjected to electrodialysis treatment using an electrodialysis device under the following conditions: water to material volume ratio of 10:1, voltage of 12V, current of 6A, treatment for 2 hours, filtration through a 200-mesh filter, concentration (60℃, 100mbar), and after concentration, 10wt% zeolite (A5) was added for adsorption treatment for 4 hours, filtration through a 600-mesh filter, and concentration (60℃, 60mbar) to obtain the first tobacco extract, denoted as tobacco extract D3.

[0133] Example 4

[0134] Tobacco extract C1 from Basic Example 1 and tobacco extract D1 prepared in Example 1 were mixed at a mass ratio of 1:1 to obtain tobacco extract E1.

[0135] Example 5

[0136] Tobacco extract C2 from Basic Example 2 and tobacco extract D2 prepared in Example 2 were mixed at a mass ratio of 1:0.2 to obtain tobacco extract E2.

[0137] Example 6

[0138] Tobacco extract C3 from Basic Example 3 and tobacco extract D3 prepared in Example 3 were mixed at a mass ratio of 1:5 to obtain tobacco extract E3.

[0139] Application examples

[0140] Preparation of atomizing fluid:

[0141] The tobacco extracts from Comparative Examples 1-2, Basic Examples 1-3, and Examples 1-6 were used to prepare atomized liquids according to the following formulations: 5% tobacco extract, 2% nicotine, 2% benzoic acid, 41% glycerol (vegetable glycerin), and 50% propylene glycol.

[0142] Test case

[0143] 1. Sensory evaluation

[0144] Sensory evaluation was conducted on the atomizing liquid prepared for the corresponding use cases. The specific method was as follows: a three-stage inhalation evaluation method was adopted. Initial stage: first, smell the aroma to feel whether the atomizing liquid has an elegant aroma and whether the added fragrance can enhance the desire to inhale; take the first puff to feel the aroma upon entry, paying attention to the degree of aroma complexity and the stimulation to the oral and nasal cavities; then take two to three puffs within one minute to feel the aroma upon entry into the throat, paying attention to the reaction to throat stimulation and nasal cavity sensation; middle stage: inhale at a frequency of 10-30 seconds per puff, feeling the aroma through the nasal cavity, and feeling the sensation of the smoke in the oral cavity during inhalation and the sensation in the oral cavity during inhalation intervals. This stage mainly focuses on the aroma, aftertaste and other characteristics of the atomizing liquid; tail stage: when inhaling the tail stage, feel the off-flavors through the oral and nasal cavities; after inhaling, feel the oral cavity residue about 5 minutes later. A gentle, short-lived, light smoke flavor is more preferred. If it causes adverse reactions such as dryness and irritation in the throat, it indicates that there is a problem with the atomizing liquid. The results are shown in Table 1.

[0145] Table 1 Sensory evaluation results

[0146] As can be seen from Table 1, under the condition of no refining, the tobacco extract prepared by Comparative Example 1 using ethanol as the extraction solvent has better aroma, permeability and aftertaste than that prepared by Comparative Example 2 using water as the extraction solvent. The unrefined tobacco water extract has a poor sensory experience.

[0147] The first tobacco extract or the second tobacco extract prepared by using water as a solvent and refining through different routes in Basic Example 1 and Example 1 have a sensory experience comparable to Comparative Example 1, and Example 1 is superior to Basic Example 1. It can be seen that by using the preparation process of this application, a product with pure aroma, rising smoke and clean aftertaste can be produced without the participation of ethanol.

[0148] Example 4 was obtained by combining the second tobacco extract of Basic Example 1 and the first tobacco extract of Example 1. Its sensory score was better than that of Basic Example 1 and Example 1. It can be seen that the combined use of the second tobacco extract of Basic Example 1 and the first tobacco extract of Example 1 can have a synergistic effect and enrich the sensory experience.

[0149] 2. Ethanol residue and TSNA content

[0150] The results of ethanol residue and TSNA (detection of NNK content) in tobacco extract were obtained by liquid chromatography-tandem triple quadrupole mass spectrometry and gas chromatography, as shown in Table 2.

[0151] Table 2 Ethanol Residue and TSNA Content

[0152] According to the ethanol residue results, no ethanol was used or contacted with ethanol in the entire process of Basic Examples 1-3, Examples 1-6, and Comparative Example 2, and the ethanol residue was 0, which meets the requirements for alcohol-free atomizing liquid. In addition, the NNK content of Basic Examples 1-3 and Examples 1-6 was <0.05μg / g, which was significantly lower than that of Comparative Example 1-2. It can be seen that the preparation process of this application can significantly reduce the TSNA residue and has higher safety.

[0153] 3. Atomization performance

[0154] The atomization performance of the atomizing liquid used in the application example was tested as follows: The atomizing liquid was injected into the atomizer, equipped with a 6.5W battery, and the inhalation parameters were set as follows: 3 seconds of inhalation followed by 15 seconds of pause, with 200 puffs taken in total. The cartridge mass was recorded every 25 puffs. The atomization volume was calculated as follows: (200 puff cartridge mass - initial cartridge mass) / 200 = average atomization volume (mg / puff); atomization attenuation rate = [(0-25 puff average atomization volume) - (175-200 puff average atomization volume)] / (0-25 puff average atomization volume) × 100%. After recording the data, the atomizer core was removed, cut open, and photographed. The carbon buildup height was recorded under a microscope. The results are shown in Table 3. The front views of the carbon buildup in Comparative Examples 1-2, Basic Example 1, and Examples 1 and 4 are shown in Figures 1-5 respectively.

[0155] Table 3 Atomization Performance

[0156] As can be seen from Table 3, the traditional ethanol extraction process in Comparative Example 1 has better atomization performance than the water extraction process in Comparative Example 2, with less carbon buildup, less flue gas attenuation, and greater atomization volume. In other words, the traditional ethanol extraction process is more effective without refining.

[0157] Compared with Comparative Examples 1-2, the basic Examples 1-3 and Examples 1-3 have significantly better atomization performance, and Examples 1-3 also have a significant advantage in atomization performance compared with the basic Examples 1-3. It can be seen that the tobacco extract prepared by the preparation process of this application has better atomization performance.

[0158] Furthermore, Examples 4-6 were obtained by combining the second tobacco extract of Basic Examples 1-3 and the first tobacco extract of Examples 1-3, and they were superior in terms of carbon deposition, smoke attenuation, and atomization. It can be seen that the combined use of the second tobacco extract of Basic Examples 1-3 and the first tobacco extract of Examples 1-3 can synergistically enhance the atomization performance.

[0159] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0160] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this patent application should be determined by the appended claims.

Claims

1. A method for preparing a tobacco extract, comprising the following steps: The tobacco extract was prepared by thermal decomposition, electrodialysis and adsorption treatment of the tobacco aqueous extract.

2. A method for preparing a tobacco extract, comprising the following steps: The first tobacco aqueous extract was prepared by thermal decomposition, electrodialysis and adsorption treatment. Take the second tobacco aqueous extract for H + The second tobacco extract was prepared by adsorption using a type cation exchange resin. The tobacco extract is prepared by mixing the first tobacco extract with the second tobacco extract.

3. The preparation method according to claim 1 or 2, wherein, It meets one or more of the following characteristics: (1) The thermal decomposition includes at least one of pressure pyrolysis and dynamic pyrolysis; (2) The adsorption material for the adsorption treatment includes at least one of molecular sieve and activated carbon.

4. The preparation method according to claim 3, wherein, It meets one or more of the following characteristics: (1) The conditions for the electrodialysis treatment include: voltage 10V-25V; current 2A-15A; treatment time 1h-4h; (2) The conditions for the adsorption treatment include: the amount of adsorbent material used is 5%-100% of the mass of the material to be treated; the adsorption treatment time is 1h-48h; and the adsorption treatment temperature is 15℃-65℃. (3) The conditions for the pressurized pyrolysis include: pyrolysis temperature 110℃-380℃; pyrolysis pressure 0.3MPa-1MPa; pyrolysis time 2h-6h; (4) The conditions for dynamic pyrolysis include: pyrolysis temperature of 180℃-350℃; pyrolysis time of 40min-80min.

5. The preparation method according to claim 4, wherein, The conditions for dynamic pyrolysis include: 180℃-240℃, 10min-20min; 240℃-280℃, 10min-20min; 280℃-320℃, 10min-20min; and 320℃-350℃, 10min-20min.

6. The preparation method according to any one of claims 2-5, wherein, The H + Type cation exchange resins include strongly acidic cation exchange resins and / or weakly acidic cation exchange resins; And / or, the H + The adsorption conditions for type I cation exchange resins include: H + The amount of type cation exchange resin used is 20%-200% of the filtrate mass; The adsorption time is 0.5h-24h; the adsorption temperature is 15℃-65℃.

7. The tobacco extract prepared by the preparation method according to any one of claims 1-6.

8. A tobacco extract having an ethanol content of <0.1 mg / g and an NNK content of <0.05 μg / g.

9. A tobacco extract, comprising a first tobacco extract; the method for preparing the first tobacco extract comprises the following steps: The first tobacco aqueous extract was prepared by thermal decomposition, electrodialysis and adsorption treatment.

10. The tobacco extract of claim 9, further comprising a second tobacco extract; the method for preparing the second tobacco extract comprising: Take the second tobacco aqueous extract for H + The second tobacco extract was prepared by adsorption using a type cation exchange resin.

11. The tobacco extract of claim 10, wherein, The mass ratio of the first tobacco extract to the second tobacco extract is 1:(0.2-3).

12. An atomizing liquid comprising the tobacco extract according to any one of claims 7-11.

13. The atomizing liquid as described in claim 12, wherein, The atomizing fluid also includes nicotine, a matrix, and organic acids.

14. The atomizing liquid as described in claim 13, wherein, The atomizing liquid comprises, by mass percentage: 1%-10% tobacco extract; 0.1%-2% nicotine; 0.5%-5% organic acids; and 83%-97% matrix. And / or, the organic acid includes at least one of benzoic acid, citric acid, cinnamic acid, fumaric acid, 2-ethylbutyric acid, acetic acid, lactic acid, levulinic acid, malic acid, myristic acid, oxalic acid and succinic acid; And / or, the matrix comprises glycerol and / or propylene glycol.

15. An electronic atomization product comprising the tobacco extract according to any one of claims 7-11 or the atomizing liquid according to any one of claims 12-14.

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