Adsorbent carrier material for supercritical co 2 extraction, tobacco extract, tobacco concentrate and preparation method therefor, and atomization matrix

Abstract

An adsorbent carrier material for supercritical CO2 extraction, comprising one or more of walnut shell, pecan shell and cocoa bean, each of which independently has a porous structure. The adsorbent carrier material has good permeability, facilitating sufficient contact between a tobacco extract and a CO2 fluid, and exhibits high compatibility with tobacco. In addition to acting as a tobacco extract adsorbent carrier, it can also enhance the intensity and richness of a characteristic tobacco aroma. In addition, after supercritical CO2 extraction using said adsorbent carrier material, the tobacco aroma is well-balanced, the smoke is natural, and there are no undesirable industrial odors or other off-flavors, improving tobacco aroma quality and increasing the application value of different tobacco extracts. Also disclosed are a tobacco extract, a tobacco concentrate and a preparation method therefor, and an atomization matrix.

Description

Adsorption carrier material for supercritical CO2 extraction, tobacco extract, tobacco concentrate, preparation method thereof and atomization substrate

[0001] The present application claims priority to the Chinese patent application No. 202411045614.1, filed on July 31, 2024, entitled "Adsorption carrier material for supercritical CO2 extraction, tobacco extract, tobacco concentrate, preparation method thereof and atomization substrate", the content of which is incorporated herein by reference in its entirety. TECHNICAL FIELD

[0002] The present application relates to the technical field of electronic cigarettes, and in particular to an adsorption carrier material for supercritical CO2 extraction, a tobacco extract, a tobacco concentrate, a preparation method thereof and an atomization substrate. BACKGROUND

[0003] With the improvement of consumers' health awareness, traditional cigarette products are subject to more and more regulatory restrictions. Electronic cigarettes, as one of the new types of tobacco products in recent years, have triggered a consumption boom worldwide.

[0004] Traditional tobacco flavor ingredients are usually extracted from tobacco leaves, redried tobacco leaves and tobacco waste. However, with the increasing regulation of tobacco leaves, tobacco extract is more easily obtained compared to tobacco leaves. However, the direct application of tobacco extract to electronic cigarettes brings adverse odors such as core paste and heavy odor, which affect the taste of electronic cigarettes. Therefore, it is necessary to re-separate the tobacco extract to meet the demand for atomization raw materials. SUMMARY

[0005] Based on this, the present application provides an adsorption carrier material for supercritical CO2 extraction, a tobacco extract, a tobacco concentrate, a preparation method thereof and an atomization substrate to re-separate the tobacco extract to meet the demand for atomization raw materials.

[0006] The first aspect of the present application provides an adsorption carrier material for supercritical CO2 extraction, the adsorption carrier material comprising one or more of walnut shells, quassia and cocoa beans, each of the walnut shells, the quassia and the cocoa beans independently having a pore structure.

[0007] In some embodiments, the adsorption carrier material comprises the walnut shells, the quassia and the cocoa beans.

[0008] In some embodiments, the adsorption carrier material comprises, in mass percentage: 10%-50% of the walnut shells, 10%-50% of the quassia and 10%-50% of the cocoa beans.

[0009] In some embodiments, the walnut shells have a water content <10% and a particle size ≤425 μm.

[0010] In some embodiments, the water content of the hickory wood is <10%, and the particle size is ≤425 μm.

[0011] In some embodiments, the water content of the cocoa bean is <10%, and the particle size is ≤425 μm.

[0012] A second aspect of the present application provides a tobacco extract material comprising the adsorption carrier material for supercritical CO2 extraction of the first aspect of the present application.

[0013] In some embodiments, the tobacco extract is further adsorbed on the surface and pore structure of the adsorption carrier material.

[0014] In some embodiments, the tobacco extract is further adsorbed on the surface and pore structure of the walnut shell, the surface and pore structure of the hickory wood, and the surface and pore structure of the cocoa bean.

[0015] In some embodiments, the tobacco extract comprises one or more of a pipe tobacco extract, a burley tobacco extract, and a cigar tobacco extract.

[0016] In some embodiments, the mass of the tobacco extract accounts for 20%-50% of the mass of the adsorption carrier material.

[0017] A third aspect of the present application provides a preparation method of a tobacco concentrate, comprising the following steps:

[0018] mixing the adsorption carrier material with the tobacco extract to prepare a tobacco extract material; the adsorption carrier material comprises one or more of a walnut shell, a hickory wood, and a cocoa bean, each of the walnut shell, the hickory wood, and the cocoa bean independently has a pore structure;

[0019] performing supercritical CO2 extraction on the tobacco extract material to prepare the tobacco concentrate.

[0020] In some embodiments, the process parameters of the supercritical CO2 extraction include: an extraction pressure of 25 MPa-35 MPa, an extraction temperature of 40°C-60°C, an extraction time of 3 h-5 h, a carrying agent comprising an ethanol aqueous solution with a volume fraction of 70%-90%, a pressure of separation kettle I of 5 MPa-8 MPa, and a pressure of separation kettle II of 5 MPa-8 MPa.

[0021] In some embodiments, the tobacco extract comprises one or more of a pipe tobacco extract, a burley tobacco extract, and a cigar tobacco extract.

[0022] In some embodiments, the mass of the tobacco extract accounts for 20%-50% of the mass of the adsorption carrier material.

[0023] The fourth aspect of the present application provides a tobacco concentrate prepared by the preparation method of the third aspect of the present application.

[0024] The fifth aspect of the present application provides an atomization substrate comprising the tobacco concentrate of the fourth aspect of the present application.

[0025] In some embodiments, the mass fraction of the tobacco concentrate in the atomization substrate is 0.5%-2%.

[0026] In some embodiments, the atomization substrate further comprises at least one of propylene glycol and glycerol.

[0027] The adsorption carrier material provided above for supercritical CO2 extraction includes walnut shells, hickory, and cocoa beans each having a pore structure. The adsorption carrier material has good permeability, which facilitates sufficient contact between the tobacco extract and the CO2 fluid. Moreover, the adsorption carrier material has high adaptability to tobacco, and can improve the strength and richness of characteristic tobacco aroma while serving as an adsorption carrier for tobacco extract. In addition, after supercritical CO2 extraction using the adsorption carrier material, the tobacco aroma is coordinated, the smoke is natural, and there is no industrial odor or other undesirable odor, which improves the quality of tobacco aroma and enhances the application value of different tobacco extracts. DETAILED DESCRIPTION

[0028] In order to facilitate the understanding of the present application, the present application will be described more fully below with reference to relevant embodiments. The following describes the preferred embodiments of the present application. However, the present application can be implemented in many different forms, and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present application more thorough and comprehensive.

[0029] 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 the present application belongs. The terms used in the specification of the present application are only for the purpose of describing the specific embodiments of the present application, and are not intended to limit the present application.

[0030] The selection range of the terms "and / or", "or / and", and "and / or" used herein includes any one of two or more related listed items, and also includes any and all combinations of related listed items, including any two related listed items, any more related listed items, or all related listed items. It should be noted that when at least three items are connected by at least two conjunctions selected from "and / or", "or / and", and "and / or", it should be understood that in the present application, the technical solution undoubtedly includes the technical solution connected by "logical and", and also undoubtedly includes the technical solution connected by "logical or".

[0031] In the present application, the open description of the technical features includes the closed technical solution consisting of the listed features, and also includes the open technical solution containing the listed features.

[0032] In the present application, if no special description is made, the numerical interval is considered to be continuous, and includes the minimum value and the maximum value of the range, and every value between the minimum value and the maximum value. Further, when the range refers to an integer, every integer between the minimum value and the maximum value of the range is included. In addition, when multiple ranges are provided to describe a feature or a characteristic, the ranges can be combined. In other words, unless otherwise indicated, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein.

[0033] Only some numerical ranges are specifically disclosed herein. However, any lower limit can be combined with any upper limit to form a range not explicitly recited; and any lower limit can be combined with other lower limits to form a range not explicitly recited, and likewise any upper limit can be combined with any other upper limit to form a range not explicitly recited. In addition, each individual disclosed point or single numerical value can itself be combined as a lower limit or an upper limit with any other point or single numerical value or with other lower limits or upper limits to form a range not explicitly recited.

[0034] In the present application, the temperature parameter, if not specifically limited, allows for constant temperature treatment, and also allows for treatment within a certain temperature range. The constant temperature treatment allows the temperature to fluctuate within the accuracy range controlled by the instrument. Fluctuation within a range such as ±5°C, ±4°C, ±3°C, ±2°C, ±1°C is allowed.

[0035] In the present application, the "suitable" in "suitable combination", "suitable manner", "any suitable manner" and the like means that the technical solution of the present application can be implemented, the technical problems of the present application can be solved, and the expected technical effects of the present application can be achieved.

[0036] In the present application, "further", "still further", "in particular" and the like are used for the purpose of description, indicating differences in content, but should not be understood as limiting the scope of protection of the present application.

[0037] In the present application, "optionally", "optional" and "optional" mean that it can or can not be present, i.e. it means to select either of the two parallel schemes of "have" or "have not". If there are multiple "optional" in a technical solution, unless otherwise specified, and there is no contradictory or mutual restrictive relationship, each "optional" is independent of each other.

[0038] In the description of the application, "multiple" means at least two, for example, two, three, etc., unless otherwise specifically limited.

[0039] All the embodiments and optional embodiments of the present application can be combined with each other to form new technical solutions if no special instructions are given. All the technical features and optional technical features of the present application can be combined with each other to form new technical solutions if no special instructions are given.

[0040] All the steps of the present application can be performed in sequence or randomly if no special instructions are given, and preferably are performed in sequence.

[0041] Compared with tobacco leaves, tobacco extract is easier to obtain, but the direct application of tobacco extract to electronic cigarettes causes bad breath such as core paste and heavy gas, which affects the taste of electronic cigarettes. Therefore, the tobacco extract needs to be re-separated to meet the demand of atomization raw materials.

[0042] Supercritical CO2 extraction, as a new extraction technology developed in the 1970s, is particularly suitable for the separation and extraction of bioactive substances and heat-sensitive substances due to its environmental protection, high extraction efficiency and low temperature. In recent years, it has been widely used in the tobacco flavor industry. Supercritical CO2 extraction separation technology is to use CO2 fluid in a supercritical state to fully contact and dissolve the substances to be separated, and then change the temperature or pressure to selectively extract the substances according to the polarity and boiling point of the extracted substances. Therefore, the full contact between CO2 fluid and the separated substances is beneficial to the extraction of target substances.

[0043] Traditional tobacco flavor components are usually extracted from tobacco leaves, redried tobacco leaves and tobacco waste. In supercritical CO2 extraction, tobacco leaves are crushed or cut into shreds and then contacted with CO2 fluid in a supercritical CO2 extraction kettle, and then the aroma components are efficiently extracted. However, tobacco extract is not conducive to full contact with CO2 fluid, resulting in incomplete extraction of tobacco aroma.

[0044] Based on the above problems, the present application uses one or more of plant raw materials such as walnut shells, hickory and cocoa powder to prepare a carrier material for supercritical CO2 extraction. The carrier material has good permeability, which is conducive to the full contact of tobacco extract with CO2 fluid, and the supercritical CO2 extract of the carrier material is coordinated with the tobacco aroma, which can improve the quality of tobacco aroma.

[0045] One or more embodiments of the present application provide an adsorption carrier material for supercritical CO2 extraction, which comprises one or more of walnut shells, hickory and cocoa beans, and the walnut shells, hickory and cocoa beans each independently have a pore structure.

[0046] Understandably, the adsorption carrier material for supercritical CO2 extraction provided by the present application includes walnut shell, hickory and cocoa bean respectively having a pore structure. The adsorption carrier material has good permeability, which is conducive to the full contact of tobacco extract with CO2 fluid. Moreover, the adsorption carrier material has high adaptability with tobacco, and can improve the strength and richness of characteristic tobacco aroma while serving as an adsorption carrier for tobacco extract. In addition, after supercritical CO2 extraction using the adsorption carrier material, the tobacco aroma is coordinated, the smoke is natural, and there is no industrial odor and other bad odors, thereby improving the quality of tobacco aroma and enhancing the application value of different tobacco extracts.

[0047] As a possible implementation, the adsorption carrier material includes walnut shell, hickory and cocoa bean.

[0048] In some optional implementations, the adsorption carrier material includes, in terms of mass percentage, 10%-50% of walnut shell, 10%-50% of hickory and 10%-50% of cocoa bean. When the content of walnut shell, hickory and cocoa bean in the adsorption carrier material is within the above range respectively, the tobacco concentrate prepared using the adsorption carrier has rich tobacco aroma, obvious nut characteristics, natural and delicate smoke, and good coordination of tobacco aroma without odor.

[0049] The mass percentage of walnut shell in the adsorption carrier material is 10%-50%; for example, it can be but is not limited to 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46%, 48%, 50% or a range between any two of the above values, etc.

[0050] The mass percentage of hickory in the adsorption carrier material is 10%-50%; for example, it can be but is not limited to 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46%, 48%, 50% or a range between any two of the above values, etc.

[0051] The mass percentage of cocoa bean in the adsorption carrier material is 10%-50%; for example, it can be but is not limited to 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46%, 48%, 50% or a range between any two of the above values, etc.

[0052] As a non-limiting example, the sum of the mass percentages of walnut shell, hickory and cocoa bean in the adsorption carrier material is 100%.

[0053] In some alternative embodiments, the walnut shell has a moisture content < 10% and a particle size < 425 μm. When the walnut shell has a moisture content and a particle size within the above ranges, the tobacco extract has a large adsorption capacity and good CO2 permeability after adsorption, which is conducive to the full contact between the tobacco extract and the CO2 fluid, thereby facilitating the improvement of the extraction efficiency of tobacco flavor components.

[0054] In some of the embodiments, the dogwood has a moisture content < 10% and a particle size < 425 μm. When the dogwood has a moisture content and a particle size within the above ranges, the tobacco extract has a large adsorption capacity and good CO2 permeability after adsorption, which is conducive to the full contact between the tobacco extract and the CO2 fluid, thereby facilitating the improvement of the extraction efficiency of tobacco flavor components.

[0055] In some of the embodiments, the dogwood has a moisture content < 10% and a particle size < 425 μm. When the dogwood has a moisture content and a particle size within the above ranges, the tobacco extract has a large adsorption capacity and good CO2 permeability after adsorption, which is conducive to the full contact between the tobacco extract and the CO2 fluid, thereby facilitating the improvement of the extraction efficiency of tobacco flavor components.

[0056] One or more embodiments of the present application provide a tobacco extraction material comprising the above-mentioned adsorption carrier material for supercritical CO2 extraction.

[0057] It should be noted that the above-mentioned "tobacco extraction material" refers to a material for supercritical CO2 extraction.

[0058] In some embodiments, the tobacco extract is further adsorbed on the surface and pore structure of the adsorption carrier material. In this way, the full contact between the tobacco extract and the CO2 fluid is facilitated.

[0059] In some alternative embodiments, the tobacco extraction material further comprises a tobacco extract, which is adsorbed on the surface and pore structure of the walnut shell, the surface and pore structure of the dogwood, and the surface and pore structure of the cocoa bean.

[0060] As a possible embodiment, the tobacco extract comprises one or more of a pipe tobacco extract, a burley tobacco extract, and a cigar tobacco extract.

[0061] In some optional embodiments, the mass of the tobacco extract is 20%-50% of the mass of the adsorption carrier material; for example, but not limited to, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46%, 48%, 50%, or a range between any two of the above values, etc. When the mass of the tobacco extract is within the above range of the mass of the adsorption carrier material, the tobacco concentrate produced has obvious smoke, prominent nutty flavor characteristics, significantly improved tobacco aroma richness and fullness, and better mouthfeel.

[0062] One or more embodiments of the present application provide a method for preparing a tobacco concentrate, comprising the following steps:

[0063] Mixing the adsorption carrier material with the tobacco extract to prepare a tobacco extraction material; the adsorption carrier material comprises one or more of walnut shells, hickory wood, and cocoa beans, each of the walnut shells, the hickory wood, and the cocoa beans independently having a pore structure; and supercritical CO2 extraction of the tobacco extraction material to prepare the tobacco concentrate.

[0064] The method for preparing the tobacco concentrate provided above has a simple process and low cost; the tobacco concentrate produced has high characteristic smoke intensity and richness, and has coordinated smoke aroma, natural smoke, and no industrial odor or other undesirable odors.

[0065] In some optional embodiments, the extraction pressure of the supercritical CO2 extraction is 25 MPa-35 MPa; for example, but not limited to, 25 MPa, 26 MPa, 27 MPa, 28 MPa, 29 MPa, 30 MPa, 31 MPa, 32 MPa, 33 MPa, 34 MPa, 35 MPa, or a range between any two of the above pressures, etc. When the extraction pressure is within the above range, the aroma components in the tobacco extract can be effectively extracted, while at the same time, the sugars, proteins, and other substances that are prone to causing the atomizer wick to be clogged can be effectively separated, so that the smoke aroma consistency and atomization performance of the tobacco concentrate are more stable.

[0066] As one possible embodiment, the extraction temperature of the supercritical CO2 extraction is 40℃-60℃; for example, but not limited to, 40℃, 41℃, 42℃, 43℃, 44℃, 45℃, 46℃, 47℃, 48℃, 49℃, 50℃, 51℃, 52℃, 53℃, 54℃, 55℃, 56℃, 57℃, 58℃, 59℃, 60℃, or a range between any two of the above temperatures, etc. When the extraction temperature is within the above range, the thermal-sensitive aroma components can be reduced or even avoided from undergoing intense chemical reactions due to high temperatures, thereby ensuring the smoke aroma reduction degree and smoke aroma stability.

[0067] In some example embodiments, the supercritical CO2 extraction has an extraction time of 3-5 hours; for example, but not limited to, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, or a range between any two of the foregoing, etc.

[0068] In some of the embodiments, the supercritical CO2 extraction has a carrier including an aqueous ethanol solution with a volume fraction of 70-90%; for example, but not limited to, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 70%, or a range between any two of the foregoing, etc. When the volume fraction of the aqueous ethanol solution is within the foregoing range, the aroma components in the tobacco extract can be better dissolved, and the tobacco aroma components can be more easily extracted. In addition, when the volume fraction of the aqueous ethanol solution is within the foregoing range, the main component extracted is tobacco absolute oil, which can effectively reduce or even avoid the extraction of more polar impurities, so that the richness of the tobacco extract is higher, and the smoking experience is better.

[0069] As a possible embodiment, the supercritical CO2 extraction has a pressure of 5-8 MPa in the separation kettle I; for example, but not limited to, 5 MPa, 6 MPa, 7 MPa, 8 MPa, or a range between any two of the foregoing, etc.

[0070] In some alternative embodiments, the supercritical CO2 extraction has a pressure of 5-8 MPa in the separation kettle II; for example, but not limited to, 5 MPa, 6 MPa, 7 MPa, 8 MPa, or a range between any two of the foregoing, etc.

[0071] As a non-limiting example, the pressure in the separation kettle I is greater than or equal to the pressure in the separation kettle II.

[0072] In some embodiments, the tobacco extract includes one or more of a pipe tobacco extract, a burley tobacco extract, and a cigar tobacco extract.

[0073] In some embodiments, the tobacco extract has a mass of 20-50% of the mass of the adsorption carrier material; for example, but not limited to, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46%, 48%, 50%, or a range between any two of the foregoing, etc.

[0074] One or more embodiments of the present application provide a tobacco concentrate prepared by the method described above.

[0075] The tobacco concentrate provided by the present application has high characteristic smoke intensity and richness, and the smoke is harmonious, natural and free of industrial odor.

[0076] One or more embodiments of the present application provide an atomized substrate comprising the tobacco concentrate provided above.

[0077] The single tobacco oil provided by the present application has prominent nut aroma, obvious cocoa aroma, delicate smoke aroma, natural smoke, rich aroma, high concentration and less oral residue.

[0078] The present application does not limit the amount of tobacco concentrate added to the atomized substrate. In some alternative embodiments, the mass fraction of the tobacco concentrate in the atomized substrate is 0.5%-2%; for example, it can be but is not limited to 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2% or a range between any two of the above mass fractions. When the amount of tobacco concentrate in the atomized substrate is within the above range, the atomized substrate has rich smoke aroma and obvious characteristic aroma, which can reduce the use cost while ensuring the smoke aroma.

[0079] In some alternative embodiments, the atomized substrate further comprises at least one of propylene glycol and glycerol.

[0080] The technical solutions of the present application are described in detail below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present application and do not limit the scope of the present application. If the specific conditions are not specified in the following examples, the experimental methods are preferred to be referred to the guidelines given in the present application, and can also be performed according to the experimental manuals or conventional conditions in the art, or according to the conditions suggested by the manufacturers, or by referring to the known experimental methods in the art.

[0081] In the following specific examples, the measurement parameters of the raw material components may have slight deviations within the weighing accuracy range if not otherwise specified. Acceptable deviations caused by instrument testing accuracy or operation accuracy are allowed for temperature and time parameters.

[0082] I. Preparation of tobacco concentrate

[0083] Example 1

[0084] Step S1, treatment and preparation of adsorption carrier material: wash walnut shells, hickory, cocoa beans, etc., and place them in a forced air drying oven, adjust the temperature to 60°C, and dry them until the moisture content of the walnut shells, hickory and cocoa beans is less than 10%, and then crush the walnut shells, hickory and cocoa beans through a 40-mesh sieve; mix them according to the mass fraction of 25% walnut shells, 25% hickory and 50% cocoa beans to prepare the adsorption carrier material.

[0085] Step S2, select the tobacco extract (SKME000161) as raw material, take 250g, with 500g of the adsorption carrier material prepared in step S1 for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 35MPa, extraction temperature 45℃, extraction time 4h, carrying agent is the volume fraction of 80% ethanol aqueous solution, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0086] Example 2

[0087] Step S1, adsorption carrier material processing and preparation: walnut shell, hickory, cocoa beans and the like are washed, placed in the air drying oven, the temperature is adjusted to 60℃, dried to the moisture content of walnut shell, hickory and cocoa beans is less than 10% respectively, and the walnut shell, hickory and cocoa beans are respectively crushed through 40 mesh sieve; according to the mass ratio of walnut shell is 30%, hickory mass ratio is 40%, cocoa beans mass ratio is 30%, mixed to prepare adsorption carrier material.

[0088] Step S2, select the tobacco extract (SKMB01020) as raw material, take 250g, with 500g of the adsorption carrier material prepared in step S1 for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 35MPa, extraction temperature 45℃, extraction time 4h, carrying agent is the volume fraction of 80% ethanol aqueous solution, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0089] Example 3

[0090] Step S1, adsorption carrier material processing and preparation: walnut shell, hickory, cocoa beans and the like are washed, placed in the air drying oven, the temperature is adjusted to 60℃, dried to the moisture content of walnut shell, hickory and cocoa beans is less than 10% respectively, and the walnut shell, hickory and cocoa beans are respectively crushed through 40 mesh sieve; according to the mass ratio of walnut shell is 30%, hickory mass ratio is 40%, cocoa beans mass ratio is 30%, mixed to prepare adsorption carrier material.

[0091] Step S2, select the tobacco extract (SKMB01020) as raw material, take 250g, with 500g of the adsorption carrier material prepared in step S1 for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 35MPa, extraction temperature 45℃, extraction time 4h, carrying agent is the volume fraction of 80% ethanol aqueous solution, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0092] Example 4

[0093] Step S1, adsorption carrier material processing and preparation: wash the walnut shell, hickory, cocoa beans and the like, and place them in a forced air drying oven, adjust the temperature to 60℃, dry until the moisture content of the walnut shell, hickory and cocoa beans is less than 10%, and then crush the walnut shell, hickory and cocoa beans through a 40-mesh sieve respectively; mix them according to the mass ratio of 50% walnut shell, 10% hickory and 40% cocoa beans to prepare the adsorption carrier material.

[0094] Step S2, select the white burley extract (SKMB01020) as the raw material, weigh 250g, and mix it with 500g of the adsorption carrier material prepared in step S1, then place it in a supercritical CO2 extraction kettle for extraction, with the extraction pressure being 35MPa, the extraction temperature being 45℃, the extraction time being 4h, the carrying agent being an ethanol aqueous solution with a volume fraction of 80%, the separation kettle I pressure being 7MPa, and the separation kettle II pressure being 5MPa, and then concentrate the extract under reduced pressure to remove ethanol to obtain a tobacco concentrate.

[0095] Example 5

[0096] Step S1, adsorption carrier material processing and preparation: wash the walnut shell, hickory, cocoa beans and the like, and place them in a forced air drying oven, adjust the temperature to 60℃, dry until the moisture content of the walnut shell, hickory and cocoa beans is less than 10%, and then crush the walnut shell, hickory and cocoa beans through a 40-mesh sieve respectively; mix them according to the mass ratio of 10% walnut shell, 45% hickory and 45% cocoa beans to prepare the adsorption carrier material.

[0097] Step S2, select the white burley extract (SKMB01020) as the raw material, weigh 250g, and mix it with 500g of the adsorption carrier material prepared in step S1, then place it in a supercritical CO2 extraction kettle for extraction, with the extraction pressure being 35MPa, the extraction temperature being 45℃, the extraction time being 4h, the carrying agent being an ethanol aqueous solution with a volume fraction of 80%, the separation kettle I pressure being 7MPa, and the separation kettle II pressure being 5MPa, and then concentrate the extract under reduced pressure to remove ethanol to obtain a tobacco concentrate.

[0098] Example 6

[0099] Step S1, adsorption carrier material processing and preparation: wash the walnut shell, hickory, cocoa beans and the like, and place them in a forced air drying oven, adjust the temperature to 60℃, dry until the moisture content of the walnut shell, hickory and cocoa beans is less than 10%, and then crush the walnut shell, hickory and cocoa beans through a 40-mesh sieve respectively; mix them according to the mass ratio of 25% walnut shell, 25% hickory and 50% cocoa beans to prepare the adsorption carrier material.

[0100] Step S2, select tobacco extract (SKME000161) as raw material, take 250g, with 1250g adsorption carrier material prepared in step S1 for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 25MPa, extraction temperature 40℃, extraction time 5h, carrying agent is 70% ethanol aqueous solution by volume fraction, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0101] Example 7

[0102] Step S1, adsorption carrier material treatment and preparation: walnut shell, hickory, cocoa beans and the like are washed, placed in the air drying oven, the temperature is adjusted to 60℃, dried to the moisture content of walnut shell, hickory and cocoa beans is less than 10% respectively, and the walnut shell, hickory and cocoa beans are respectively crushed through 40 mesh sieve; according to the mass ratio of walnut shell is 25%, hickory mass ratio is 25%, cocoa beans mass ratio is 50%, mixed to prepare adsorption carrier material.

[0103] Step S2, select tobacco extract (SKME000161) as raw material, take 250g, with 1000g adsorption carrier material prepared in step S1 for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 30MPa, extraction temperature 60℃, extraction time 3h, carrying agent is 90% ethanol aqueous solution by volume fraction, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0104] Comparative example 1

[0105] Select tobacco extract (SKME000161) as raw material, take 250g, with 500g silicon dioxide for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 35MPa, extraction temperature 45℃, extraction time 4h, carrying agent is 80% ethanol, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0106] Comparative example 2

[0107] Select tobacco extract (SKME000161) as raw material, take 250g, with 500g silicon dioxide for mixing, after mixing evenly, placed in supercritical CO2 extraction kettle for extraction, extraction pressure 35MPa, extraction temperature 45℃, extraction time 4h, carrying agent is 80% ethanol, separation kettle I pressure 7MPa, separation kettle II pressure 5MPa, the extract was concentrated by reducing pressure to remove ethanol to obtain tobacco concentrate.

[0108] II. Sensory evaluation and ingredient test

[0109] 1. Sensory smoking comparison experiment

[0110] The tobacco concentrate prepared in each of the above comparative examples and examples was added to a mixed solvent (99.5wt% solvent) of propylene glycol (PG) and glycerol (VG) in a mass ratio of 6:4 in an amount of 0.5wt% to obtain an electronic atomized tobacco oil. Sensory smoking was performed by 7 evaluators, and sensory evaluation was performed in terms of comfort, richness, stimulation, tobacco aroma, and offensive odor. The sensory evaluation was mainly based on GB5606.4-2005, and the following sensory evaluation was given in combination with the sensory characteristics of electronic cigarettes. The sensory smoking evaluation criteria are shown in Table 1, and the sensory evaluation results are shown in Table 2.

[0111] Table 1

[0112] Table 2

[0113] As can be seen from the results of Examples 1-7 and Comparative Examples 1-2 in Table 2, the tobacco concentrate prepared by the present application has significantly enhanced tobacco aroma, and significantly improved offensive odor, harmony, and aftertaste.

[0114] In Example 1, the tobacco extract retains the high satisfaction of pipe tobacco, while enhancing the nutty and cocoa aroma, and better coordinating the stimulating acid aroma in pipe tobacco, so that the overall aroma tends to be more like a burley tobacco and a cigar, thereby improving the application value and application range of pipe tobacco extract.

[0115] In Examples 2-5, the nutty and cocoa aroma is enhanced, and the burley tobacco characteristics are prominent. This shows that the supercritical CO2 extraction carrier material prepared from walnut shells, hickory, and cocoa beans can effectively enhance the tobacco aroma quality, improve the tobacco aroma aftertaste and harmony, and reduce the offensive odor, thereby effectively improving the product quality.

[0116] In Examples 6-7, by increasing the proportion of the adsorption carrier material, the tobacco aroma is slightly reduced, but the stimulation of pipe tobacco is significantly reduced, the smoke is softer, the aftertaste is significantly enhanced, and the overall aroma tends to be more like a burley tobacco.

[0117] 2. Comparison experiment of aroma components

[0118] The tobacco concentrate prepared in each of the above comparative examples and examples was added to a mixed solvent (99.5wt% solvent) of propylene glycol (PG) and glycerol (VG) in a mass ratio of 6:4 in an amount of 0.5wt% to obtain an electronic atomized tobacco oil.

[0119] 500 μL of the sample of the atomized substrate was taken in a centrifuge tube, 500 μL of dichloromethane solution containing an internal standard (the internal standard was 2-methyl-3-heptanone and 2-octanol at 10.0 mg / mL) was added, oscillation (3000 rpm) was performed for 10 min for sufficient extraction, then centrifugation (10000 rpm) was performed for 5 min, an appropriate amount of the extract was passed through a 0.24 μm organic phase filter membrane, and was moved to a chromatographic analysis bottle for GC-MS / MS analysis.

[0120] The determination of the aroma components of the extract was performed on a GC-MS / MS (model: Agilent 5977B GC / MSD 8890GC System), and the specific parameters were as follows: the chromatographic column was a DB-5MS ultra-high inert column (60 m, 0.25 mm, 0.25 μm); split injection 10:1; injection volume 1 μL; column oven temperature: 40°C for 2 min, increased to 150°C at 3°C / min, maintained for 2 min, increased to 300°C at 5°C / min, maintained for 1 min, increased to 320°C at 10°C / min, maintained for 1 min; MSD temperature 280°C; solvent delay 5.8 min; scan range: 35-550; threshold: 150; scan speed N=2; the mass spectrum was full scan; the data were compared with the NIST20 library, and each component was checked and determined.

[0121] The results of the above examples and comparative examples are shown in Table 3.

[0122] Table 3

[0123] It can be seen from the results in Table 3 that the nut aroma, cocoa aroma and roasted sweet aroma in Comparative Example 1 are not obvious; the nut aroma and cocoa aroma in Example 1 are relatively prominent, and the richness and harmony are better; in terms of aroma components, the nut aroma and cocoa aroma are mainly 2-methylpyrazine, 2,5-dimethylpyrazine, 2,3-dimethylpyrazine, 2,3,5-trimethylpyrazine, 5-methyl-2-acetylfuran, furan and other pyrazine and furan substances; the roasted sweet aroma substances are mainly furfural, 5-hydroxymethylfurfural, 2-ethyl-6-methylpyrazine, 5-methylfurfural and other pyrazine, aldehyde and phenol substances.

[0124] In summary, the adsorption carrier material provided in the application is conducive to the full contact of the tobacco extract with CO2 fluid; and the adsorption carrier material has high adaptability with tobacco, can improve the strength and richness of the characteristic tobacco aroma while serving as an adsorption carrier for the tobacco extract. In addition, after supercritical CO2 extraction using the adsorption carrier material, the tobacco aroma is harmonious, the smoke is natural, and there is no industrial odor and other bad odors, which improves the quality of the tobacco aroma and improves the application value of different tobacco extracts.

[0125] Any combination of the technical features in the above-described embodiments can be made, and for the sake of brevity, not all possible combinations are described, however, as long as there is no conflict, any combination of the technical features should be considered within the scope of the present disclosure.

[0126] The above-described embodiments only express several implementation manners of the present application, and the description is relatively specific and detailed, but it should not be understood as a limitation on the patent scope of the present application. It should be pointed out that, for ordinary skilled persons in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the patent protection scope of the present application should be subject to the appended claims.

Claims

1. An adsorption carrier material for supercritical CO2 extraction, the adsorption carrier material comprising one or more of walnut shell, hickory wood and cocoa bean, each of the walnut shell, the hickory wood and the cocoa bean independently having a pore structure.

2. The adsorbent support material of claim 1, wherein, The adsorption carrier material comprises the walnut shell, the hickory wood and the cocoa bean.

3. The adsorbent support material of any of claims 1-2, wherein, The adsorption carrier material comprises, in mass percentage, 10%-50% of the walnut shell, 10%-50% of the hickory wood and 10%-50% of the cocoa bean.

4. The adsorbent support material of any one of claims 1 to 3, wherein, The walnut shell has a water content of <10% and a particle size of ≤425μm.

5. The adsorbent support material of any one of claims 1 to 4, wherein, The hickory wood has a water content of <10% and a particle size of ≤425μm.

6. The adsorbent support material of any one of claims 1 to 5, wherein, The cocoa bean has a water content of <10% and a particle size of ≤425μm. 7.A tobacco extract comprising the adsorption carrier material for supercritical CO2 extraction according to any one of claims 1 to 6.

8. The tobacco extract of claim 7, wherein, The tobacco extract further comprises a tobacco extractive adsorbed on the surface and the pore structure of the adsorption carrier material.

9. The tobacco extract of any one of claims 7 to 8, wherein, The tobacco extractive comprises one or more of a pipe tobacco extractive, a burley tobacco extractive and a cigar tobacco extractive.

10. A tobacco extract as claimed in any one of claims 7 to 9 wherein, The mass of the tobacco extractive accounts for 20%-50% of the mass of the adsorption carrier material. 11.A method for preparing a tobacco concentrate, comprising the following steps: mixing an adsorption carrier material with a tobacco extractive to prepare a tobacco extractive material, the adsorption carrier material comprising one or more of walnut shell, hickory wood and cocoa bean, each of the walnut shell, the hickory wood and the cocoa bean independently having a pore structure; subjecting the tobacco extractive material to supercritical CO2 extraction to prepare the tobacco concentrate.

12. The production method according to claim 11, wherein The process parameters of the supercritical CO2 extraction comprise an extraction pressure of 25MPa-35MPa, an extraction temperature of 40℃-60℃, an extraction time of 3h-5h, a carrying agent comprising an ethanol aqueous solution with a volume fraction of 70%-90%, a pressure of separation kettle I of 5MPa-8MPa and a pressure of separation kettle II of 5MPa-8MPa.

13. The production method according to any one of claims 11 to 12, wherein The tobacco extractive comprises one or more of a pipe tobacco extractive, a burley tobacco extractive and a cigar tobacco extractive.

14. The production method according to any one of claims 11 to 13, wherein The mass of the tobacco extractive accounts for 20%-50% of the mass of the adsorption carrier material. 15.A tobacco concentrate prepared by the method according to any one of claims 11 to 14. 16.An atomization substrate comprising the tobacco concentrate according to claim 15.

17. The aerosolizing substrate of claim 16 wherein, The mass of the tobacco concentrate in the atomization substrate accounts for 0.5%-2%.

18. The aerosolizing substrate of claim 17 wherein, The atomization substrate further comprises at least one of propylene glycol and glycerol.

Images