Tobacco extract, preparation method thereof and application of tobacco extract in electronic cigarette atomized liquid

Abstract

The invention provides a tobacco extract, a preparation method of the tobacco extract and application of the tobacco extract in electronic cigarette atomized liquid, and belongs to the technical field of electronic cigarettes. The method comprises the following steps: step 1, carrying out moisture regaining fermentation treatment on tobacco leaves of the tobacco, baking and crushing; 2, extracting the tobacco leaves crushed in the step 1 to obtain extract liquor; and step 3, carrying out segmented rectification on the extract liquid, and compounding rectified materials of all rectification segments to obtain the tobacco extract. When the tobacco extract prepared by the preparation method provided by the invention is applied to atomized liquid, the tobacco flavor concentration and satisfaction can be increased, the problems of solubility, carbon deposition, easiness in core pasting and the like are solved, and the smoking experience of a user is effectively enhanced.

Description

Technical Field

[0001] The invention belongs to the technical field of electronic cigarettes, and in particular relates to a dry tobacco extract and a preparation method thereof and application thereof in electronic cigarette atomizer liquid. Background Art

[0003] The prior art provides some methods for preparing dry tobacco extracts so that dry tobacco can be used in electronic cigarettes. For example, patent CN114209085A provides a dry tobacco extract, which is extracted after flexible carbonization of dry tobacco; patent CN118975691A provides a method for preparing dry tobacco extract, which uses solvent steam to directly extract dry tobacco shreds by dry distillation, and then compound the reflux component and the distillate component. However, the dry tobacco extracts of the above methods are prepared by a single method, and often have insufficient layering, balance and concentration of aroma, which is not conducive to improving the smoking experience; and the solubility in the atomizing liquid solvent is general, which easily causes the core to become sticky and carbonized; and the extracts often contain more macromolecular substances such as sugars and pigments, and thus perform poorly in storage stability. Summary of the invention

[0004] In order to solve the above problems, the present application aims to provide a method for preparing a dry tobacco extract and its application in an atomized liquid. The preparation method provided by the present invention is simple to operate, easy to implement and low in price. The present invention adopts a preparation method of high-temperature extraction reaction followed by distillation and enrichment in a distillation tower, which can increase the concentration of tobacco aroma and satisfaction, and the dry tobacco extract prepared by using an atomizer directly as a reaction solvent is applied in an atomized liquid, which can solve solubility, carbon deposition, easy sticking of the core, etc., and effectively enhance the user's smoking experience.

[0005] In one aspect, the present application provides a method for preparing a dry tobacco extract, the method comprising the following steps:

[0006] Step 1, subjecting the dry tobacco leaves to moisture conditioning, fermentation, baking and crushing;

[0007] Step 2, extracting the crushed dry tobacco leaves in step 1 to obtain an extract;

[0008] Step three, distilling the extract in sections, and compounding the distillates from each distillation section to obtain the dry tobacco extract.

[0009] In one embodiment, in step 1, the conditions for moisture conditioning and fermentation are: the amount of water added is 10% to 50% of the weight of the tobacco leaves, and the moisture conditioning is carried out in a closed environment at room temperature for 48 to 60 hours.

[0010] Among them, when dry tobacco leaves are fermented, macromolecular substances such as starch, protein and vitamins will decompose and transform, gradually forming aldehydes, alcohols, ammonia and other substances that have adverse effects on dry tobacco smoking. These substances are volatile. Using the above conditions for rehumidification fermentation can remove the green smell and fat smell of dry tobacco leaves, mellow the tobacco leaves, and improve the sensory quality.

[0011] In one embodiment, the baking conditions are: baking at 70° C. to 250° C. for 10 min to 300 min.

[0012] Among them, baking can increase pyrrole, pyridine, and pyrazine substances through caramelization reaction, purify tobacco leaves, give dry tobacco leaves baking fragrance, and increase tobacco aroma. For example, during the baking process, chlorophyll and carotene are degraded quickly and thoroughly, avoiding the presence of green impurities. The aroma substances such as neophytadiene, cypermethrin, and phenylalanine increase, increasing the tobacco aroma effect.

[0013] At the same time, after the rehumidification, fermentation and baking treatments, it is more conducive to reducing the dissolution of impurities in the dry tobacco leaves during the subsequent extraction and increasing the solubility of aroma substances in the atomizing liquid solvent, thereby further improving the purity of the distillate during distillation, retaining the aroma substances while significantly improving their solubility in the atomizing solvent, which is beneficial to improving carbon deposition and core sticking and improving storage stability.

[0014] In one embodiment, the tobacco leaves are ground into 10-30 meshes after baking. The ground tobacco leaves can enlarge the specific surface area, facilitate the dissolution of aroma substances in the tobacco leaves, and improve the reaction efficiency.

[0015] In one embodiment, in step 2, the extraction conditions are: using 50% to 200% of the extractant based on the weight of the tobacco leaves, extracting at 90° C. to 400° C. for 30 to 300 minutes.

[0016] In one embodiment, the extractant is selected from one or more of propylene glycol, glycerol, ethanol, and water.

[0017] Among them, the aroma components in tobacco leaves can be directly dissolved in solvents such as propylene glycol and glycerin. After high-temperature heating, the macromolecular aroma substances in the aroma components are decomposed into small molecular aroma substances such as olefins and organic acids that are well soluble and easy to release.

[0018] In one embodiment, the added amount of 95% ethanol is 100% to 200%, the added amount of propylene glycol is 50% to 100%, and the added amount of glycerol is 50% to 100%.

[0019] In one embodiment, in step three, the vacuum degree of distillation is 30-300 Pa, and the heating temperature is 60-300° C.

[0020] In one embodiment, in step three, the staged distillation is two to five stage distillation, preferably four stage distillation.

[0021] Among them, the distillation method can enrich the aroma components of dry tobacco extract and increase the aroma concentration of the extract. The segmented distillation can effectively separate and enrich the aroma substances in different temperature ranges. When compounding, they can be combined according to the fractions or usage requirements to prepare extracts with high aroma intensity.

[0022] In one embodiment, the number of distillation sections is 2, and the composite mass ratio of the distillate in each section is 6:1 to 2:1.

[0023] In one embodiment, the parameters of the 2-stage distillation are as follows:

[0024] In the first stage, the vacuum degree of the distillation tower is adjusted to 180Pa, the distillation temperature is adjusted to 60°C, and the distillation is carried out for 30min-40min until no material is distilled out of the distillation end, and the first-stage distillate is collected; in the second stage, the vacuum degree of the distillation tower is adjusted to 60Pa, the distillation temperature is adjusted to 220°C, and the distillation is carried out for 20-30min until no material is distilled out of the distillation end, and the second-stage distillate is collected.

[0025] In one embodiment, the number of distillation sections is 3, and the composite mass ratio of the distillation products in each section is 5:5:1 to 1:1:1.

[0026] In one embodiment, the parameters of the 3-stage distillation are as follows:

[0027] In the first stage, the vacuum degree of the distillation tower is adjusted to 180Pa, the distillation temperature is adjusted to 60°C, and the distillation is carried out for 30min-40min until no material is distilled out of the distillation end, and the first stage distillate is collected; in the second stage, the vacuum degree of the distillation tower is adjusted to 120Pa, the distillation temperature is adjusted to 120°C, and the distillation is carried out for 20min-30min until no material is distilled out of the distillation end, and the second stage distillate is collected; in the third stage, the vacuum degree of the distillation tower is adjusted to 60Pa, the distillation temperature is adjusted to 220°C, and the distillation is carried out for 20-30min until no material is distilled out of the distillation end, and the third stage distillate is collected.

[0028] In one embodiment, the number of distillation sections is 4, and the composite mass ratio of the distillation products in each section is 4:4:4:1 to 1:1:1:1.

[0029] In one embodiment, the parameters of the 4-stage distillation are as follows:

[0030] In the first section, the vacuum degree of the distillation tower is adjusted to 240Pa, the distillation temperature is adjusted to 80°C, and the distillation is carried out for 15min-30min until no material is distilled out of the distillation end, and the first distillate is collected; in the second section, the vacuum degree of the distillation tower is adjusted to 180Pa, the distillation temperature is adjusted to 120°C, and the distillation is carried out for 15min-25min until no material is distilled out of the distillation end, and the second distillate is collected; in the third section, the vacuum degree of the distillation tower is adjusted to 120Pa, the distillation temperature is adjusted to 210°C, and the distillation is carried out for 15min-25min until no material is distilled out of the distillation end, and the third distillate is collected; in the fourth section, the vacuum degree of the distillation tower is adjusted to 80Pa, the distillation temperature is adjusted to 300°C, and the distillation is carried out for 20-30min until no material is distilled out of the distillation end, and the fourth distillate is collected.

[0031] In one embodiment, the number of distillation sections is 5, and the composite mass ratio of the distillation products in each section is 3:3:3:3:1 to 2:1:1:1:3.

[0032] In one embodiment, the parameters of the 5-stage distillation are as follows:

[0033] In the first stage, the vacuum degree of the distillation tower is adjusted to 300Pa, the distillation temperature is adjusted to 60℃, and the distillation is carried out for 15min-30min until no substance is distilled out of the distillation end, and the first stage distillate is collected; in the second stage, the vacuum degree of the distillation tower is adjusted to 250Pa, the distillation temperature is adjusted to 120℃, and the distillation is carried out for 15min-25min until no substance is distilled out of the distillation end, and the second stage distillate is collected; in the third stage, the vacuum degree of the distillation tower is adjusted to 180Pa, the distillation temperature is adjusted to 180℃, and the distillation is carried out. Distill for 15min-25min until no more material is distilled out of the distillation end, and collect the third-stage distillate; in the fourth stage, adjust the vacuum degree of the distillation tower to 120Pa, adjust the distillation temperature to 240℃, distill for 20-30min until no more material is distilled out of the distillation end, and collect the fourth-stage distillate; in the fifth stage, adjust the vacuum degree of the distillation tower to 60Pa, adjust the distillation temperature to 300℃, distill for 20-30min until no more material is distilled out of the distillation end, and collect the fifth-stage distillate.

[0034] On the other hand, the present application provides a dry tobacco extract prepared by the above method.

[0035] On the other hand, the present application provides the use of the dry tobacco extract prepared by the above method in the preparation of heat-not-burn tobacco products.

[0036] In one embodiment, the heat-not-burn tobacco product includes but is not limited to cigarettes or e-liquids suitable for heat-not-burn electronic cigarette products.

[0037] In one embodiment, the dry tobacco extract can be added into an electronic cigarette atomization liquid to prepare an atomization liquid containing the dry tobacco extract for use; in another embodiment, the dry tobacco extract can be sprayed on tobacco leaves to prepare cigarettes for use.

[0038] On the other hand, the present application provides the use of the dry tobacco extract obtained by the method described in the preparation of electronic cigarette atomizer liquid and / or electronic cigarette products with high sensory quality and low core sticking degree.

[0039] In one embodiment, the amount of the dry tobacco extract added to the electronic cigarette atomizer liquid is 0.01% to 10%, preferably 0.1% to 6%, and more preferably 0.3% to 2%, where the % is the mass percentage (w / w) or mass volume percentage (w / v).

[0040] In one embodiment, the applicable atomization temperature of the electronic cigarette atomization liquid is 200-400° C., such as 230-280° C., 290-380° C., etc.

[0041] In one embodiment, the oil-conducting core suitable for the electronic cigarette atomization liquid is a ceramic core or a cotton core.

[0042] In one embodiment, the applicable number of puffs of the electronic cigarette atomizer liquid is at least 750, preferably at least 760, and more preferably 770 to 1000.

[0043] On the other hand, the present application provides an electronic cigarette atomization liquid containing the dry tobacco extract prepared by the method described.

[0044] In one embodiment, the electronic cigarette atomizer liquid may further contain additives such as nicotine, flavors, cooling agents, sweeteners, etc.

[0045] This application has at least the following beneficial effects:

[0046] 1. Compared with the extract prepared by the traditional method, the dry tobacco extract prepared by the present invention is transparent and clear, and it is easy to observe whether the extract contains macromolecular filamentous substances. When added to the atomizing liquid and atomized into an aerosol, the aroma-causing substances are more easily atomized and released, which can effectively enhance the concentration of tobacco aroma, reduce the risk of burnt smell, and improve user experience.

[0047] 2. The preparation method of the dry tobacco extract provided in the present application adopts a specific rehumidification fermentation and then baking and a treatment method containing atomized solvent extraction and multi-stage distillation. On the one hand, it can significantly reduce the amount of impurities and large molecular sugars and pigments, and significantly increase the content of aroma substances in the dry tobacco leaf raw materials, so that during multi-stage distillation, it can better obtain distillates of different numbers of sections to produce different levels of aroma substances, and at a specific number of sections and compounding ratio, significantly improve the aroma concentration, balance and purity of the smoke; on the other hand, it can also improve the solubility of the distillate in the atomized solvent, which is beneficial to improve the degree of carbon deposition and core sticking, and is more suitable for making electronic cigarette atomizer liquid for use in electronic cigarette products; and the experimental results also show that the dry tobacco extract prepared by this method does not change in properties after long-term storage and has better stability.

[0048] 3. The preparation method provided by the present invention has simple process, easy operation, low cost, high product yield, and is easy to produce and apply, which has positive significance for improving the quality of atomized liquid and its healthy development. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention.

[0050] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following briefly introduces the drawings required for use in the embodiments or the prior art descriptions. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. In the drawings:

[0051] Figure 1 are the physical pictures of dry tobacco extracts prepared in Examples 1 to 16 and Comparative Example 1, respectively, wherein a1 to a4 correspond to Examples 1 to 4, b1 to b4 correspond to Examples 5 to 8, c1 to c4 correspond to Examples 9 to 12, d1 to d4 correspond to Examples 13 to 16, and D1 corresponds to Comparative Example 1;

[0052] Figure 2 It is a comparison chart of the degree of oil-conducting core sticking of a typical embodiment (Example 7) and comparative example 1. DETAILED DESCRIPTION

[0053] In order to more clearly explain the overall concept of the application, the following is described in detail by way of embodiment. In the following description, a large amount of specific details are provided so as to provide a more thorough understanding of the application. However, it is obvious to those skilled in the art that the application can be implemented without one or more of these details. In other examples, in order to avoid confusion with the application, some technical features well known in the art are not described.

[0054] Unless otherwise specified, in the following embodiments, the reagents or instruments used without indicating the manufacturer are all conventional products that can be purchased commercially.

[0055] If no specific conditions are specified in the examples, the experiments were carried out according to conventional conditions or conditions recommended by the manufacturer.

[0056] In the following embodiments, the dry tobacco leaf raw materials were provided by Yunnan Qujing Cigarette Factory.

[0057] Example 1

[0058] This embodiment provides a method for preparing a dry tobacco extract suitable for electronic cigarette atomizer, and the specific steps are as follows:

[0059] S1. Cut dry tobacco leaves into small pieces of 1 cm in length, weigh 10% pure water based on the weight of the tobacco leaves, spray it evenly on the tobacco leaf pieces, place them in a closed environment or container, and perform moisture regeneration and fermentation at room temperature (20° C.-25° C.) for 60 hours.

[0060] S2. The tobacco leaves after moisture restoration and fermentation are taken out and re-baked to simulate traditional cigarettes, specifically, microwave baking is adopted with the conditions of temperature: 70°C and time: 120 min.

[0061] S3, crushing the cured tobacco leaves into 10-30 mesh sizes.

[0062] S4. Place the crushed tobacco leaves in a reactor, add 50% propylene glycol, 200% 95% ethanol and 50% glycerol based on the weight of the tobacco leaves as extraction reagents and stir evenly.

[0063] S5. Under closed conditions, the material is subjected to high-temperature extraction reaction, the reaction temperature is 150° C., and the reaction time is 240 min.

[0064] S6. After the reaction is completed, the reaction product is filtered.

[0065] S7, placing the filtrate in a distillation tower for segmented distillation, wherein the number of distillation sections is 2:

[0066] In the first stage, the vacuum degree of the distillation tower is adjusted to 180 Pa, the distillation temperature is adjusted to 60° C., and the distillation is carried out for 30 to 40 minutes until no substance is distilled out of the distillation end, and the distillate is collected and numbered as dry tobacco distillate 1#;

[0067] In the second stage, the vacuum degree of the distillation tower is adjusted to 60Pa, the distillation temperature is set to 220°C, and the distillation is carried out for 20 to 30 minutes until no more material is distilled out of the distillation end. The distillate is collected and numbered as dry tobacco distillate 2#.

[0068] S8, compounding the dry tobacco rectified product 1# and 2# according to a ratio of dry tobacco rectified product 1#: dry tobacco rectified product 2#=2:1, to obtain the dry tobacco extract a1, such as Figure 1 As shown in a1, it is an almost colorless and transparent liquid.

[0069] S9. Dissolve 0.3% of the dry tobacco extract a1 in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0070] Example 2

[0071] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the number of distillation sections in step S7 is 3, specifically:

[0072] In the first stage, the vacuum degree of the distillation tower is adjusted to 180 Pa, the distillation temperature is adjusted to 60° C., and the distillation is carried out for 30 to 40 minutes until no substance is distilled out of the distillation end, and the distillate is collected and numbered as dry tobacco distillate 1#;

[0073] In the second stage, the vacuum degree of the distillation tower is adjusted to 120 Pa, the distillation temperature is adjusted to 120° C., and the distillation is carried out for 20 to 30 minutes until no substance is distilled out of the distillation end, and the distillate is collected and numbered as dry tobacco distillate 2#;

[0074] In the third stage, the vacuum degree of the distillation tower is adjusted to 60Pa, the distillation temperature is set to 220°C, and the distillation is carried out for 20 to 30 minutes until no more material is distilled out of the distillation end. The distillate is collected and numbered as dry tobacco distillate 3#.

[0075] The dry tobacco distillate 1#, 2#, and 3# are compounded in a proportion, and the compounding mass ratio is dry tobacco distillate 1#: dry tobacco distillate 2#: dry tobacco distillate 3#=5:3:1, so as to obtain the dry tobacco extract a2. Figure 1 As shown in a2, it is a light yellow and transparent liquid.

[0076] 0.6% of dry tobacco extract a2 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0077] Example 3

[0078] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the number of distillation sections in step S7 is 4, specifically:

[0079] In the first stage, the vacuum degree of the distillation tower is adjusted to 240 Pa, the distillation temperature is adjusted to 80° C., and the distillation is carried out for 15 to 30 minutes until no substance is distilled out of the distillation end, and the distillate is collected and numbered as dry tobacco distillate 1#;

[0080] In the second stage, the vacuum degree of the distillation tower is adjusted to 180 Pa, the distillation temperature is adjusted to 120° C., and the distillation is carried out for 15 to 25 minutes until no substance is distilled out of the distillation end, and the distillate is collected and numbered as dry tobacco distillate 2#;

[0081] In the third stage, the vacuum degree of the distillation tower is adjusted to 120Pa, the distillation temperature is adjusted to 210°C, and the distillation is carried out for 15min to 25min until no substance is distilled out of the distillation end, which is numbered as dry tobacco distillate 3#;

[0082] In the fourth stage, the vacuum degree of the distillation tower is adjusted to 80Pa, the distillation temperature is adjusted to 300°C, and the distillation is carried out for 20 to 30 minutes until no material is distilled out of the distillation end. The distillate is collected and numbered as dry tobacco distillate 4#.

[0083] The dry tobacco distillate 1#, 2#, 3#, and 4# are compounded in proportion to obtain the dry tobacco extract a3, and the compounding mass ratio is dry tobacco distillate 1#: dry tobacco distillate 2#: dry tobacco distillate 3#: dry tobacco distillate 4#=4:1:2:1, and the dry tobacco extract a3 is obtained. Figure 1 As shown in a3, it is a yellow and transparent liquid.

[0084] 0.9% of dry tobacco extract a3 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0085] Example 4

[0086] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the number of distillation sections in step S7 is 5, specifically:

[0087] In the first stage, the vacuum degree of the distillation tower is adjusted to 300 Pa, the distillation temperature is adjusted to 60°C, and the distillation is carried out for 15-30 minutes until no substance is distilled out of the distillation end, and the distillate is collected and numbered as dry tobacco distillate 1#;

[0088] In the second stage, the vacuum degree of the distillation tower is adjusted to 250 Pa, the distillation temperature is adjusted to 120° C., and the distillation is continued for 15 to 25 minutes until no substance is distilled out of the distillation end. The distillate is collected and numbered as dry tobacco distillate 2#;

[0089] In the third stage, the vacuum degree of the distillation tower is adjusted to 180Pa, the distillation temperature is adjusted to 180°C, and the distillation is carried out for 15min to 25min until no substance is distilled out of the distillation end, which is numbered as dry tobacco distillate 3#;

[0090] In the fourth stage, the vacuum degree of the distillation tower is adjusted to 120Pa, the distillation temperature is adjusted to 240°C, and the distillation is carried out for 20 to 30 minutes until no substance is distilled out from the distillation end, and the distillate is collected and numbered as dry tobacco distillate 4#;

[0091] In the fifth stage, the vacuum degree of the distillation tower is adjusted to 60 Pa, the distillation temperature is adjusted to 300°C, and the distillation is carried out for 20 to 30 minutes until no material is distilled out of the distillation end. The distillate is collected and numbered as dry tobacco distillate 5#.

[0092] The dry tobacco distillates 1#, 2#, 3#, 4#, and 5# are compounded in proportion, and the compounding mass ratio is dry tobacco distillate 1#: dry tobacco distillate 2#: dry tobacco distillate 3#: dry tobacco distillate 4#: dry tobacco distillate 5#=3:3:3:2:1, so as to obtain a dry tobacco extract a4, such as Figure 1 As shown in a4, Figure 1 As shown in a4, it is a yellow and transparent liquid.

[0093] 1.2% of dry tobacco extract a4 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0094] Example 5

[0095] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the moisture conditioning and fermentation conditions in step S1 are: the amount of water added is 20% of the weight of the tobacco leaves, and the moisture conditioning and fermentation time is 48 hours.

[0096] The dry tobacco distillate 1# and 2# are compounded in proportion to obtain a dry tobacco extract. The compounding mass ratio is: dry tobacco distillate 1#: dry tobacco distillate 2# = 4:1. The dry tobacco extract b1 is obtained, such as Figure 1 As shown in b1, it is a colorless and transparent liquid.

[0097] 1.5% of dry tobacco extract b1 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0098] Example 6

[0099] The preparation methods of this embodiment are substantially the same as those of embodiment 5, with the only difference being that the three-stage distillation of embodiment 2 is adopted.

[0100] The dry tobacco distillate 1#, 2#, and 3# are compounded in proportion to obtain a dry tobacco extract. The compounding mass ratio is dry tobacco distillate 1#: dry tobacco distillate 2#: dry tobacco distillate 3# = 5:4:1. The dry tobacco extract b2 is obtained, such as Figure 1 As shown in b2, it is a yellow and transparent liquid.

[0101] 2% of dry tobacco extract b2 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0102] Example 7

[0103] The preparation method of this embodiment is substantially the same as that of embodiment 5, except that the four-stage distillation of embodiment 3 is adopted. The mass ratio of the obtained distillates of each stage is 4:2:1:1. Figure 1 As shown in b3, it is a yellow and transparent liquid.

[0104] 2.3% of dry tobacco extract b3 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0105] Example 8

[0106] The preparation method of this embodiment is substantially the same as that of embodiment 5, except that the 5-stage distillation of embodiment 4 is adopted. The mass ratio of the obtained distillates of each stage is 3:3:3:2:1. Figure 1 As shown in b4, it is an orange-red and transparent liquid.

[0107] 2.6% of dry tobacco extract b4 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0108] Example 9

[0109] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that in step S2, the baking temperature is 120°C and the baking time is 80 minutes. Figure 1 As shown in c1, it is a yellow and transparent liquid.

[0110] 3% of the dry tobacco extract c1 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0111] Example 10

[0112] The preparation methods of this embodiment are substantially the same as those of embodiment 9, with the only difference being that the three-stage distillation of embodiment 2 is adopted.

[0113] The dry tobacco distillate 1#, 2#, and 3# are compounded in proportion to obtain a dry tobacco extract. The compounding mass ratio is dry tobacco distillate 1#: dry tobacco distillate 2#: dry tobacco distillate 3# = 5:3:1. The dry tobacco extract c2 is obtained, such as Figure 1 As shown in c2, it is an orange-red and transparent liquid.

[0114] 0.7% of dry tobacco extract c2 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0115] Embodiment 11

[0116] The preparation method of this embodiment is substantially the same as that of embodiment 9, except that the four-stage distillation of embodiment 3 is adopted. The mass ratio of the obtained distillates of each stage is 4:2:1:1. Figure 1 As shown in c3, it is an orange-red and transparent liquid.

[0117] 1.4% of dry tobacco extract c3 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0118] Example 12

[0119] The preparation method of this embodiment is substantially the same as that of embodiment 9, except that the 5-stage distillation of embodiment 4 is adopted. The mass ratio of the obtained distillates of each stage is 3:3:3:2:1. Figure 1 As shown in c4, it is an orange-red and transparent liquid.

[0120] 1.7% dry tobacco extract C4 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0121] Embodiment 13

[0122] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that in steps S4 and S5, the amount of extraction solvent added is: 100% of the tobacco mass of propylene glycol, 100% of 95% ethanol and 50% glycerol. The reaction temperature is: 200°C. The reaction time is: 180 min. The dry tobacco extract d1 is obtained, such as Figure 1 As shown in d1, it is a golden and transparent liquid.

[0123] 3.5% of dry tobacco extract d1 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0124] Embodiment 14

[0125] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the three-stage distillation of embodiment 2 is adopted.

[0126] The dry tobacco distillate 1#, 2#, and 3# are compounded in proportion to obtain a dry tobacco extract. The compounding mass ratio is dry tobacco distillate 1#: dry tobacco distillate 2#: dry tobacco distillate 3# = 5:3:1. The dry tobacco extract d2 is obtained. Figure 1 As shown in d2, it is an orange-red and transparent liquid.

[0127] 3.8% of dry tobacco extract d2 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0128] Embodiment 15

[0129] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the four-stage distillation of embodiment 3 is adopted. The mass ratio of the obtained distillates of each stage is 4:2:1:1. Figure 1 As shown in d3, it is an orange-red and transparent liquid.

[0130] 4.5% of dry tobacco extract d3 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0131] Example 16

[0132] The preparation method of this embodiment is substantially the same as that of embodiment 1, except that the 5-stage distillation of embodiment 4 is adopted. The mass ratio of the obtained distillates of each stage is 3:3:3:2:1. Figure 1 As shown in d4, it is an orange-red and transparent liquid.

[0133] 6% dry tobacco extract d4 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0134] Comparative Example 1

[0135] This comparative example adopts a conventional extraction method to prepare a dry tobacco extract, and the specific steps include:

[0136] 1. Crush the dry tobacco leaves into 10-30 mesh.

[0137] 2. Place the crushed tobacco leaves in a reactor, add 95% ethanol (500% of the tobacco leaves' mass) as an extraction reagent and stir evenly.

[0138] 3. Carry out extraction reaction on the material under closed conditions. The extraction temperature is: 75℃. The extraction time is: 120min.

[0139] 4. After the extraction is completed, filter the extract.

[0140] 5. Repeat steps 2 to 4 to perform a second extraction on the residue after the first extraction.

[0141] 6. Combine the two extraction filtrates, concentrate the filtrate under reduced pressure, and remove the extraction solvent to obtain the tobacco extract. This extract is recorded as D1. Figure 1 As shown in D1, it is a dark brown liquid containing some solidified material.

[0142] The 1% dry tobacco extract of Comparative Example 1 was dissolved in a solvent prepared by mixing glycerol and propylene glycol in a volume ratio of 4:6 to prepare an electronic cigarette atomization liquid.

[0143] Effect experiment:

[0144] The dry tobacco extracts prepared in the above examples were dissolved in the atomizing solvent (glycerol: propylene glycol = 4:6 (volume ratio)), and the mass concentrations of each example were 0.1%, 0.3%, 0.5%, 1%, 1.2%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 8%, 10% electronic cigarette atomizing liquid, and the dissolution was observed after fully stirring. The observation results show that the dry tobacco extracts prepared in Examples 1-16 can be completely dissolved in the atomizing solvent at each mass concentration to prepare the electronic cigarette atomizing liquid, and the prepared atomized liquid is still clear and transparent, and the color is colorless or light yellow; while the dry tobacco extract prepared in Comparative Example 1 can be dissolved in the atomizing solvent at a low mass concentration, but the difficulty of dissolving increases at a higher mass concentration, and a small amount of insoluble filaments or flocs are suspended.

[0145] The dry tobacco extracts obtained in the above-mentioned embodiments and comparative examples were added to the atomization solvent (VG:PG=4:6) in proportion to obtain an electronic cigarette atomization liquid, and the electronic cigarette atomization liquid was placed in an electronic atomizer for atomization to produce an aerosol. There are two types of tests. The first type is to organize a group of smoking evaluation personnel to conduct sensory evaluation; the second type is to use a smoking machine for simulated smoking, and the smoking parameters are: 35ml per puff, 2 seconds of suction and 15 seconds of rest. After every 100 puffs of the smoking machine, manual mouth suction is required to confirm whether the core is burnt. A total of 1000 puffs are puffed, and the test is no longer continued after the core is burnt.

[0146] Organize a group of tasters to conduct sensory taste evaluation:

[0147] Sensory evaluation rules: The samples of the embodiment and the comparative samples were randomly numbered and evaluated by the sensory evaluation team. A total of 5 evaluators conducted sensory evaluation from the aspects of overall aroma balance, smoke aroma concentration, comfort, irritation, miscellaneous odor and aftertaste; the full score for overall aroma balance was 20 points, the full score for smoke aroma concentration was 20 points, the full score for comfort was 20 points, the full score for irritation was 20 points, the full score for miscellaneous odor was 20 points and the full score for aftertaste was 20 points; the higher the scores for overall aroma balance, smoke aroma concentration, comfort and aftertaste, the better the expression of smoke aroma; the lower the scores for irritation and miscellaneous odor, the purer the smoke aroma taste.

[0148] The sensory evaluation results of Examples 1 to 16 and the comparative example are shown in Table 1.

[0149] Table 1 Sensory evaluation results of different dry tobacco extracts

[0150]

[0151]

[0152] It can be seen from the results in Table 1 that, compared with the comparative example, in the process of atomizing to form an aerosol, the tobacco aroma in the dry tobacco extract of the electronic cigarette atomizer liquid prepared by the dry tobacco extract prepared by the embodiment method is very outstanding, the tobacco aroma concentration is high, the overall aroma is well balanced, and the impurities are significantly reduced. While obtaining the tobacco aroma, the irritation is reduced, the comfort is enhanced, and the aftertaste of the tobacco aroma is significantly enhanced, thereby significantly improving the user's smoking satisfaction, experience and pleasure. Moreover, when other conditions are not much different, the sensory quality of the electronic cigarette atomizer liquid containing the dry tobacco extract obtained by four-stage distillation is more excellent.

[0153] The second category is to use a smoking machine for simulated smoking. The smoking parameters are: 35ml per puff, 2 seconds of puff and 15 seconds of rest. After every 100 puffs of the smoking machine, manual mouth puffing is required to confirm whether the cigarette wick is burnt. A total of 1,000 puffs are taken. If the cigarette wick is burnt, the test will not continue.

[0154] The results of the simulated smoking test of the smoking machine of Examples 1 to 16 and the comparative example are shown in Table 2.

[0155] Table 2 Test results of different tobacco extracts

[0156]

[0157]

[0158] It can be seen from the results in Table 2 that, compared with the comparative example, the electronic cigarette atomizer liquid prepared from the dry tobacco extract of the embodiment can extend the service life of the electronic cigarette product when used in electronic cigarette products, and can be inhaled for at least 800 puffs or more without the core becoming sticky. The aerosol taste is stable, which reduces the user's use cost and improves the user experience. Among them, when other conditions are not much different, the electronic cigarette atomizer liquid containing the dry tobacco extract obtained by four-stage or five-stage distillation has a better resistance to core sticking.

[0159] Exemplarily, the oil-conducting core of Example 7 is not pasted in the embodiment as shown in FIG. Figure 2 As shown in the middle left figure, the oil guide core of comparative example 1 with a sticky core is as follows Figure 2 As shown in the middle right figure. As can be seen from the comparison in the figure, the electronic cigarette atomizer liquid made from the dry tobacco extract provided in the embodiment of the present application has no core sticking phenomenon after use.

[0160] The yield of the dry tobacco extract prepared by Examples 1 to 16 and the comparative example was calculated to obtain the yield of the dry tobacco extract, which was calculated by dividing the mass of the final product by the mass of the raw material. The following Table 3 shows the yield of the dry tobacco extract prepared by Examples 1 to 16 and the comparative example 1, the storage time of the dry tobacco extract and the corresponding changes in properties.

[0161] Table 3

[0162] Example Yield Storage time Changes in traits Example 1 112％ Half a year Transparent and clear, no color change Example 2 103％ Half a year Transparent and clear, no color change Example 3 94％ Half a year Transparent and clear, no color change Example 4 89％ Half a year Transparent and clear, no color change Example 5 110％ Half a year Transparent and clear, no color change Example 6 103％ Half a year Transparent and clear, no color change Example 7 94％ Half a year Transparent and clear, no color change Example 8 89％ Half a year Transparent and clear, no color change Example 9 112％ Half a year Transparent and clear, no color change Example 10 103％ Half a year Transparent and clear, no color change Embodiment 11 94％ Half a year Transparent and clear, no color change Example 12 89％ Half a year Transparent and clear, no color change Embodiment 13 96％ Half a year Transparent and clear, no color change Embodiment 14 93％ Half a year Transparent and clear, no color change Embodiment 15 89％ Half a year Transparent and clear, no color change Example 16 88％ Half a year Transparent and clear, no color change Comparative Example 1 56％ 3 months More solids precipitate and the color deepens

[0163] It can be seen from the results in Table 3 that, compared with the dry tobacco extract of Comparative Example 1, the dry tobacco extract prepared by the embodiment has a higher yield and good stability, is not easy to volatilize and be oxidized, has a prolonged storage time, is a transparent and clear liquid, is clean and hygienic, and has no flocs, thereby reducing the phenomenon of core sticking.

[0164] The above is only an embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims

1. A method for preparing a dry tobacco extract, characterized in that: The method comprises the following steps: Step 1, subjecting the dry tobacco leaves to moisture conditioning, fermentation, baking and crushing; Step 2, extracting the crushed dry tobacco leaves in step 1 to obtain an extract; Step three, distilling the extract in sections, and compounding the distillates from each distillation section to obtain the dry tobacco extract.

2. The preparation method according to claim 1, characterized in that: In the step 1, the conditions for moisture recovery and fermentation are: the amount of water added is 10% to 50% of the weight of the tobacco leaves, and the moisture recovery is carried out in a closed environment at room temperature for 48 to 60 hours; And / or, the baking conditions are: baking at 70° C. to 250° C. for 10 min to 300 min.

3. The preparation method according to claim 1, characterized in that: In the step 2, the extraction conditions are: using 50% to 200% of the extractant based on the weight of the tobacco leaves, extracting at 90° C. to 400° C. for 30 to 300 minutes; Preferably, the extractant is selected from one or more of propylene glycol, glycerol, ethanol and water.

4. The preparation method according to claim 1, characterized in that: In the step 3, the vacuum degree of distillation is 30-300 Pa, and the heating temperature is 60-300° C.

5. The preparation method according to claim 1, characterized in that: In the step 3, the segmented distillation is divided into two to five segments; Preferably, the staged distillation is a four-stage distillation or a five-stage distillation; Preferably, the composite mass ratio of the distillates of each stage of the four-stage distillation is 4:4:4:1 to 1:1:1:1; and / or, the composite mass ratio of the distillates of each stage of the five-stage distillation is 3:3:3:3:1 to 2:1:1:1:

3.

6. The dry tobacco extract prepared by the method according to any one of claims 1 to 5.

7. Use of the dry tobacco extract obtained by the method according to any one of claims 1 to 5, or the dry tobacco extract according to claim 6 in the preparation of heat-not-burn tobacco products.

8. Use of the dry tobacco extract obtained by the method according to any one of claims 1 to 5, or the dry tobacco extract according to claim 6 in the preparation of electronic cigarette atomizer liquid and / or electronic cigarette products with high sensory quality and low core sticking degree.

9. The use according to claim 8, characterized in that: The amount of the dry tobacco extract added to the electronic cigarette atomizer liquid is 0.01% to 10%, where the % is the mass percentage (w / w) or the mass volume percentage (w / v).

10. An electronic cigarette atomizing liquid, characterized in that: Contains a dry tobacco extract obtained by the method according to any one of claims 1 to 5, or a dry tobacco extract according to claim 6.

Images