CN111528517B - Extract for heating non-burning cigarette and preparation method thereof - Google Patents

Extract for heating non-burning cigarette and preparation method thereof Download PDF

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Publication number
CN111528517B
CN111528517B CN202010360303.XA CN202010360303A CN111528517B CN 111528517 B CN111528517 B CN 111528517B CN 202010360303 A CN202010360303 A CN 202010360303A CN 111528517 B CN111528517 B CN 111528517B
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extract
tobacco
cigarette
solution
heating
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CN111528517A (en
CN111528517B8 (en
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龙小洲
瞿方
高占甫
龙李进
李汶琪
欧明毅
童福强
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Guizhou Huangguoshu Golden Leaf Technology Co ltd
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Guizhou Huangguoshu Golden Leaf Technology Co ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/167Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00Cigars; Cigarettes
    • A24D1/20Cigarettes specially adapted for simulated smoking devices

Abstract

The invention provides an extract for heating non-combustible cigarettes and a preparation method thereof, and the preparation method of the extract for heating non-combustible cigarettes comprises the following steps: mixing and leaching the crushed tobacco raw materials with an alcohol solution, performing solid-liquid separation after leaching to obtain a leaching solution, and filtering the leaching solution to obtain a tobacco extracting solution; concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract; adding alkali liquor into the tobacco alcohol extract, uniformly stirring, and mixing with an organic solvent for extraction; separating the liquid after extraction to obtain an organic phase and a water phase, and concentrating the organic phase under reduced pressure to obtain an essential oil product which is an extract for heating the non-combustible cigarettes. The extract for heating the non-combustible cigarette prepared by the invention has higher nicotine content than the conventional tobacco extract, and has obvious tobacco original fragrance and strength. The extract can be used as a tobacco tar component, and a small amount of the extract is added into a cigarette which is not combusted by heating, so that the requirement of the cigarette for keeping the herbal fragrance and strength of the cigarette is met.

Description

Extract for heating non-burning cigarette and preparation method thereof
Technical Field
The invention relates to a tobacco technology, in particular to an extract for heating non-combustible cigarettes and a preparation method thereof.
Background
The cigarette is a new type of cigarette product which is made up in recent years by heating and non-burning, and the key material of its core material mainly consists of tobacco tar, smoke-producing agent and humectant. The core material is heated at about 350 ℃, and the experience feeling similar to that of smoking a traditional cigarette can be obtained. Because the content of harmful substances in the smoke can be reduced, and open fire does not exist, the cigarette which is not combusted by heating gradually becomes the key point of the development of the tobacco industry in China.
At present, the style of the cigarette which is not burned by heating and is popular in the market is different, and the tobacco tar determines the style of the cigarette. The tobacco tar is generally formed by mixing various natural aroma extracts and tobacco extracts, wherein the natural aroma extracts are mainly extracted from natural aromatic plants, the contained aromatic substances are basically compounds with lower molecular weight, the boiling point is low, the volatility is strong, the characteristic aroma can be given to the cigarettes, and the aroma amount of the cigarettes is obviously increased; the latter contains nicotine, organic acid, tobacco phenols and lipid compounds, can increase the concentration of cigarette, the original fragrance and strength of tobacco, and provide satisfaction for smokers; the relative proportions of the two are difficult to equalize. In the formula of the heating non-combustion cigarette, when the content of the natural aroma extract is too high, the characteristic aroma of non-tobacco is obvious, the tobacco aroma is covered, and the cigarette is not stiff and can not meet the experience of smoking; when the content of the natural aroma extract is too low, the proportion of nicotine in the tobacco oil is too high, the aroma of the cigarette is not uniformly released during smoking, the strength and the irritation of the cigarette are increased, and the choking and stinging feeling is generated in the oral cavity and the throat.
In the formula of the cigarette which is not combusted by heating, the natural aroma extract with high content is kept, and the tobacco extract which is enriched with nicotine is added, so that the cigarette can give consideration to characteristic aroma and taste, and the cigarette is very important.
Disclosure of Invention
The invention aims to provide a preparation method of an extract for heating non-combustible cigarettes, aiming at the problem that the existing tobacco extract cannot meet the requirements of the heating non-combustible cigarettes on aroma and taste.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing a cigarette for heating non-combustion, comprising the steps of:
(1) extraction: mixing and leaching the crushed tobacco raw materials with an alcohol solution, performing solid-liquid separation after leaching to obtain a leaching solution, and filtering the leaching solution to obtain a tobacco extracting solution;
(2) concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract, cooling and recovering alcohol;
(3) alkalizing and extracting: adding alkali liquor into the tobacco alcohol extract, uniformly stirring, and mixing with an organic solvent for extraction;
(4) refining: separating the liquid after extraction to obtain an organic phase and a water phase, concentrating the organic phase under reduced pressure to obtain an essential oil product which is an extract used for heating the non-combustible cigarettes, and condensing and recovering the organic solvent.
Further, the particle size of the crushed tobacco raw material powder in the step (1) is 20-80 meshes.
Further, the alcohol solution concentration in the step (1) is 80-95% (v/v), and the mass ratio of the pulverized tobacco raw material to the alcohol solution is 1:7-1: 9.
Further, in the step (1), the leaching temperature is 55-65 ℃, and the leaching time is 1-2 h.
Further, in the step (2), the reduced pressure concentration temperature is 60-75 ℃, the vacuum degree is 0.07-0.08Mpa, the cooling temperature of the recovered alcohol is-5-10 ℃, the solid content of the tobacco alcohol paste is 55-70%, and the solid content is the solid content of the paste liquid in percentage by mass. In the present invention,% represents a mass percentage unless otherwise specified.
Further, in the step (3), the alkali liquor is one or a mixture of more of NaOH solution, KOH solution and ammonia water, and the pH value of the alkali liquor is 12-14; the mass ratio of the tobacco alcohol extract to the alkali liquor is 1:1-3, and the stirring time is 5-10 min.
Further, in the step (3), the organic solvent is one or a mixture of more of petroleum ether, ethyl acetate, dichloromethane and n-hexane, the mass ratio of the tobacco alcohol extract to the organic solvent is 1:2-4, and the extraction time is 0.5-2 h.
Further, in the step (4), the reduced pressure concentration temperature is 20-70 ℃, the vacuum degree is 0.07-0.08Mpa, and the cooling temperature for recovering the organic solvent is-5-10 ℃.
The invention also discloses an extract for heating non-combustible cigarettes, which is prepared by adopting the method.
The invention also discloses a heat non-combustion cigarette, which comprises the extract for heating the non-combustion cigarette.
Further, the heat non-combustible cigarette comprises 0.001-0.01 wt% of the extract for heat non-combustible cigarettes. Further, the tobacco shred of the non-combustible cigarette is coated with 0.001-0.01 wt% of the extract for heating the non-combustible cigarette. The formula of the cigarette without burning by heating comprises the extract for the cigarette without burning by heating, and the dosage of the natural aroma extract can be correspondingly increased. The extract can remarkably increase the original fragrance, concentration and strength of the tobacco without affecting the fragrance amount and concentration; the cigarette has the advantages of giving consideration to characteristic aroma and taste, and having the effects of better improving the quality and experience of the cigarette which is not combusted by heating.
Compared with the prior art, the extract for heating the non-burning cigarette and the preparation method thereof have the following advantages:
(1) the nicotine content of the tobacco extract is 10-20 wt%, and is higher than that of conventional tobacco extract. The invention utilizes the solubility of nicotine to ensure that the transfer sequence of nicotine is as follows: the tobacco raw material → the tobacco extract → the tobacco alcohol extract → the alkali solution → the organic solvent, and finally most of the nicotine is enriched by concentrating the organic solvent, so that the tobacco extract with high nicotine content, excellent aroma quality and excellent aroma quantity is prepared.
(2) The process of replacing nicotine and tobacco aroma substances adopts liquid-liquid extraction, the temperature is low in the concentration stage, and the loss of aroma components of the extract is small; the tobacco extract is concentrated into alcohol paste, and then nicotine and tobacco aroma substances are transferred, so that the consumption of alkali liquor and organic solvent is low, the pollution is low, the recovery rate is high, and the method is suitable for mass production.
(3) The tobacco extract used for heating the non-combustible cigarette has higher nicotine content, can be used as a tobacco tar component, and can be added into the heating non-combustible cigarette in a small amount, so that the requirement of the cigarette for keeping the herbal fragrance and strength of the cigarette is met. Therefore, in the formula of the cigarette, the content of the natural aroma extract can be increased to a certain degree, so that the cigarette can give consideration to characteristic aroma and taste.
(4) The extract for heating the non-combustible cigarette can also be used for treating mildewed tobacco raw materials and low-grade and lower tobacco leaf raw materials.
Detailed Description
The invention is further illustrated by the following examples:
example 1
The embodiment discloses a method for preparing an extract for heating non-combustible cigarettes by taking burley tobacco as a raw material, which comprises the following specific steps:
(1) extraction: pulverizing raw materials with mass m, sieving with 40 mesh sieve, mixing with 7m alcohol solution (90%, v/v), and extracting at 55 deg.C for 1 hr; and (4) carrying out solid-liquid separation after extraction, and filtering the liquid to obtain a tobacco extract.
(2) Concentration: concentrating the tobacco extract at 60 deg.C under reduced pressure until the solid content is 60% to obtain tobacco alcohol extract; cooling to 0 deg.C, and recovering ethanol.
(3) Alkalizing and extracting: adding 2n NaOH solution (pH value of 12) into n tobacco alcohol extract, and stirring for 5 min; mixing with petroleum ether with a mass of 2n, and extracting for 1 h.
(4) Refining: layering the extractive solution, collecting organic phase, and concentrating under reduced pressure at 50 deg.C until no petroleum ether volatilizes to obtain extract for heating non-combustible cigarette; the cooling temperature for recovering petroleum ether was 0 ℃.
The nicotine content of the extract for a heat non-combustible cigarette prepared in this example was 15.35 wt%.
Example 2
The embodiment discloses a method for preparing an extract for heating non-combustible cigarettes by using tobacco raw materials in Zhaotong area of Yunnan, which comprises the following specific steps:
(1) extraction: pulverizing raw materials with mass m, sieving with 60 mesh sieve, mixing with 8m alcohol solution (95%, v/v), and extracting at 60 deg.C for 1.5 hr; and (4) carrying out solid-liquid separation after extraction, and filtering the liquid to obtain a tobacco extract.
(2) Concentration: concentrating the tobacco extract at 65 deg.C under reduced pressure until the solid content is 70% to obtain tobacco alcohol extract; cooling to-10 deg.C, and recovering ethanol.
(3) Alkalizing and extracting: adding NaOH solution (pH value is 12) with mass of 3n into the tobacco alcohol extract with mass of n, and stirring for 5 min; then mixing with dichloromethane with mass n, and extracting for 2 h.
(4) Refining: layering the extractive solution, collecting organic phase, concentrating at 40 deg.C under reduced pressure until no dichloromethane volatilizes to obtain extract for heating non-combustible cigarette; the cooling temperature for the recovery of methylene chloride was-5 ℃.
The extract for a heat non-combustible cigarette prepared in this example had a nicotine content of 12.74 wt%.
Example 3
The embodiment discloses a method for preparing an extract for heating non-combustible cigarettes by using tobacco raw materials in Yuxi region of Yunnan, which comprises the following specific steps:
(1) extraction: pulverizing raw materials with mass m, sieving with 40 mesh sieve, mixing with 10m alcohol solution (80%, v/v), and extracting at 60 deg.C for 1.5 hr; and (4) carrying out solid-liquid separation after extraction, and filtering the liquid to obtain a tobacco extract.
(2) Concentration: concentrating the tobacco extract at 70 deg.C under reduced pressure until the solid content is 55% to obtain tobacco alcohol extract; cooling to 0 deg.C, and recovering ethanol.
(3) Alkalizing and extracting: adding 2n NaOH solution (pH value is 13) into the tobacco alcohol extract with mass of n, and stirring for 10 min; then mixing with n-hexane with the mass of 2n, and extracting for 1 h.
(4) Refining: layering the extractive solution, collecting organic phase, and concentrating under reduced pressure at 50 deg.C until n-hexane is not volatilized to obtain extract for heating non-combustible cigarette; the cooling temperature of the recovered n-hexane was 0 ℃.
The nicotine content of the extract for a heat non-combustible cigarette prepared in this example was 16.63 wt%.
Examples 4 to 6
Examples 4 to 6 disclose three types of cigarettes which are not combusted by heating, and the extracts described in examples 1 to 3 are added to the three types of cigarettes which are not combusted by heating.
Comparative examples 1 to 3 were each prepared by adding an aqueous extract of the tobacco material described in examples 1 to 3 under substantially the same conditions as in the step (1) extraction and the step (2) concentration of examples 1 to 3, except that the extraction solution in the step (1) was water (instead of alcohol in the original examples).
Sensory evaluation comparative experiments were conducted for examples 4 to 6 and comparative examples 1 to 3, respectively, and the results are shown in Table 1.
TABLE 1 sensory evaluation results
Figure GDA0003403232620000051
The result shows that the tobacco extract prepared by the invention is applied to the tobacco shreds of the novel heating non-combustion cigarettes, is coordinated with smoke, maintains the style of the cigarettes, enhances the herbal fragrance of the cigarettes, can obviously improve the strength and satisfaction of the heating non-combustion cigarettes and improve the mouthfeel.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (5)

1. A preparation method of an extract for heating non-combustible cigarettes is characterized by comprising the following steps:
(1) extraction: mixing and leaching the crushed tobacco raw materials with an alcohol solution, performing solid-liquid separation after leaching to obtain a leaching solution, and filtering the leaching solution to obtain a tobacco extracting solution; the concentration of the alcohol solution is 80-95%, and the mass ratio of the crushed tobacco raw materials to the alcohol solution is 1:7-1: 9; the leaching temperature is 55-65 ℃, and the leaching time is 1-2 h;
(2) concentration: concentrating the tobacco extract under reduced pressure to obtain tobacco alcohol extract; the reduced pressure concentration temperature is 60-75 ℃, the vacuum degree is 0.07-0.08Mpa, and the solid content of the tobacco alcohol extract is 55-70%;
(3) alkalizing and extracting: adding alkali liquor into the tobacco alcohol extract, uniformly stirring, and mixing with an organic solvent for extraction; the organic solvent is one or a mixture of more of petroleum ether, ethyl acetate, dichloromethane and n-hexane, the mass ratio of the tobacco alcohol extract to the organic solvent is 1:2-4, and the extraction time is 0.5-2 h;
(4) refining: separating the liquid after extraction to obtain an organic phase and a water phase, and concentrating the organic phase under reduced pressure to obtain an essential oil product which is an extract for heating the non-combustible cigarettes; the vacuum concentration temperature is 20-70 deg.C, and the vacuum degree is 0.07-0.08 Mpa.
2. The method for preparing an extract for heating non-combustible cigarettes according to claim 1, wherein the alkali solution in step (3) is one or more of a NaOH solution, a KOH solution or ammonia water, and the pH value of the alkali solution is 12-14; the mass ratio of the tobacco alcohol extract to the alkali liquor is 1:1-3, and the stirring time is 5-10 min.
3. An extract for use in heating a non-combustible cigarette, characterized by being produced by the method of any one of claims 1 to 2.
4. A heat-nonflammable cigarette, characterized by comprising the extract for heat-nonflammable cigarette of claim 3.
5. The heat non-combustible cigarette according to claim 4, wherein the heat non-combustible cigarette comprises 0.001 to 0.01 wt% of the extract for heat non-combustible cigarette.
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN114698867A (en) * 2022-04-08 2022-07-05 贵州黄果树金叶科技有限公司 Preparation method of reconstituted tobacco with accurate components and reconstituted tobacco

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113383986B (en) * 2021-07-13 2022-08-02 云南中烟工业有限责任公司 Preparation of low-temperature fraction capable of improving strength applied to heated cigarettes and application of low-temperature fraction in heated cigarettes
CN113349413B (en) * 2021-07-13 2022-08-02 云南中烟工业有限责任公司 Preparation method of low-temperature fraction capable of enhancing aroma and reducing harm for heating cigarettes and application of low-temperature fraction in heating cigarettes

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CN1064680A (en) * 1992-03-07 1992-09-23 吴景峰 The production technique of nicotine salt and pure nicotine products
CN1074103A (en) * 1993-01-11 1993-07-14 成都新源天然香料技术开发研究所 The production method of natural nicotine for cigarette
CN106235415A (en) * 2016-08-05 2016-12-21 广西中烟工业有限责任公司 A kind of cigarette perfume (or spice) tobacco juice for electronic smoke
CN106387990A (en) * 2016-11-22 2017-02-15 中国烟草总公司郑州烟草研究院 High-nicotine tobacco extract and application thereof
CN107660811A (en) * 2016-07-27 2018-02-06 湖南中烟工业有限责任公司 A kind of burley tobacco nicotine extract and extraction process
CN109512014A (en) * 2017-09-18 2019-03-26 湖南中烟工业有限责任公司 A method of the extraction nicotine from tobacco

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GB754772A (en) * 1954-05-24 1956-08-15 Plate Ges Mit Beschraenkter Ha Aromatic, mild tobacco with reduced nicotine content and process for the production thereof
CN1064680A (en) * 1992-03-07 1992-09-23 吴景峰 The production technique of nicotine salt and pure nicotine products
CN1074103A (en) * 1993-01-11 1993-07-14 成都新源天然香料技术开发研究所 The production method of natural nicotine for cigarette
CN107660811A (en) * 2016-07-27 2018-02-06 湖南中烟工业有限责任公司 A kind of burley tobacco nicotine extract and extraction process
CN106235415A (en) * 2016-08-05 2016-12-21 广西中烟工业有限责任公司 A kind of cigarette perfume (or spice) tobacco juice for electronic smoke
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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN114698867A (en) * 2022-04-08 2022-07-05 贵州黄果树金叶科技有限公司 Preparation method of reconstituted tobacco with accurate components and reconstituted tobacco
CN114698867B (en) * 2022-04-08 2023-03-03 贵州黄果树金叶科技有限公司 Preparation method of reconstituted tobacco with accurate components and reconstituted tobacco

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CI03 Correction of invention patent

Correction item: Address

Correct: 561018 Songqi Town, economic and Technological Development Zone, Anshun City, Guizhou Province

False: 116000 Songqi Town, Dalian Economic and Technological Development Zone, Liaoning Province

Number: 04-02

Volume: 38

Correction item: Address

Correct: 561018 Songqi Town, economic and Technological Development Zone, Anshun City, Guizhou Province

False: 116000 Songqi Town, Dalian Economic and Technological Development Zone, Liaoning Province

Number: 04-02

Page: The title page

Volume: 38

CI03 Correction of invention patent