CN113115977A - Green preparation method of tobacco lysate - Google Patents
Green preparation method of tobacco lysate Download PDFInfo
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- CN113115977A CN113115977A CN202110363674.8A CN202110363674A CN113115977A CN 113115977 A CN113115977 A CN 113115977A CN 202110363674 A CN202110363674 A CN 202110363674A CN 113115977 A CN113115977 A CN 113115977A
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- tobacco
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention relates to a green preparation method of tobacco cracking liquid, which comprises the steps of crushing tobacco leaves, mixing the crushed tobacco leaves with ionic liquid, carrying out catalytic cracking on tobacco powder at the temperature of 150-400 ℃, taking out cracking products by using nitrogen or air, condensing the products by using a condenser to obtain the tobacco cracking liquid, filtering reaction liquid and recovering the ionic liquid, wherein no wastewater is generated in the whole process. Therefore, the method provided by the invention has the characteristics of no waste liquid generation, convenience in separation and the like, and has the advantages of thorough reaction and high yield of the target product. The obtained tobacco cracking liquid is mainly a micromolecular aromatic substance, and can be directly added into the heated cigarette to achieve the purpose of increasing the aroma.
Description
Technical Field
The invention belongs to the field of fragrance increasing of cigarettes, and particularly relates to a green preparation method of a tobacco lysate.
Background
The smoking set temperature of the heating cigarette is about 300 ℃, compared with the conventional cigarette, due to the lower temperature, harmful ingredients in the smoke are obviously less, but macromolecular aroma precursor compounds in the tobacco leaves are difficult to thermally crack, and the smoke aroma is obviously insufficient, so the aroma increasing technology of the heating cigarette is a problem to be solved urgently at present. The catalyst can reduce the energy barrier of the reaction, reduce the reaction temperature and accelerate the reaction speed, and the catalyst is used for causing the tobacco leaves to undergo catalytic cracking reaction to generate aroma substances, so that the method is a new way for heating the cigarettes to increase the aroma.
The green synthesis technology can reduce the pollution to the environment and reduce the cost and energy consumption of the process, and is a novel technology with wide development prospect. The ionic liquid has the characteristics of small vapor pressure, difficult combustion, good stability, good conductivity, designability and the like, has extremely low vapor pressure and extremely small pollution to a reaction system, is a green solvent and catalyst, and is widely applied in the fields of green chemistry and catalysis. The ionic liquid is used for catalyzing the tobacco leaf cracking to prepare the tobacco cracking liquid, and the method is an effective green synthetic method.
Disclosure of Invention
The invention aims to provide a green preparation method of tobacco pyrolysis liquid, which aims to solve the problem that the temperature of a smoking set for heating cigarettes cannot realize thermal cracking of macromolecular aroma precursor compounds in tobacco leaves, so that the aroma in the smoke is obviously insufficient.
In order to realize the purpose, the invention is realized by the following technical scheme:
a green preparation method of tobacco lysate comprises the following steps:
s1, crushing tobacco leaves into tobacco powder, mixing the tobacco powder with ionic liquid, carrying out catalytic cracking on the tobacco powder at the temperature of 120-400 ℃, taking out a cracking product by using nitrogen or air, and condensing the product by using a condenser to obtain a reaction liquid containing a tobacco cracking liquid;
and S2, filtering the reaction solution to recover ionic liquid, thereby obtaining the tobacco lysate.
Further, the ionic liquid comprises a cation and an anion;
wherein the cation comprises 1-alkyl-3-methylimidazole, wherein the alkyl group is methyl, ethyl, propyl, butyl, pentyl, hexyl, octyl, dodecyl, tetradecyl or hexadecyl; the anion comprises one of chlorine, bromine, iodine, tetrafluoroboric acid, hexafluorophosphoric acid, acetic acid, bistrifluoromethanesulfonimide, nitric acid, perchloric acid, hydrogen sulfate, dihydrogen phosphate, trifluoromethanesulfonic acid, trifluoroacetic acid or p-toluenesulfonic acid.
Further, in step S1, the mass ratio of the tobacco powder to the ionic liquid is 1-100.
Further, in step S1, the reaction time is 1-100h, and the nitrogen or air flow is 1-100 ml/min.
Further, the condensation temperature of the condenser is-10-10 ℃.
The invention has the beneficial effects that:
the invention uses ionic liquid, which is a reaction medium and also a reaction catalyst, to carry out cracking reaction on tobacco leaves under the condition of heating so as to produce the cracking liquid. The pyrolysis product is a micromolecular aromatic substance, can be volatilized from a reaction system at high temperature, and is condensed to obtain the tobacco pyrolysis liquid. Other solvents are not needed in the whole reaction process, no wastewater is generated, the separation is simple, the yield of the obtained tobacco lysate is high, and the method is green and efficient.
Drawings
FIG. 1 is a schematic view of a reaction apparatus according to the present invention.
Detailed Description
The technical solutions of the present invention are described in detail by the following examples, which are only exemplary and can be used for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
In the following examples of the present application, the equipment, reagents or instruments used, unless otherwise specified, can be purchased commercially. The reaction apparatus of the present application is shown in FIG. 1.
Example 1
As shown in fig. 1, the main experimental reagents and instruments: ionic liquid, N2The device comprises air, a heat collection type constant temperature heating magnetic stirrer 1, a magneton, a reaction bottle 2, a recovery bottle 4, a condenser pipe 3, cooling liquid ethylene glycol and the like.
The specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-dodecyl-3-methylimidazole trifluoromethanesulfonate, introducing 10ml/min of nitrogen, heating to 300 ℃ under a stirring state, keeping for 5 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 2
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 20.0g of 1-ethyl-3-methylimidazolium bromide, introducing 10ml/min of nitrogen, heating to 120 ℃ under a stirring state, keeping the temperature for 1h, and condensing a reaction product by a condenser (the temperature is set to 10 ℃) to obtain the tobacco lysate.
Example 3
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 20.0g of 1-propyl-3-methylimidazolium iodide, introducing 50ml/min of nitrogen, heating to 200 ℃ under a stirring state, keeping the temperature for 20h, and condensing a reaction product by a condenser (the temperature is set to be-5 ℃) to obtain the tobacco lysate.
Example 4
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round bottom flask, adding 400.0g of 1-butyl-3-methylimidazolium tetrafluoroborate, introducing 100ml/min of nitrogen, heating to 220 ℃ under the stirring state, keeping the temperature for 15h, and condensing a reaction product by a condenser (the temperature is set to be-5 ℃) to obtain the tobacco pyrolysis solution.
Example 5
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder into a 250ml round bottom flask, adding 1000.0g of 1-pentyl-3-methylimidazolium hexafluorophosphate, introducing 20ml/min of nitrogen, heating to 250 ℃ under a stirring state, keeping the temperature for 100h, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 6
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder into a 250ml round-bottom flask, adding 2000.0g of 1-hexyl-3-methylimidazole acetate, introducing 20ml/min of nitrogen, heating to 200 ℃ under a stirring state, keeping the temperature for 1h, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 7
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-octyl-3-methylimidazole bistrifluoromethanesulfonylimide salt, introducing 1ml/min of nitrogen, heating to 240 ℃ under a stirring state, keeping the temperature for 5 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain tobacco pyrolysis liquid.
Example 8
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round bottom flask, adding 200.0g of 1-dodecyl-3-methylimidazolium salt, introducing 10ml/min of nitrogen, heating to 320 ℃ under a stirring state, keeping for 4 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 9
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-tetradecyl-3-methylimidazolium salt, introducing 10ml/min of nitrogen, heating to 350 ℃ under a stirring state, keeping for 5 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 10
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-tetradecyl-3-methylimidazolium salt, introducing 10ml/min of nitrogen, heating to 330 ℃ under a stirring state, keeping the temperature for 1h, and condensing a reaction product by a condenser (the temperature is set to be-10 ℃) to obtain the tobacco lysate.
Example 11
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-butyl-3-methylimidazole nitrate, introducing 10ml/min of nitrogen, heating to 300 ℃ under a stirring state, keeping the temperature for 5 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 12
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder into a 250ml round-bottom flask, then adding 200.0g of 1-methyl-3-methylimidazole perchlorate, introducing 10ml/min of air, heating to 280 ℃ under a stirring state, keeping for 2h, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 13
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-hexyl-3-methylimidazole bisulfate, introducing 10ml/min of nitrogen, heating to 230 ℃ under a stirring state, keeping for 5 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 14
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round bottom flask, adding 200.0g of 1-propyl-3-methylimidazole dihydrogen phosphate, introducing 10ml/min of nitrogen, heating to 220 ℃ under a stirring state, keeping for 1h, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 15
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder into a 250ml round bottom flask, adding 200.0g of 1-butyl-3-methylimidazole trifluoromethanesulfonic acid, introducing 10ml/min of nitrogen, heating to 400 ℃ under a stirring state, keeping for 2h, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
Example 16
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder into a 250ml round bottom flask, adding 200.0g of 1-butyl-3-methylimidazole trifluoroacetate, introducing 10ml/min of nitrogen, heating to 260 ℃ under a stirring state, keeping the temperature for 1h, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain a tobacco lysate.
Example 17
The reagent and the apparatus are implemented in the same way as in the embodiment 1, and the specific implementation steps are as follows: weighing 20.0g of tobacco powder, placing the tobacco powder in a 250ml round-bottom flask, adding 200.0g of 1-alkyl-3-methylimidazole p-toluenesulfonate, introducing 10ml/min of nitrogen, heating to 300 ℃ under a stirring state, keeping for 5 hours, and condensing a reaction product by a condenser (the temperature is set to be 0 ℃) to obtain the tobacco lysate.
TABLE 1 summary of experimental conditions and yields in the examples
Note: the liquid yield refers to the mass of tobacco lysate obtained per unit mass of tobacco dust.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (5)
1. A green preparation method of tobacco lysate is characterized by comprising the following steps:
s1, crushing tobacco leaves into tobacco powder, mixing the tobacco powder with ionic liquid, carrying out catalytic cracking on the tobacco powder at the temperature of 120-400 ℃, taking out a cracking product by using nitrogen or air, and condensing the product by using a condenser to obtain a reaction liquid containing a tobacco cracking liquid;
and S2, filtering the reaction solution to recover ionic liquid, thereby obtaining the tobacco lysate.
2. The green preparation method of tobacco lysate according to claim 1, characterized in that the ionic liquid comprises a cation and an anion;
wherein the cation comprises 1-alkyl-3-methylimidazole, wherein the alkyl group is methyl, ethyl, propyl, butyl, pentyl, hexyl, octyl, dodecyl, tetradecyl or hexadecyl; the anion comprises one of chlorine, bromine, iodine, tetrafluoroboric acid, hexafluorophosphoric acid, acetic acid, bistrifluoromethanesulfonimide, nitric acid, perchloric acid, hydrogen sulfate, dihydrogen phosphate, trifluoromethanesulfonic acid, trifluoroacetic acid or p-toluenesulfonic acid.
3. The green preparation method of tobacco lysate according to claim 1, wherein in step S1, the mass ratio of tobacco powder to ionic liquid is 1-100.
4. The green preparation method of tobacco lysate according to claim 1, characterized in that, in step S1, the reaction time is 1-100h, and the nitrogen or air flow is 1-100 ml/min.
5. The green preparation method of tobacco lysate according to claim 1, wherein the condensation temperature of the condenser is-10 to 10 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113812668A (en) * | 2021-09-27 | 2021-12-21 | 浙江中烟工业有限责任公司 | Method for extracting rectified aroma substances by dry distillation of tobacco leaves |
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