CN105768202B - A kind of method of nicotine in extraction tobacco waste - Google Patents
A kind of method of nicotine in extraction tobacco waste Download PDFInfo
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- CN105768202B CN105768202B CN201610278965.6A CN201610278965A CN105768202B CN 105768202 B CN105768202 B CN 105768202B CN 201610278965 A CN201610278965 A CN 201610278965A CN 105768202 B CN105768202 B CN 105768202B
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- Prior art keywords
- nicotine
- tobacco waste
- ionic liquid
- extraction
- liquid
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Classifications
-
- 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
- A24B15/243—Nicotine
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Extraction Or Liquid Replacement (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention discloses a kind of method for extracting nicotine in tobacco waste, comprise the following steps：Atmospheric extraction is carried out during alkali ionic liquid salting liquid and tobacco waste are added into synthesis abstraction instrument, temperature is 50~70 DEG C, and extraction time is 25~35min, obtains nicotine；The alkali ionic liquid salting liquid is made up of alkali ionic liquid and potassium acetate.The method of nicotine substantially increases the extraction efficiency of nicotine in tobacco waste in extraction tobacco waste of the invention, and be conducive to the application of nicotine to produce, reconstituted tobacoo quality is improve, and alkali ionic liquid can be recycled repeatedly, and pollution is not resulted in environment.
Description
Technical field
The present invention relates to the extracting method of tobacco extract, more particularly to a kind of side for extracting nicotine in tobacco waste
Method.
Background technology
Tobacco extract has tobacco this perfume, is commonly used for tobacco product perfume material, and its note can be coordinated and make with cigarette perfume
Cigarette perfume is strong, and the application in cigarette blending is widely.Tobacco is a kind of complex system, and the chemical composition for therefrom identifying is more
Up to thousands of kinds.Tobacco extract is different due to its extraction process, product chemical composition difference, and in tobacco extract most
Important also most noticeable composition is exactly nicotine.
Nicotine is the important chemical composition in tobacco, nicotine (nicotine) also known as nicotine, is a kind of biological pyridine type
Alkali, is present in Nicotiana industrial crops.Nicotine is at room temperature colourless or light bronze-colored oily liquids, and sterling is colorless oil
Liquid, brown color is quickly become with air contact, and nicotine content then strength high is big, there is strong impulse, and taste is pungent is peppery, and content is low
Then strength is small, sucks tasteless.Therefore in tobacco extract nicotine content height, its addition is had a major impact, be
Tobacco extract quality, the important parameter of specification are weighed, is the leading indicator for controlling tobacco extract.
The purposes of nicotine is a lot, and it can serve as insecticide first.The nicotine sulphate that nicotine is obtained with sulfuric acid reaction is exactly
One.40% nicotine sulphate, in the trade name " Blaikleaf 40 " in the U.S., is a kind of widely used desinsection in the world
Agent.People develop class nicotine insecticide according to the structural research of nicotine, and nicotine can also be used as some class nicotine insecticides
Raw material.Such as He'nan University in 1991 using nicotine for substrate has successfully synthesized class nicotine insecticide " aphid fourth of getting killed ".
In addition, nicotine has extensive pharmaceutical value.Lang Sha companies of Switzerland are made nicotinic acid using nicotine through peroxidating very early,
(vitaminF, anti-scurf element) is simultaneously produced in batches.Abroad, nicotinoids medicine can be used for smoking deterent.As nicotine transdermal sticks agent,
Nicotine or its acylate (lactate, citrate, salicylate etc.) are made nicotine by skin by it by transdermal slow-release system
Absorb, reduce additive；The ion exchange resin containing a certain amount of nicotine can also be made, similar to chewing gum, can be in mouth
Chew, nicotine direct oral cavity mucosal absorption is discharged in chewing, it is also possible to mitigate the symptom of smoking addiction.Can also be natural with other
Plant extracts dispensing, is made tobacco piece of keeping in mouth.In addition, the nicotine chemical combination such as quaternary ammonium salt of nicotine citrate, oxynicotine, nicotine
Thing, can make the fragrance of tobacco leaf more make a gift of people as the additive of tobacco.For containing nicotine tobacco high, usually thering is extraction, water to steam
The methods such as steam distillation extract a part of nicotine, then the nicotine that a part is extracted is become citrate are added in tobacco leaf, with
Lifting tobacco flavor.The further exploitation of nicotine emerges in an endless stream, with good market prospects.
Nicotine can be combined with the nicotine cholinergic of external application and central nervous system.It has excitation to nervous system, can
Awakening, notice and reactivity are improved, anxiety and nervous reaction is reduced.The tartrate of nicotine can substantially reduce hypertension immediately
The diastolic pressure and systolic pressure of patient.Two tartrate local drug deliveries of nicotine, can treat muscle cramp and arthralgia.
At present, the extracting method of Performance Liquid Chromatography Analysis for Nicotine in Tobacco mainly has：The side such as distillation extraction, ion exchange and supercritical fluid extraction
Method.Water distillation extractor is the relatively early more universal extracting method for being applied to industrialized production, (the twice extraction and distillation method such as Lu Xuwang
Extract research [J] application chemical industry of nicotine in waste/hypo-tobacco leaf, 2006,35 (1):Twice extraction and distillation method 48-53) is used, from useless
The nicotine that purity is 40% has been obtained in hypo-tobacco leaf.But the method operating procedure is complicated, extraction time is more long.Ion-exchange is
Raw material is extracted with diluted acid, after being heated to reflux, filtrate is flowed through ion exchange resin, then exchanged with alkali and obtain free nicotine
The aqueous solution.Though the method energy consumption is relatively low, still suffers from the pretreatment of ion exchange resin and regenerate relatively complicated shortcoming.
(the Preliminary study on thesupercritical carbon dioxide extraction of such as Rincon
nicotine from tobaccowastes[J].Separation Science and Technology,1998,33(3):
411-423.) in 25MPa, supercritical CO is used at 60 DEG C2Nicotine in extraction solid cigarette sample, obtains and preferably extracts effect
Rate, but the equipment cost of the method is higher, is unfavorable for popularizing and promotes.
The content of the invention
In order to overcome the disadvantages mentioned above and deficiency of prior art, extract tobacco it is an object of the invention to provide one kind and discard
The method of nicotine in thing, effectively increases the recovery rate of nicotine in tobacco waste.
The purpose of the present invention is achieved through the following technical solutions：
The method of nicotine, comprises the following steps in a kind of extraction tobacco waste：
Atmospheric extraction is carried out during alkali ionic liquid salting liquid and tobacco waste are added into synthesis abstraction instrument, temperature is 50
~70 DEG C, extraction time is 25~35min, obtains nicotine；
The alkali ionic liquid salting liquid is made up of alkali ionic liquid and potassium acetate.
The alkali ionic liquid is in [MMIM] DMP, [Bmim] [HCOO], [Hmim] [Ac], [Emim] [Ac] alkali
It is a kind of.
The alkali ionic liquid salting liquid is made up of following methods：
Will alkali ionic liquid add potassium salt solution in, control mass concentration of the potassium acetate in system be 3%~
12%, filtered after stirring 20~24 hours at room temperature, filtrate washed with diethylether 2~3 times uses Rotary Evaporators vacuum distillation 1
~2 hours.
The synthesis abstraction instrument is that microwave catalysis synthesize abstraction instrument, and microwave power is 400~500W during extraction.
The tobacco waste is offal；The alkali ionic liquid salting liquid is 23 with the mass ratio of offal:1~27:
1。
The tobacco waste is offal；The alkali ionic liquid salting liquid is 18 with the mass ratio of offal:1~22:
1。
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) present invention substantially increases tobacco and gives up using alkali ionic liquid salting liquid as the leaching liquor of careless discarded object
The extraction efficiency of nicotine in gurry, compared with being extracted using industrial tap water, nicotine recovery rate improves 30%, offal in offal
Middle nicotine recovery rate improves 34.2%.
(2) use alkali ionic liquid salting liquid of the invention is solved and uses tradition as the leaching liquor of careless discarded object
Organic solvent extraction pollution environment, using the big shortcoming of organic solvent amount, at the same also solve some traditional extraction process behaviour
Make complicated, high cost, the shortcoming of high energy consumption.
(3) present invention can effectively improve the nicotine recovery rate in raw material, be conducive to the application of nicotine to produce, and improve cigarette
Careless thin slice quality, and alkali ionic liquid can be recycled repeatedly, and pollution is not resulted in environment.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
Configuration quality concentration is 10% potassium salt solution, by ionic liquid ([MMIM] DMP, [Bmim] [HCOO]),
[Hmim] [Ac], [Emim] [Ac] alkalescence strengthen successively) it is added sequentially in the different beakers equipped with potassium salt solution, room temperature
Lower strong agitation 24 hours, is filtered to remove white precipitate, is then washed 2 times with a small amount of ether, and filtrate is placed in into 70 DEG C after filtering
Lower decompression rotary evaporation 1 hour, obtains colourless viscous shape liquid ionic liquid salting liquid, for the leaching liquor of tobacco sheet material.
Normal pressure single extracts offal and offal raw material, wherein leaching liquor with offal in mass ratio in microwave catalysis synthesis abstraction instrument respectively
23:1, extraction temperature is 50 DEG C, and extraction time is 25min, and microwave power is 400W, leaching liquor and offal in mass ratio 18:1,
Extraction temperature is 50 DEG C, and extraction time is 35min, the results are shown in Table 1.
Table 1
The result of table 1 shows that the nicotine recovery rate between different ions liquid liquid is also different, under certain alkalescence condition
Nicotine recovery rate strengthens with the enhancing of ionic liquid alkalescence.This is depositing due to pyrrole ring in nicotine base molecule and pyridine ring
Make the nicotine can separate out, the dissolution more strong more that be conducive to nicotine in tobacco material of alkalescence when alkalescence is bigger.
Embodiment 2
The potassium salt solution of different quality concentration is configured, alkali ionic liquid [Emim] [Ac] is added thereto, room temperature
Lower strong agitation 20 hours, is filtered to remove white precipitate, is then washed 3 times with a small amount of ether, and filtrate is placed in into 70 DEG C after filtering
Lower decompression rotary evaporation 2 hours, obtains colourless viscous shape liquid alkaline ionic liquid salting liquid and synthesizes extraction in microwave catalysis respectively
Normal pressure single extraction offal and offal raw material, wherein leaching liquor and offal in mass ratio 27 in instrument:1, extraction temperature is 70 DEG C, extraction
The time is taken for 35min, microwave power is 500W, leaching liquor and offal in mass ratio 22:1, extraction temperature is 70 DEG C, extraction time
It is 5min, the results are shown in Table 2.
Table 2
The result of table 2 shows, in leaching process, nicotine is extracted during addition potassium acetate significantly facilitates raising offal and offal
Rate because under ion liquid medium heating condition, the polarity of inorganic salts potassium acetate can destroy in biomass fiber with
Hydrogen bond connection and network structure between fiber, promote the dissolution of nicotine.The addition concentration of potassium acetate is with 3%- in leaching process
12% is advisable, and when it is higher than 12% to add concentration, recovery rate is declined slightly, and is unfavorable for subsequent treatment, so the present invention chooses
The potassium acetate solution of 3%-12% is added in leaching liquor as extract solution system.
Embodiment 3
Configuration quality concentration is 10% potassium salt solution, by laboratory self-control or commercially available alkali ionic liquid
[Emim] [Ac] is added thereto, at room temperature strong agitation 24 hours, is filtered to remove white precipitate, is then washed with a small amount of ether,
Decompression rotary evaporation 1 hour, obtains colourless viscous shape liquid alkaline ionic liquid salting liquid at filtrate is placed in into 70 DEG C after filtering, point
Normal pressure single extraction offal and offal raw material, wherein leaching liquor and cigarette not in thering are microwave catalysis to synthesize and synthesize without microwave catalysis
Stalk in mass ratio 25:1, extraction temperature is 60 DEG C, and extraction time is 30min, leaching liquor and offal in mass ratio 20:1, extraction temperature
It is 50~70 DEG C to spend, and extraction time is 35~45min, the results are shown in Table 3.
Table 3
The result of table 3 shows that under the conditions of microwave catalysis nicotine recovery rate is notable in raw material, more than 85%, hence it is evident that
Higher than leaching process of the equal conditions without microwave catalysis, because the motion of biomass macromolecular more aggravates under microwave condition
It is strong, produce bigger fuel factor, and microwave to be produced necessarily to the hydrogen bond in large biological molecule, hydrophobic bond and Van der Waals force
Effect so that Microwave Dissolution promote raw material in nicotine dissolving extract.
Embodiment 4
Configuration quality concentration is 10% potassium salt solution, and by ionic liquid, ([MMIM] DMP is added thereto, at room temperature
Strong agitation 20 hours, is filtered to remove white precipitate, is then washed with a small amount of ether, is depressurized at filtrate is placed in into 70 DEG C after filtering
Rotary evaporation 2 hours, obtains colourless viscous shape liquid alkaline ionic liquid salting liquid normal in microwave catalysis synthesis abstraction instrument respectively
Pressure single extraction offal and offal raw material, wherein leaching liquor and offal in mass ratio 27:1, extraction temperature is 70 DEG C, extraction time
It is 35min, leaching liquor and offal in mass ratio 22:1, extraction temperature is 70 DEG C, and extraction time is 5min, the results are shown in Table 4.
Table 4
The result of table 4 shows, compared with industrial tap water and [MMIM] DMP ionic liquid extracts, leaching liquor of the present invention is used
The effect of nicotine clearly, effectively raises the nicotine recovery rate in tobacco waste in tobacco waste is extracted, and has
The quality that improve reconstituted tobacoo of effect and effect of smokeing panel test.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by the embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (6)
1. it is a kind of extract tobacco waste in nicotine method, it is characterised in that comprise the following steps：
Atmospheric extraction is carried out during alkali ionic liquid salting liquid and tobacco waste are added into synthesis abstraction instrument, temperature is 50~70
DEG C, extraction time is 25~35min, obtains nicotine；
The alkali ionic liquid salting liquid is made up of alkali ionic liquid and potassium acetate.
2. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the alkali ion liquid
Body is the one kind in [MMIM] DMP, [Bmim] [HCOO], [Hmim] [Ac], [Emim] [Ac] alkali.
3. it is according to claim 2 extract tobacco waste in nicotine method, it is characterised in that the alkali ion liquid
Body salting liquid is made up of following methods：
By in alkali ionic liquid addition potassium salt solution, it is 3%~12% to control mass concentration of the potassium acetate in system,
Filtered after stirring 20~24 hours at room temperature, filtrate washed with diethylether 2~3 times is small using Rotary Evaporators vacuum distillation 1~2
When.
4. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the synthesis abstraction instrument
For microwave catalysis synthesize abstraction instrument, microwave power is 400~500W during extraction.
5. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the tobacco waste
It is offal；The offal is 23 with the mass ratio of alkali ionic liquid salting liquid:1~27:1.
6. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the tobacco waste
It is offal；The offal is 18 with the mass ratio of alkali ionic liquid salting liquid:1~22:1.
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| CN201610278965.6A CN105768202B (en) | 2016-04-29 | 2016-04-29 | A kind of method of nicotine in extraction tobacco waste |
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| CN105768202B true CN105768202B (en) | 2017-06-23 |
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| CN113508919B (en) * | 2020-12-31 | 2023-05-02 | 上海零诺生物科技有限公司 | Tobacco extract and preparation method and application thereof |
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| CN113933432B (en) * | 2021-10-22 | 2023-08-25 | 中国烟草总公司郑州烟草研究院 | High-sensitivity and high-precision analysis method suitable for detecting alkaloid in tobacco leaves |
| CN113999202B (en) * | 2021-11-22 | 2024-01-12 | 红云红河烟草(集团)有限责任公司 | Method for extracting nicotine by microwave-assisted three-stage extraction technology |
| CN116235983B (en) * | 2023-02-20 | 2024-08-27 | 广州华芳烟用香精有限公司 | Method for extracting nicotine from tobacco absolute |
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