CN105768202A - Method for extracting nicotine from tobacco wastes - Google Patents
Method for extracting nicotine from tobacco wastes Download PDFInfo
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- CN105768202A CN105768202A CN201610278965.6A CN201610278965A CN105768202A CN 105768202 A CN105768202 A CN 105768202A CN 201610278965 A CN201610278965 A CN 201610278965A CN 105768202 A CN105768202 A CN 105768202A
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- nicotine
- extraction
- ionic liquid
- tobacco waste
- 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
- 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 method for extracting nicotine from tobacco wastes. The method comprises the following step of adding an alkaline ion liquid salt solution and the tobacco waste into a synthetic extractor to extract at normal pressure, wherein the temperature is 50 to 70 DEG C, and the extraction time is 25 to 35min, so as to obtain the nicotine; the alkaline ion liquid salt solution is prepared from alkaline ion liquid and potassium acetate. The method for extracting the nicotine from the tobacco wastes has the advantages that the efficiency of extracting the nicotine from the tobacco wastes is greatly improved, the application production of the nicotine is favorable, and the quality of tobacco sheets is improved; the alkaline ion liquid can be recycled for multiple times, so that the pollution to environments is avoided.
Description
Technical field
The present invention relates to the extracting method of tobacco extract, extract the method for nicotine in tobacco waste particularly to a kind of.
Background technology
Tobacco extract has this perfume of Nicotiana tabacum L., is commonly used for tobacco product perfume material, and its note can be coordinated with cigarette perfume (or spice) and make cigarette aromatic strongly fragrant, and the application in Medicated cigarette perfumery is widely.Nicotiana tabacum L. is a kind of complex system, and the chemical composition therefrom identified is up to thousands of kinds.Tobacco extract is different due to its extraction process, product chemical composition difference to some extent, and also the most noticeable most important composition is exactly nicotine in tobacco extract.
Nicotine is the important chemical composition in Nicotiana tabacum L., and nicotine (nicotine) has another name called nicotine, is a kind of pyridine type alkaloid, is present in Nicotiana industrial crops.Nicotine is at room temperature colourless or light bronze-colored oily liquids, and sterling is colourless oil liquid, quickly becomes brown color with air contact, and nicotine content height then strength is big, has strong impulse, and acrid in the mouth is peppery, and the low then strength of content is little, and it is tasteless to suck.Therefore the height of nicotine content in tobacco extract, has material impact to its addition, is the important parameter weighing tobacco extract quality, specification, is the leading indicator controlling tobacco extract.
The purposes of nicotine is a lot, and first it can serve as insecticide.The nicotine neutral sulfate. that nicotine and sulfuric acid reaction obtain is exactly an example.The nicotine neutral sulfate. of 40%, at the commodity by name " Blaikleaf40 " of the U.S., is a kind of widely used insecticide in the world.People develop class nicotine insecticide according to the structural research of nicotine, and nicotine can also as the raw material of some class nicotine insecticide.Such as 1991, He'nan University utilized nicotine successfully to synthesize class nicotine insecticide " aphid fourth of getting killed " for substrate.
Additionally, nicotine has pharmaceutical value widely.Lang Sha company of Switzerland utilizes nicotine to make nicotinic acid through peroxidating very early, and (vitaminF, anti-scurf element) is also produced in batches.Abroad, nicotinoids medicine can be used for smoking deterent.Agent as glutinous in nicotine transdermal, it, by nicotine or its acylate (lactate, citrate, Salicylate etc.), makes nicotine be absorbed by the skin by transdermal slow-release system, reduces additive；The ion exchange resin containing a certain amount of nicotine can also be made, be similar to chewing gum, can chew in mouth, discharge nicotine direct oral cavity mucosal absorption in chewing, it is also possible to alleviate the symptom of smoking addiction.With other natural plant extracts dispensing, tobacco piece of keeping in mouth can also be made.Additionally, nicotine citrate, oxynicotine, nicotine the nicotinic compounds such as quaternary ammonium salt, the fragrance of Nicotiana tabacum L. as the additive of Nicotiana tabacum L., can be made more to make a gift of people.For the Nicotiana tabacum L. high containing nicotine, usually there is the method such as extraction, steam distillation to extract a part of nicotine, then the nicotine that a part is extracted becomes citrate and adds in Nicotiana tabacum L., to promote tobacco flavor.The exploitation further of nicotine emerges in an endless stream, and has good market prospect.
Nicotine can be combined with the nicotine cholinergic of external and central nervous system.Nervous system is had excitation by it, can improve awakening, attention and reactivity, reduces anxiety and nervous reaction.The tartrate of nicotine can substantially reduce the diastolic pressure of hyperpietic immediately and shrink pressure.Two tartrate local drug delivery of nicotine, can treat muscle spasm and arthralgia.
At present, the extracting method of Performance Liquid Chromatography Analysis for Nicotine in Tobacco mainly has: the methods such as the exchange of distillation extraction, ion and supercritical fluid extraction.Water distillation extractor is the more general extracting method being relatively early applied to industrialized production, Lu Xuwang etc. (twice extraction and distillation method extracts the research [J] of nicotine in waste/hypo-tobacco leaf. application chemical industry, 2006,35 (1): 48-53) adopt twice extraction and distillation method, from waste/hypo-tobacco leaf, obtain the nicotine that purity is 40%.But the method operating procedure is complicated, and extraction time is longer.Ion exchange is by raw material diluted acid lixiviate, after being heated to reflux, makes filtrate flow through ion exchange resin, then obtains the aqueous solution of free nicotine with alkali exchange.Though the method energy consumption is relatively low, but still suffers from the pretreatment of ion exchange resin and regenerate relatively complicated shortcoming.(Preliminarystudyonthesupercriticalcarbondioxideextractio nofnicotinefromtobaccowastes [J] .SeparationScienceandTechnology such as Rincon, 1998,33 (3): 411-423.) at 25MPa, supercritical CO at 60 DEG C, is adopted2Extract the nicotine in solid cigarette sample, it is thus achieved that extraction efficiency preferably, but the equipment cost of the method is higher, be unfavorable for universal and promote.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, it is an object of the invention to provide and a kind of extract the method for nicotine in tobacco waste, the extraction ratio being effectively increased in tobacco waste nicotine.
The purpose of the present invention is achieved through the following technical solutions:
A kind of extract the method for nicotine in tobacco waste, comprise the following steps:
Alkali ionic liquid saline solution and tobacco waste being added in synthesis abstraction instrument and carry out atmospheric extraction, temperature is 50～70 DEG C, and extraction time is 25～35min, obtains nicotine；
Described alkali ionic liquid saline solution is made up of alkali ionic liquid and potassium acetate.
Described alkali ionic liquid is the one in [MMIM] DMP, [Bmim] [HCOO], [Hmim] [Ac], [Emim] [Ac] alkali.
Described alkali ionic liquid saline solution is made up of following methods:
Being added by alkali ionic liquid in potassium salt solution, controlling potassium acetate mass concentration in system is 3%～12%, filters, filtrate washed with diethylether 2～3 times under room temperature after stirring 20～24 hours, uses Rotary Evaporators decompression distillation 1～2 hour.
Described synthesis abstraction instrument is microwave catalysis synthesis abstraction instrument, and during extraction, microwave power is 400～500W.
Described tobacco waste is cabo；The mass ratio of described alkali ionic liquid saline solution and cabo is 23:1～27:1.
Described tobacco waste is offal；The mass ratio of described alkali ionic liquid saline solution and offal is 18:1～22:1.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) present invention adopts alkali ionic liquid saline solution as the lixiviating solution of grass garbage, substantially increase the extraction efficiency of nicotine in tobacco waste, compared with adopting industrial tap water extraction, in offal, nicotine extraction ratio improves 30%, and in cabo, nicotine extraction ratio improves 34.2%.
(2) the employing alkali ionic liquid saline solution of the present invention is as the lixiviating solution of grass garbage, solve and use traditional organic solvent extraction contaminated environment, use the shortcoming that organic solvent amount is big, also solve some traditional extraction process complicated operations simultaneously, cost is high, the shortcoming that energy consumption is high.
(3) present invention can be effectively improved the nicotine extraction ratio in raw material, is conducive to the application of nicotine to produce, improves reconstituted tobacoo quality, and alkali ionic liquid can repeatedly be recycled, and environment is not resulted in pollution.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Configuration quality concentration is the potassium salt solution of 10%, ionic liquid ([MMIM] DMP, [Bmim] [HCOO]), [Hmim] [Ac], [Emim] [Ac] alkalescence are strengthened successively) it is added sequentially in the different beaker equipped with potassium salt solution, strong agitation 24 hours under room temperature, it is filtered to remove white precipitate, then with a small amount of washed with diethylether 2 times, filtrate is placed at 70 DEG C to reduce pressure rotary evaporation 1 hour after filtration, obtain colourless viscous shape liquid ionic liquid saline solution, for the lixiviating solution of tobacco sheet material.Synthesize normal pressure single in abstraction instrument at microwave catalysis respectively and extract cabo and offal raw material, wherein lixiviating solution and cabo 23:1 in mass ratio, extraction temperature is 50 DEG C, extraction time is 25min, microwave power is 400W, lixiviating solution and offal 18:1 in mass ratio, and extraction temperature is 50 DEG C, extraction time is 35min, and result is in Table 1.
Table 1
Table 1 it is shown that the nicotine extraction ratio between different ions liquid liquid is also different, under certain alkali condition nicotine extraction ratio with ionic liquid alkalescence enhancing and strengthen.This is due to the existence of pyrrole ring and pyridine ring in nicotine base molecule, makes nicotine can dissociate out when alkalescence is bigger, and alkalescence is more strong more is conducive to the dissolution of nicotine in tobacco material.
Embodiment 2
The potassium salt solution of differently configured mass concentration, alkali ionic liquid [Emim] [Ac] is added wherein, strong agitation 20 hours under room temperature, it is filtered to remove white precipitate, then with a small amount of washed with diethylether 3 times, filtrate is placed at 70 DEG C to reduce pressure rotary evaporation 2 hours after filtration, obtain colourless viscous shape liquid alkaline ionic liquid saline solution and synthesize normal pressure single extraction cabo and offal raw material in abstraction instrument at microwave catalysis respectively, wherein lixiviating solution and cabo 27:1 in mass ratio, extraction temperature is 70 DEG C, extraction time is 35min, microwave power is 500W, lixiviating solution and offal 22:1 in mass ratio, extraction temperature is 70 DEG C, extraction time is 5min, result is in Table 2.
Table 2
The result of table 2 shows, in leaching process, add potassium acetate and significantly facilitate nicotine extraction ratio in raising cabo and offal, this is because under ion liquid medium heating condition, the hydrogen bond that the polarity of inorganic salt potassium acetate can be destroyed in biomass between fiber with fiber is connected and network structure, promotes the dissolution of nicotine.In leaching process, the interpolation concentration of potassium acetate is advisable with 3%-12%, and when adding concentration higher than 12%, extraction ratio slightly declines, and is unfavorable for subsequent treatment, so the potassium acetate solution that the present invention chooses 3%-12% joins in lixiviating solution as extracting solution system.
Embodiment 3
Configuration quality concentration is the potassium salt solution of 10%, laboratory self-control or commercially available alkali ionic liquid [Emim] [Ac] are added wherein, strong agitation 24 hours under room temperature, it is filtered to remove white precipitate, then a small amount of washed with diethylether is used, filtrate is placed at 70 DEG C to reduce pressure rotary evaporation 1 hour after filtration, obtain colourless viscous shape liquid alkaline ionic liquid saline solution, in having microwave catalysis synthesis and synthesizing without microwave catalysis, normal pressure single extracts cabo and offal raw material respectively, wherein lixiviating solution and cabo 25:1 in mass ratio, extraction temperature is 60 DEG C, extraction time is 30min, lixiviating solution and offal 20:1 in mass ratio, extraction temperature is 50～70 DEG C, extraction time is 35～45min, result is in Table 3.
Table 3
The result of table 3 shows when microwave catalysis, in raw material, nicotine extraction ratio is notable, all more than 85%, apparently higher than the equal conditions leaching process without microwave catalysis, this is because the motion of biomass macromole is more violent under microwave condition, produce bigger heat effect, and the hydrogen bond in biomacromolecule, hydrophobic bond and Van der Waals force can also be produced certain effect by microwave so that Microwave Dissolution promotes that in raw material, the dissolving of nicotine is extracted.
Embodiment 4
Configuration quality concentration is the potassium salt solution of 10%, by ionic liquid, ([MMIM] DMP adds wherein, strong agitation 20 hours under room temperature, it is filtered to remove white precipitate, then a small amount of washed with diethylether is used, filtrate is placed at 70 DEG C to reduce pressure rotary evaporation 2 hours after filtration, obtain colourless viscous shape liquid alkaline ionic liquid saline solution and synthesize normal pressure single extraction cabo and offal raw material in abstraction instrument at microwave catalysis respectively, wherein lixiviating solution and cabo 27:1 in mass ratio, extraction temperature is 70 DEG C, extraction time is 35min, lixiviating solution and offal 22:1 in mass ratio, extraction temperature is 70 DEG C, extraction time is 5min, result is in Table 4.
Table 4
The result of table 4 shows, compared with industrial tap water and [MMIM] DMP ionic liquid extract, lixiviating solution of the present invention is for extracting in tobacco waste the effect of nicotine clearly, effectively raise the nicotine extraction ratio in tobacco waste, effectively raise the quality of reconstituted tobacoo and effect of smokeing panel test.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted by the embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. one kind is extracted the method for nicotine in tobacco waste, it is characterised in that comprise the following steps:
Alkali ionic liquid saline solution and tobacco waste being added in synthesis abstraction instrument and carry out atmospheric extraction, temperature is 50～70 DEG C, and extraction time is 25～35min, obtains nicotine；
Described alkali ionic liquid saline solution is made up of alkali ionic liquid and potassium acetate.
2. the method for nicotine in extraction tobacco waste according to claim 1, it is characterized in that, described alkali ionic liquid is the one in [MMIM] DMP, [Bmim] [HCOO], [Hmim] [Ac], [Emim] [Ac] alkali.
3. the method for nicotine in extraction tobacco waste according to claim 2, it is characterised in that described alkali ionic liquid saline solution is made up of following methods:
Being added by alkali ionic liquid in potassium salt solution, controlling potassium acetate mass concentration in system is 3%～12%, filters, filtrate washed with diethylether 2～3 times under room temperature after stirring 20～24 hours, uses Rotary Evaporators decompression distillation 1～2 hour.
4. the method for nicotine in extraction tobacco waste according to claim 1, it is characterised in that described synthesis abstraction instrument is microwave catalysis synthesis abstraction instrument, and during extraction, microwave power is 400～500W.
5. the method for nicotine in extraction tobacco waste according to claim 1, it is characterised in that described tobacco waste is cabo；The mass ratio of described cabo and alkali ionic liquid saline solution is 23:1～27:1.
6. the method for nicotine in extraction tobacco waste according to claim 1, it is characterised in that described tobacco waste is offal；The mass ratio of described offal and alkali ionic liquid saline solution is 18:1～22:1.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106235385A (en) * | 2016-09-12 | 2016-12-21 | 甘肃烟草工业有限责任公司 | Tobacco stalk fibre microwave degradation prepares cigarette feed liquid method and application |
| CN107320998A (en) * | 2017-08-01 | 2017-11-07 | 青岛科技大学 | A kind of method of utilization ionic liquid and inorganic salts extracting mixed extractant isolating alkaloids |
| WO2019229704A1 (en) * | 2018-05-31 | 2019-12-05 | Radient Technologies Inc. | Process for reducing nicotine in tobacco biomass and tobacco composition |
| CN111771922A (en) * | 2020-07-24 | 2020-10-16 | 云南煜天农业发展有限公司 | Special pesticide for gardening flowers and preparation method thereof |
| CN113115977A (en) * | 2021-04-02 | 2021-07-16 | 河南中烟工业有限责任公司 | Green preparation method of tobacco lysate |
| CN113208149A (en) * | 2021-05-24 | 2021-08-06 | 中烟施伟策（云南）再造烟叶有限公司 | Method suitable for retaining fragrance and improving quality of paper-making reconstituted tobacco |
| CN113508919A (en) * | 2020-12-31 | 2021-10-19 | 上海零诺生物科技有限公司 | Tobacco extract and preparation method and application thereof |
| CN113933432A (en) * | 2021-10-22 | 2022-01-14 | 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 |
| CN113999202A (en) * | 2021-11-22 | 2022-02-01 | 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 |
| WO2022122650A1 (en) * | 2020-12-09 | 2022-06-16 | Philip Morris Products S.A. | Improved method of producing a liquid tobacco extract |
| CN116235983A (en) * | 2023-02-20 | 2023-06-09 | 广州华芳烟用香精有限公司 | Method for extracting nicotine from tobacco absolute |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106235385B (en) * | 2016-09-12 | 2017-09-29 | 甘肃烟草工业有限责任公司 | Tobacco stalk fibre microwave degradation prepares cigarette feed liquid method and application |
| CN106235385A (en) * | 2016-09-12 | 2016-12-21 | 甘肃烟草工业有限责任公司 | Tobacco stalk fibre microwave degradation prepares cigarette feed liquid method and application |
| CN107320998A (en) * | 2017-08-01 | 2017-11-07 | 青岛科技大学 | A kind of method of utilization ionic liquid and inorganic salts extracting mixed extractant isolating alkaloids |
| WO2019229704A1 (en) * | 2018-05-31 | 2019-12-05 | Radient Technologies Inc. | Process for reducing nicotine in tobacco biomass and tobacco composition |
| CN111771922A (en) * | 2020-07-24 | 2020-10-16 | 云南煜天农业发展有限公司 | Special pesticide for gardening flowers and preparation method thereof |
| WO2022122650A1 (en) * | 2020-12-09 | 2022-06-16 | Philip Morris Products S.A. | Improved method of producing a liquid tobacco extract |
| CN113508919A (en) * | 2020-12-31 | 2021-10-19 | 上海零诺生物科技有限公司 | Tobacco extract and preparation method and application thereof |
| 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 |
| CN113115977A (en) * | 2021-04-02 | 2021-07-16 | 河南中烟工业有限责任公司 | Green preparation method of tobacco lysate |
| CN113208149A (en) * | 2021-05-24 | 2021-08-06 | 中烟施伟策（云南）再造烟叶有限公司 | Method suitable for retaining fragrance and improving quality of paper-making reconstituted tobacco |
| CN113933432A (en) * | 2021-10-22 | 2022-01-14 | 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 |
| 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 |
| CN113999202A (en) * | 2021-11-22 | 2022-02-01 | 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 |
| 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 |
| CN116235983A (en) * | 2023-02-20 | 2023-06-09 | 广州华芳烟用香精有限公司 | Method for extracting nicotine from tobacco absolute |
| 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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