CN107660811A - A kind of burley tobacco nicotine extract and extraction process - Google Patents
A kind of burley tobacco nicotine extract and extraction process Download PDFInfo
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- CN107660811A CN107660811A CN201610597872.XA CN201610597872A CN107660811A CN 107660811 A CN107660811 A CN 107660811A CN 201610597872 A CN201610597872 A CN 201610597872A CN 107660811 A CN107660811 A CN 107660811A
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- electronic cigarette
- activated carbon
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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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- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The present invention provides a kind of burley tobacco nicotine extract and extraction process; by weight percent; the burley tobacco nicotine extract includes nicotine 94 97%, cotinine 0.4 0.6%, N picolines formamide 0.2 0.3%, benzofuranone 0.1 0.2%, indoles 0.1 0.2%, 5,5 dimethyl pyrazolines 0.1 0.2%, acetylpyridine 0.05 0.15%, Megastigmatrienone 0.05 0.1%, methyl heptenone 0.02 0.05%, hydroxyl damascenone 0.02 0.05%, hexadecylic acid 0.02 0.05%, nornicotine 0.01 0.04%.The burley tobacco nicotine extract nicotine content is high, is configured to electronic cigarette liquid, unique style, can improve the satisfaction of electronic cigarette, make electronic cigarette closer to the taste of cigarette.
Description
Technical field
The present invention relates to a kind of burley tobacco nicotine extract and extraction process.
Background technology
In recent years, even decline as the sales volume of conventional tobacco products occurs stagnating in some developed country markets, and
Many state's public places in Nan Chong ban on opium-smoking and the opium trade dynamics continue to increase, the novel tobacco system such as low temperature cigarette, smoke-free tobacco product, electronic cigarette
Product are just also actively researched and developed from strategic height in the transnational tobacco company such as rapid rising, the Fei Mo worlds, BAT, Japan Tobacco and pushed away
Wide novel tobacco product.Electronic cigarette profile is similar to common cigarette, is a kind of dress that nicotine solution can be vaporized into fog
Put, real smoke is taken out by simulation, excitement is brought to smoker.It is by lithium battery（It is chargeable）, atomizer（Heating element heater）, cigarette bullet
（The cigarette holder being commonly seen）Formed Deng element.Electronic cigarette is by the solution atomization containing nicotine, by pulmonary absorption, makes consumer
Obtain the similar satisfaction for sucking traditional cigarette.
Electronic cigarette is commercially received by increasing people at present, and its weak point also progressively shows, and grinds according to investigations
Study carefully, electronic cigarette is compared with regular-size cigarette, although the perceptual image cigarette such as shape, feel, smog, is used for these electronic cigarette liquids and produces
Smog in terms of fragrance, taste, with real cigarette perceptual difference away from larger, these deficiencies, leverage the product of electronic cigarette
Matter.The especially electronic cigarette containing nicotine, the existence form of nicotine are free nicotine mostly, stimulation of the nicotine to throat during suction
It is relatively strong, there is a throat hurt feeling, and traditional cigarette gap is larger.The purpose of this patent is optimization nicotine extraction process, improves the mouth of nicotine
Sense so that product has the distinctive satisfaction of nicotine, also certain tobacco aroma.
The extracting method of nicotine has steam distillation, solvent extraction, ion-exchange and supercritical extract at present
Method etc..Steam distillation is first to neutralize offal with alkali again with diluted acid extraction, finally uses steam distillation, cut chloroform again
Extraction can obtain nicotine.This method processing equipment is huge, and efficiency is low.Solvent extraction be by offal lime flooding, then
Extracted with chloroform or dichloromethane, nicotine salt is made with acid treatment and obtains nicotine by alkalization again.Nicotine is saline and alkaline in the technique
How to be separated after change with salt and water be technique main crux, to be separated by multiple twice extraction and distillation method.
The content of the invention
It is an object of the invention to for the deficiency in terms of existing tobacco juice for electronic smoke satisfaction, nicotine in burley tobaccos is extracted
Technique optimizes research, and existing extracting method is improved, and the nicotine that the present invention obtains is dissolved with Alevaire,
Obtained electronic cigarette liquid can improve the satisfaction of electronic cigarette, make electronic cigarette closer to the taste of cigarette；And further make nicotine with
Cigarette perfume uniformly discharges.
The technical scheme is that, there is provided a kind of burley tobacco nicotine extract, by weight percent, the burley tobaccos cigarette
Alkali extract includes nicotine 94-97%, cotinine 0.4-0.8%, N- picoline formamide 0.2-0.3%, benzofuranone 0.1-
0.2%th, indoles 0.1-0.2%, 5,5- dimethyl pyrazoline 0.1-0.2%, acetylpyridine 0.05-0.15%, Megastigmatrienone
0.05-0.1%, methyl heptenone 0.02-0.05%, hydroxyl damascenone 0.02-0.05%, hexadecylic acid 0.02-0.05%, demethyl cigarette
Alkali 0.01-0.04%.
The present invention also provides a kind of extraction process of burley tobacco nicotine extract, comprises the following steps：With the cigarette of burley tobaccos
End or/and pipe tobacco are raw material, and raw material is placed in organic acid soln, and 1~2h, cooled and filtered, filter are extracted at 70~90 DEG C
Liquid alkaline solution adjust pH value be 10~12, then with volume ratio be 4~10:1 n-hexane and the mixed solvent of ethyl acetate
Extraction, organic phase are evaporated being concentrated under reduced pressure, and obtain nicotine；The mass fraction of the organic acid soln is 5%~15%.
Further, the alkaline solution is sodium hydroxide solution or/and potassium hydroxide solution.
Further, the organic acid soln is one kind in tartaric acid solution, citric acid solution or malic acid solution
Or several mixing.
Further, the mass volume ratio of the raw material and organic acid soln is 1:5-15（g/mL）.
The present invention also provides a kind of electronic cigarette liquid that can uniformly discharge cigarette perfume, and the electronic cigarette liquid includes claim 1 institute
Burley tobacco nicotine extract, aroma component, atomization composition and the modified activated carbon stated；
The preparation method of the modified activated carbon is：After activated carbon is mixed with potassium permanganate in acid condition, reacted,
After the completion of reaction, remove excessive potassium permanganate, after obtained solid product is washed to neutrality with p-methyl benzenesulfonic acid and poly- second
Glycol carries out esterification, obtains modified activated carbon.
Further, the modified activated carbon comprises the following steps：
（1）By mass parts, the activated carbon of 100-500 parts and the potassium permanganate of 500-2000 parts are added into reaction bulb, toward reaction bulb
After middle dropwise addition acid solution, stir, 8-48 hours are reacted under 40-60 degree；
（2）After the completion of reaction, cooling, hydrogen peroxide is added up to the purplish red decoloration of potassium permanganate, reactant mixture is centrifuged, used
The solid that deionized water washing centrifugation obtains is until pH is neutrality；
（3）By step（2）Solid after washing mixes with the p-methyl benzenesulfonic acid of 50-200 parts and the polyethylene glycol of 30-60 parts, with
Toluene is reaction dissolvent, back flow reaction 15-30 hours, after reaction terminates, is evaporated under reduced pressure and removes toluene, gained residue is poured into
Centrifuged in ionized water after ultrasonic disperse, until the pH of solution is neutrality, collects solution and be freeze-dried to obtain modified activated carbon.
Further, the molecular weight of the polyethylene glycol is 200-600.
Further, modified activated carbon containing 0.1-10mg in every gram of electronic cigarette liquid.
The content of nicotine is higher in burley tobaccos, and content is between 2%-4%, and the pH value of burley tobaccos is about 5.8 or so, burley tobaccos
The content more than 10% of non-volatile organic acids in burley tobaccos（Higher than the content 7% of non-volatile organic acids in flue-cured tobacco）, in offal
Form existing for nicotine except major part is existed in the form of nicotine salt, and some free nicotine is present, by these
Free nicotine carries out salt-forming reaction with the non-volatile organic acids contained in tobacco, and the nicotine contained in burley tobaccos is totally converted
Into the form of nicotine salt, then by adjust pH to 10-12 by Nicotine Conversion into molecular state form exist, using volume ratio be 4~
10 :1 n-hexane and the mixed extractant solvent of ethyl acetate, the higher nicotine of purity can be obtained, while also contained in product
There is the fragrance component of burley tobaccos.Smoked panel test in electronic smoke atomizer, it is simultaneously fragrant containing tobacco except there is the distinctive satisfaction of nicotine
Gas, closer to the sensation of traditional cigarette.
Except nicotine also has N- picolines formamide, indoles, 5,5- dimethyl pyrazoline and acetyl group in extract
These are distinctive compositions in burley tobaccos to pyridine, assign extract burley tobaccos fragrance.Benzofuranone, Megastigmatrienone, methyl
Heptenone and hydroxyl damascenone assign extract baking fragrance, therefore obtained extract is that the nicotine with burley tobaccos cigarette perfume carries
Take thing.
Activated carbon as a kind of porous adsorbing material, have good adsorption performance, pore structure is controllable, bioaffinity is good,
Have no toxic side effect, the advantages that, it is but relatively fewer as the research of carrier adsorption nicotine, and active powdered carbon is difficult to be directly used in electronics
In tobacco juice.Therefore we by activated carbon through modification, can it is dispersed/be dissolved in Alevaire, so as to nicotine, nicotine
The materials such as salt adsorb, and finally reach the effect of sustained release.
Traditional nicotine preparation method is to utilize steam distillation, and nicotine is as vapor steams together, needs to distill
Go out substantial amounts of water, the time is oversize, and energy consumption is higher.
The present invention is improved in traditional extracting method, and it is organic to use tartaric acid, malic acid and citric acid etc. instead
The free nicotine contained in offal is carried out salt-forming reaction by acid, then adjusts pH to 10-12 with sodium hydroxide solution, straight with organic solvent
Extraction is connect, organic phase, which concentrates, produces nicotine extract, while the also fragrance component containing burley tobaccos in product.In electronic cigarette atomizing
Smoked panel test in device, except there is the distinctive satisfaction of nicotine, contain tobacco aroma simultaneously, closer to the sensation of traditional cigarette；In electronics
Modified activated carbon is added in tobacco juice, can also make nicotine stabilization, equably discharge.
Embodiment
With reference to specific embodiment, the invention will be further described.Following examples be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
The tartaric acid solution that 80g U.S. SB4F offals are added to 800 milliliters of 10wt% heats 1h under 80 degree, after cooling, filtering filter
Slag, filtrate are 11 with 40% NaOH solution regulation pH, then with 800 milliliters of n-hexane+ethyl acetate（Volume ratio is 8:1）Extraction
Take 2 times, organic phase merges concentration and is evaporated, and obtains yellow liquid, this yellow liquid is dissolved in 20 milliliters of propane diols, obtains one
Kind can increase the electronic cigarette liquid of flue gas satisfaction.
The burley tobacco nicotine extract include nicotine 96.13%, cotinine 0.56%, N- picolines formamide 0.07%,
Benzofuranone 0.08%, indoles 0.06%, 5,5- dimethyl pyrazoline 0.04%, acetylpyridine 0.03%, Megastigmatrienone
0.03%th, methyl heptenone 0.02%, hydroxyl damascenone 0.02%, hexadecylic acid 0.02%, nornicotine 0.01%, other compositions
It is unknown.
1mL electronic cigarette liquids are taken to add in atomizer, the personnel that smoke panel test that please be professional smoke panel test, and there are certain burley tobaccos fragrant, there is cigarette
Grass baking fragrance, throat and nose can feel the distinctive impact sense of nicotine and satisfaction.
Modified activated carbon is added in above-mentioned electronic cigarette liquid, 1mg modified activated carbons are added in every gram of electronic cigarette liquid, it is modified to live
The preparation method of property charcoal is：
1st, activate：
Reagent：Activated carbon；Potassium permanganate；The concentrated sulfuric acid；Concentrated phosphoric acid；Hydrogen peroxide；Deionized water
（1）At room temperature, add in 250 mL round-bottomed flasks, stir after 200 mg activated carbon are mixed with the mg of potassium permanganate 1000
After uniformly, the 50 mL concentrated sulfuric acids-concentrated phosphoric acid mixed acid solution is added dropwise toward reaction bulb（Volume ratio is 3:1）, control rate of addition is appropriate,
So that reacting liquid temperature is controlled within 30 degrees Celsius in cold bath.
（2）After acid solution is added dropwise, reaction 24 hours under 50 degree are transferred in thermostat.
（3）After reaction terminates, reactant is naturally cooled into room temperature, in being then poured into 500 mL frozen water, stirring is lower to be added
Enter hydrogen peroxide to potassium permanganate aubergine to disappear, centrifuge and wash solid repeatedly with deionized water until its pH is in
Property.
2nd, it is polyethyleneglycol modified
Reagent：Polyethylene glycol 400；Toluene；P-methyl benzenesulfonic acid；Deionized water
Solid obtained by previous step is transferred in 100 mL round-bottomed flasks, the mg of p-methyl benzenesulfonic acid 100, the mL of toluene 10 is added, gathers
The mL of ethylene glycol 30；Build the back flow reaction device with oil water separator, back flow reaction 24 hours.After reaction terminates, decompression
Toluene is distilled off, gained residue is poured into 500 mL deionized waters, and after ultrasonic disperse and centrifugation, residual solids continue to spend
Ion water washing, centrifugal treating, until the close neutrality of pH value of solution.Collect solution and be freeze-dried to obtain modified activated carbon.
The electronic cigarette liquid for take addition respectively, not adding modified activated carbon is added in electronic smoke atomizer and aspirated, and takes out
Inhale capacity to be 55 milliliters, aspirate duration 3 seconds, square wave, suction frequencies 30s, aspirate 200 mouthfuls altogether, every 40 mouthfuls of flue gases are adsorbed onto one
Open on filter disc, organic solvent extraction, nicotine content and situation of change in every 40 mouthfuls of analysis.
Not plus during activated carbon, 1-40 mouths, 41-80 mouths, 81-120 mouths, 121-160 mouths, 161-200 mouths five
The nicotine content change in individual section（Decline percentage relative to the nicotine in a upper section）Situation is：17.8%、16.5%、14.7%、
25.3%。
When adding activated carbon, 1-40 mouths, 41-80 mouths, 81-120 mouths, 121-160 mouths, 161-200 mouths five
The nicotine content change in individual section（Decline percentage relative to the nicotine in a upper section）Situation is：6.5%、5.2%、4.7%、
20.1%。
The above results show, the release of the nicotine added after modified activated carbon is more uniform, stably at first 160 mouthfuls, due to electricity
The total amount of sub- tobacco juice limits, and the content of nicotine substantially reduces after the 160th mouthful.
Embodiment 2
The citric acid solution that two offals in 80g enshis are added to 600 milliliters of 15wt% heats 2h under 70 degree, after cooling,
Filter filter residue, filtrate with 30% KOH solution regulation pH for 11, then with 700 milliliters of n-hexane+ethyl acetate（Volume ratio 5:1）
Extraction 2 times, organic phase merge concentration and are evaporated, obtain yellow liquid, this yellow liquid is dissolved in 20 milliliters of propane diols, obtained
A kind of electronic cigarette liquid that can increase flue gas satisfaction.
1mL electronic cigarette liquids are taken to add in atomizer, the personnel that smoke panel test that please be professional smoke panel test, and there are certain burley tobaccos fragrant, there is cigarette
Grass baking fragrance, throat and nose can feel the distinctive impact sense of nicotine and satisfaction.Similarly, in above-mentioned electronic cigarette liquid
After middle addition modified activated carbon, also there is similar experimental data.
Claims (9)
1. a kind of burley tobacco nicotine extract, it is characterised in that by weight percent, the burley tobacco nicotine extract includes cigarette
Alkali 94-97%, cotinine 0.4-0.8%, N- picoline formamide 0.2-0.3%, benzofuranone 0.1-0.2%, indoles 0.1-
0.2%th, 5,5- dimethyl pyrazoline 0.1-0.2%, acetylpyridine 0.05-0.15%, Megastigmatrienone 0.05-0.1%, methyl
Heptenone 0.02-0.05%, hydroxyl damascenone 0.02-0.05%, hexadecylic acid 0.02-0.05%, nornicotine 0.01-0.04%.
2. a kind of extraction process of burley tobacco nicotine extract as claimed in claim 1, it is characterised in that including following step
Suddenly：Using the offal of burley tobaccos or/and pipe tobacco as raw material, raw material is placed in organic acid soln, at 70~90 DEG C extract 1~
2h, cooled and filtered, filtrate alkaline solution adjust pH value be 10~12, then with volume ratio be 4~10:1 n-hexane and second
The mixed extractant solvent of acetoacetic ester, organic phase are evaporated being concentrated under reduced pressure, and obtain burley tobacco nicotine extract；The organic acid soln
Mass fraction be 5%~15%.
3. technique as claimed in claim 2, it is characterised in that the alkaline solution is sodium hydroxide solution or/and hydroxide
Potassium solution.
4. technique as claimed in claim 2, it is characterised in that the organic acid soln is tartaric acid solution, citric acid solution
Or one or more of mixing in malic acid solution.
5. technique as claimed in claim 2, it is characterised in that the mass volume ratio of the raw material and organic acid soln is 1:5-
15（g/mL）.
6. a kind of electronic cigarette liquid that can uniformly discharge cigarette perfume, it is characterised in that the electronic cigarette liquid is included described in claim 1
Burley tobacco nicotine extract, aroma component, atomization composition and modified activated carbon；
The preparation method of the modified activated carbon is：After activated carbon is mixed with potassium permanganate in acid condition, reacted,
After the completion of reaction, remove excessive potassium permanganate, after obtained solid product is washed to neutrality with p-methyl benzenesulfonic acid and poly- second
Glycol carries out esterification, obtains modified activated carbon.
7. electronic cigarette liquid as claimed in claim 6, it is characterised in that the modified activated carbon comprises the following steps：
（1）By mass parts, the activated carbon of 100-500 parts and the potassium permanganate of 500-2000 parts are added into reaction bulb, toward reaction bulb
After middle dropwise addition acid solution, stir, 8-48 hours are reacted under 40-60 degree；
（2）After the completion of reaction, cooling, hydrogen peroxide is added up to the purplish red decoloration of potassium permanganate, reactant mixture is centrifuged, used
The solid that deionized water washing centrifugation obtains is until pH is neutrality；
（3）By step（2）Solid after washing mixes with the p-methyl benzenesulfonic acid of 50-200 parts and the polyethylene glycol of 30-60 parts, with
Toluene is reaction dissolvent, back flow reaction 15-30 hours, after reaction terminates, is evaporated under reduced pressure and removes toluene, gained residue is poured into
Centrifuged in ionized water after ultrasonic disperse, until the pH of solution is neutrality, collects solution and be freeze-dried to obtain modified activated carbon.
8. electronic cigarette liquid as claimed in claims 6 or 7, it is characterised in that the molecular weight of the polyethylene glycol is 200-600.
9. electronic cigarette liquid as claimed in claim 6, it is characterised in that modified active containing 0.1-10mg in every gram of electronic cigarette liquid
Charcoal.
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| CN107660811B (en) | 2021-02-23 |
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