CN107660815A - A kind of electronic cigarette liquid of stable release cigarette perfume - Google Patents
A kind of electronic cigarette liquid of stable release cigarette perfume Download PDFInfo
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- CN107660815A CN107660815A CN201610600248.0A CN201610600248A CN107660815A CN 107660815 A CN107660815 A CN 107660815A CN 201610600248 A CN201610600248 A CN 201610600248A CN 107660815 A CN107660815 A CN 107660815A
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- nicotine
- electronic cigarette
- activated carbon
- cigarette liquid
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Abstract
The present invention provides a kind of electronic cigarette liquid of stable release cigarette perfume, and the electronic cigarette liquid includes nicotine, nicotine salt, 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, carried out esterification with p-methyl benzenesulfonic acid and polyethylene glycol after obtained solid product is washed to neutrality, obtain modified activated carbon.Modified absorbent charcoal material, organic acid are added in electronic cigarette liquid and combined with nicotine, the various composition in electronic cigarette liquid is adsorbed, forms nicotine salt, reach the purpose of sustained release so that the equably release that nicotine can be stablized.
Description
Technical field
The present invention relates to a kind of electronic cigarette liquid of stable release cigarette perfume, belong to electronic cigarette technical field.
Background technology
In recent years, the novel tobacco such as low temperature cigarette, electronic cigarette product is just in rapid rising.Electronic cigarette profile and common cigarette phase
Seemingly, it is that electronic cigarette liquid (also known as electronics tobacco tar, be a kind of fragrance solution) can be vaporized into the device of fog by one kind, to smoking
Person brings the sensation of similar smoking.
Electronic cigarette greatly reduces the injury to human body while people's tobacco habit is met.Generally, electronic smoking set
There are following some principal characters：First, need not burn, greatly reduce because of tar caused by burning and harmful components, compared to tradition
Cigarette harmfulness is smaller；Second, second-hand flue gas will not be produced, PE will not be had an impact, alleviated to a certain extent
Smoking and the contradiction of public place ban on opium-smoking and the opium trade；Third, the physiological requirements of consumer can be adapted to and met to a certain extent.Electronic cigarette passes through
Several generations development is crossed, it is basically identical with traditional cigarette external form at present, and taste can realize variation, while be free of in electronic cigarette
Tar, human body is injured smaller.Therefore, electronic cigarette is commercially received by increasing people.
But electronic cigarette has also progressively shown in place of some shortcomings.Study according to investigations, electronic cigarette is compared with regular-size cigarette, although shape
The perceptual image cigarette such as shape, feel, smog, but for smog caused by these electronic cigarette liquids in terms of fragrance, taste, it is and real
Cigarette perceptual difference away from larger, above-mentioned deficiency leverages the quality of electronic cigarette.The especially electronic cigarette containing nicotine, nicotine
Existence form be free nicotine mostly.Free state nicotine has 2 deficiencies in aspiration procedure：1st, it is volatile, before and after suction
Nicotine content it is inconsistent, stability is inadequate.Stimulation of the nicotine to throat is stronger when the 2nd, aspirating, and has throat hurt feeling.Such as：China
Patent CN104983063A (a kind of improved electronic cigarette liquid and preparation method thereof), electronics tobacco tar main component is electronic cigarette base fluid
10%~90%, 1%~2% free nicotine, 1%~10% electronic cigarette essence, 0%~5% deionized water, surplus add glycerine, mix
Completed electronic cigarette tobacco juice is obtained after closing uniformly.The throat hurt feeling of free nicotine and the phenomenon of inconsequent are generally existings during suction
The problem of.Chinese patent CN103284319A (utilizing oral cavity atomized liquid with cytosine replacing nicotine) is replaced using sparteine
For nicotine, the natural scents composition fragrance remaining time in the atomized liquid of oral cavity is longer, enhances the fragrance of electronic cigarette liquid.But only
Nicotine can be to people to enjoy, when people smoke tobacco leaf and its product, and primary is to obtain satisfaction of the nicotine to people's physiological strength
With the glamour of cigarette perfume, therefore this patent has carried out free nicotine into the research in terms of salt and absorption, solves before and after free nicotine not
The problems such as stable and throat hurt feeling.Free nicotine and different organic acids and inorganic acid are subjected to salt-forming reaction, in electronic cigarette tobacco tar
The existence form of nicotine is nicotine and the mixture of different nicotine salts.
In addition, absorption method is in terms of perfuming, have safely, hold that fragrant ability is strong, releases the characteristics of fragrant controllability, its key problem in technology is
The selection of porous material.In various new materials, activated carbon is because of its excellent absorption property, the cost price of relative moderate,
As the preferred material of cigarette adsorbent, at home and abroad it is widely used in cigarette market.It is existing much on work at present
Property research of the charcoal as harm reduction adsorbent, it is but relatively fewer as the research of carrier adsorption nicotine, and activated carbon is by modification, can
It is dispersed in Alevaire.We design and are prepared for a kind of active carbon adsorption material of good dispersion property in this research, profit
Nicotine carried out with sorbing material slow release method to stablize release.
The content of the invention
It is volatile, front and rear unstable and taking out for the nicotine in existing electronic cigarette tobacco tar present invention solves the technical problem that be
The problem of throat hurt feeling is stronger during suction, proposition is a kind of to stablize the mouthfeel of nicotine when discharging nicotine and cigarette perfume while improving suction
Effective ways.
The technical scheme is that, there is provided a kind of electronic cigarette liquid of stable release cigarette perfume, the electronic cigarette liquid include nicotine, cigarette
Alkali salt, 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, aoxidize instead
Should, after the completion of oxidation reaction, remove excessive potassium permanganate, after obtained solid product is washed to neutrality with p-methyl benzenesulfonic acid
Esterification is carried out with polyethylene glycol, obtains modified activated carbon.
Further, nicotine salt is the salt that nicotine is formed with acid；It is preferred that the salt formed with organic acid, i.e. nicotine acylate.
Further, the modified activated carbon comprises the following steps：
(1) mass parts are pressed, the activated carbon of 100-500 parts and the potassium permanganate of 500-2000 parts are added into reaction bulb, toward reaction
After acid solution is added dropwise in bottle, stir, 8-48 hours are reacted under 40-60 degree；
(2) react after the completion of, cooling, add hydrogen peroxide until potassium permanganate purplish red decoloration, by reactant mixture from
The heart, deionized water washing are until the pH of obtained solid is neutrality；
(3) solid after step (2) is obtained mixes with the p-methyl benzenesulfonic acid of 50-200 parts and the polyethylene glycol of 30-60 parts
Close, using toluene as reaction dissolvent, back flow reaction 15-30 hours, after reaction terminates, be evaporated under reduced pressure and remove toluene, gained is remaining
Thing is poured into ultrasonic disperse in deionized water, centrifugation, until the pH of solution is neutrality, collects solution and is freeze-dried to obtain modified active
Charcoal.
Further, the acid solution is that volume ratio is 1-9:1 concentrated sulfuric acid and the mix acid liquor of concentrated phosphoric acid.
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.
Further, nicotine salt containing 0.1-10mg in every gram of electronic cigarette liquid.
Further, the nicotine salt is nicotine malate, nicotine citrate, one kind in nicotine tartrate or several
Kind.
Further, component comprising following parts by weight：Alevaire 70-90 parts, nicotine 0.01-0.2 parts, aroma component 1-
10 parts, nicotine salt 0.01-0.1 parts, modified activated carbon 0.01-0.1 parts.
Activated carbon has good adsorption performance, pore structure is controllable, bioaffinity is good, nontoxic as a kind of porous adsorbing material
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 electronic cigarette liquid
In.Therefore we by activated carbon through modification, can it is dispersed/be dissolved in Alevaire, so as to nicotine, nicotine salt
Adsorbed Deng composition, finally reach the effect of sustained release.
Because the structure of nicotine has a pyridine ring and a pyrrole ring, the easy proton of N atoms on the N atoms and pyridine ring of pyrrole ring
Change, N atoms wherein on pyrrole ring are easier to protonate, and nicotine is therefore most of in tobacco easily with H ions bindings
Nicotine and citric acid or malic acid are combined into salt, exist in the form of proton state, and non-protonated free state nicotine content compared with
It is few, with the enhancing of tobacco alkalescence, the increase of non-protonated free state nicotine content.Organic acid such as malic acid, citric acid may be selected
Salt-forming reaction is carried out with tartaric acid and nicotine, is existed in the form of nicotine and nicotine salt, by obtained nicotine salt and nicotine with certain
Ratio allocated, the electronic cigarette liquid of different-style can also be obtained.
The invention has the advantages that adding in electronic cigarette liquid and being combined with nicotine modified absorbent charcoal material, organic acid, adsorb
The compositions such as the nicotine in electronic cigarette liquid, nicotine salt is formed, reach the purpose of sustained release so that what nicotine can be stablized equably releases
Put.
Brief description of the drawings
Tetra- kinds of nicotine forms of Fig. 1 discharge quantity research in electronic cigarette flue gas.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1：The preparation method of modified activated carbon
1st, activate：
Reagent：Activated carbon；Potassium permanganate；The concentrated sulfuric acid；Concentrated phosphoric acid；Hydrogen peroxide；Deionized water
(1) at room temperature, 100-250 is added after 100-500mg activated carbon is mixed with potassium permanganate (500-2000mg)
In mL round-bottomed flasks, after stirring, the 20-100mL concentrated sulfuric acids-concentrated phosphoric acid mixed acid solution is added dropwise toward reaction bulb, and (volume ratio is
1:1-9:1), control rate of addition appropriate so that reacting liquid temperature is controlled within 30 degrees Celsius in cold bath.
(2) after acid solution is added dropwise, it is transferred in thermostat in 50 degree of lower reaction 8-48 hours.
(3) after reaction terminates, reactant is naturally cooled into room temperature, is then poured into frozen water in (200-2000mL), stirs
Mix lower addition hydrogen peroxide to potassium permanganate aubergine to disappear, centrifuge and wash solid repeatedly with deionized water until its pH connects
Weakly acidic pH.
2nd, it is polyethyleneglycol modified
Reagent：Polyethylene glycol (MW=200-600)；Toluene；P-methyl benzenesulfonic acid；Deionized water
Solid obtained by previous step is transferred in 100mL round-bottomed flasks, adds p-methyl benzenesulfonic acid 50-200mg, toluene 10
ML, polyethylene glycol 30mL；Build the back flow reaction device with oil water separator, back flow reaction 24 hours.Reaction terminates
Afterwards, it is evaporated under reduced pressure and removes toluene, gained residue is poured into 500mL deionized waters, and after ultrasonic disperse and centrifugation, residual is solid
Body continues to be washed with deionized, centrifugal treating, until pH value of solution is close to neutrality.Solution is collected to be freeze-dried finally to modify
Product.
Embodiment 2
80g burley tobaccos offal is added to 600 milliliter 15% of tartaric acid solution and heats 2h under 70 degree, after cooling, filtering filter
Slag, filtrate adjust pH ＞ 11 with 40% KOH solution, then with 700 milliliters of n-hexane+ethyl acetate (5:1) 2 are extracted
Secondary, organic phase merges concentration and is evaporated, and obtains free nicotine.Nicotine composition in free nicotine contains more than 80%, it might even be possible to reaches
To 95%, wherein the aroma component also containing gas in tobacco.The composition of certain free nicotine can also be obtained by compounding.
Free nicotine is dissolved in Alevaire (propane diols), electronic cigarette liquid is made, wherein containing about 8mg in every gram of electronic cigarette liquid
Nicotine.
Embodiment 3
Above-mentioned free nicotine, tartaric acid are dissolved in Alevaire (propane diols), electronic cigarette liquid is made, wherein every gram of electronic cigarette liquid
In containing about 8mg nicotine, 2mg tartaric acid.The tartaric acid of addition can form tartaric acid nicotine salt with nicotine.
Embodiment 4
Above-mentioned free nicotine, modified activated carbon are dissolved in Alevaire (propane diols), electronic cigarette liquid is made, wherein every gram of electronics
Containing about 8mg nicotine, 2mg modified activated carbons in tobacco juice.
Embodiment 5
Above-mentioned free nicotine, tartaric acid, modified activated carbon are dissolved in Alevaire (propane diols), electronic cigarette liquid is made, wherein
Containing about 8mg nicotine, 1mg tartaric acid, 1mg modified activated carbons in every gram of electronic cigarette liquid.
Take 1mL embodiments 2-5 electronic cigarette liquid to add electronic smoke atomizer, smoked panel test by the specialty personnel that smoke panel test, it is as a result as follows：
Embodiment 6
Example 2-5 four kinds of electronic cigarette liquids, which are added in electronic smoke atomizer, respectively is aspirated, and pumping volume is 55 millis
Rise, aspirate duration 3 seconds, square wave, suction frequencies 30s, aspirating 200 mouthfuls altogether, every 40 mouthfuls of flue gases are adsorbed onto a filter disc
On, organic solvent extraction, nicotine content and situation of change in every 40 mouthfuls of analysis.Experimental result such as Fig. 1, in figure, each group
Data are from left to right followed successively by first 40 mouthfuls (1-40 mouths), second 40 mouthfuls (41-80 mouths), the 3rd 40 mouthfuls
(81-120 mouths), the 4th 80 mouthfuls (121-200 mouths).According to the actual conditions of consumer, electronics mouth number is sucked
Not over 200 mouthfuls (once), due to being limited by electronic cigarette liquid total amount, the nicotine content of last electronic cigarette liquid can drop
It is low obvious, therefore the 4th last 80 mouthfuls of statistics.
Four kinds of nicotine form release conditions in flue gas are have studied, (A, B, C, D are embodiment 2, embodiment 4, C respectively
The electronic cigarette liquid of embodiment 3, D embodiments 5) electronic cigarette aspirates 200 mouthfuls altogether, from figure 1 it appears that A groups sample
Two 40 mouthfuls of 40 mouthfuls of ratios first decline 13.95%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second and decline 9.20%；B group samples：
Second 40 mouthfuls of 40 mouthfuls of ratio first declines 4.58%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second and declines 5.20%；C group samples
Product：Second 40 mouthfuls of 40 mouthfuls of ratio first declines 8.26%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second and declines 8.82%, finally
80 mouthfuls of nicotine release is on the low side；D group samples：Second 40 mouthfuls of ratio first, 40 mouthfuls of decline, 5.76%, the 3rd 40 mouthfuls of ratio
Second 40 mouthfuls decline 5.87%.The most stable with B, D group nicotine content in this 4 kinds of samples, nicotine utilizes modified active
Nicotine is relatively stable at first 120 mouthfuls in the flue gas of charcoal absorption, shows to add the sample of sorbing material in nicotine at first 120 mouthfuls even
First 200 mouthfuls can relatively stablize release.And A groups sample nicotine content in 80-120 mouth flue gases declines comparatively fast.
Above-mentioned experiment shows, nicotine can be improved to add modified activated carbon or modified activated carbon+organic acid in electronic cigarette liquid
Stability, nicotine is set slowly stably to discharge.Because organic acid can not only be combined with nicotine, while production perfume can be pyrolyzed,
When being used cooperatively with modified activated carbon, it can also be tightly held by activated carbon, the release variable quantity of nicotine is also more stable, so nicotine
Salt partly can replace modified activated carbon to be used in electronic cigarette liquid.
Claims (8)
1. a kind of electronic cigarette liquid of stable release cigarette perfume, it is characterised in that the electronic cigarette liquid includes nicotine, nicotine salt, 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, oxidation reaction is carried out, after the completion of oxidation reaction, removes excessive potassium permanganate, esterification is carried out with p-methyl benzenesulfonic acid and polyethylene glycol after obtained solid product is washed to neutrality, obtains modified activated carbon.
2. electronic cigarette liquid as claimed in claim 1, 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, after acid solution is added dropwise into reaction bulb, stirred, 8-48 hours are reacted under 40-60 degree；
（2）After the completion of reaction, cooling, hydrogen peroxide is added until the purplish red decoloration of potassium permanganate, reactant mixture is centrifuged, deionized water is washed until the pH of obtained solid is neutrality；
（3）By step（2）Solid after obtaining mixes with the p-methyl benzenesulfonic acid of 50-200 parts and the polyethylene glycol of 30-60 parts, using toluene as reaction dissolvent, back flow reaction 15-30 hours, after reaction terminates, it is evaporated under reduced pressure and removes toluene, gained residue is poured into ultrasonic disperse in deionized water, centrifugation, until the pH of solution is neutrality, collects solution and is freeze-dried to obtain modified activated carbon.
3. the electronic cigarette liquid stated such as claim 2, it is characterised in that the acid solution is that volume ratio is 1-9:1 concentrated sulfuric acid and the mix acid liquor of concentrated phosphoric acid.
4. electronic cigarette liquid as claimed in claim 1 or 2, it is characterised in that the molecular weight of the polyethylene glycol is 200-600.
5. electronic cigarette liquid as claimed in claim 1, it is characterised in that modified activated carbon containing 0.1-10mg in every gram of electronic cigarette liquid.
6. electronic cigarette liquid as claimed in claim 1, it is characterised in that nicotine salt containing 0.1-10mg in every gram of electronic cigarette liquid.
7. electronic cigarette liquid as claimed in claim 1, it is characterised in that the nicotine salt is the one or more in nicotine malate, nicotine citrate, nicotine tartrate.
8. electronic cigarette liquid as claimed in claim 1, it is characterised in that the component comprising following parts by weight：Alevaire 70-90 parts, nicotine 0.01-0.2 parts, aroma component 1-10 parts, nicotine salt 0.01-0.1 parts, modified activated carbon 0.01-0.1 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610600248.0A CN107660815B (en) | 2016-07-27 | 2016-07-27 | Electronic cigarette liquid capable of stably releasing cigarette fragrance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610600248.0A CN107660815B (en) | 2016-07-27 | 2016-07-27 | Electronic cigarette liquid capable of stably releasing cigarette fragrance |
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| Publication Number | Publication Date |
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| CN107660815A true CN107660815A (en) | 2018-02-06 |
| CN107660815B CN107660815B (en) | 2020-09-11 |
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| CN201610600248.0A Active CN107660815B (en) | 2016-07-27 | 2016-07-27 | Electronic cigarette liquid capable of stably releasing cigarette fragrance |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113229521A (en) * | 2021-06-23 | 2021-08-10 | 张家港外星人新材料科技有限公司 | Electronic atomized liquid composition and packaging container thereof |
| CN114098137A (en) * | 2021-11-02 | 2022-03-01 | 深圳市真味生物科技有限公司 | Electronic atomized liquid and preparation method thereof |
| CN114252512A (en) * | 2020-09-21 | 2022-03-29 | 湖南中烟工业有限责任公司 | Method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt |
| CN114587008A (en) * | 2020-12-07 | 2022-06-07 | 深圳雾芯科技有限公司 | Electronic cigarette liquid and atomization device comprising same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114252512A (en) * | 2020-09-21 | 2022-03-29 | 湖南中烟工业有限责任公司 | Method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt |
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| CN114098137A (en) * | 2021-11-02 | 2022-03-01 | 深圳市真味生物科技有限公司 | Electronic atomized liquid and preparation method thereof |
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