CN107660817A - A kind of electronic cigarette liquid that can uniformly discharge cigarette perfume - Google Patents
A kind of electronic cigarette liquid that can uniformly discharge cigarette perfume Download PDFInfo
- Publication number
- CN107660817A CN107660817A CN201610600661.7A CN201610600661A CN107660817A CN 107660817 A CN107660817 A CN 107660817A CN 201610600661 A CN201610600661 A CN 201610600661A CN 107660817 A CN107660817 A CN 107660817A
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- electronic cigarette
- nicotine
- acid
- activated carbon
- cigarette liquid
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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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
-
- 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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The present invention provides a kind of electronic cigarette liquid that can uniformly discharge cigarette perfume, and the electronic cigarette liquid includes nicotine, 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 is added in electronic cigarette liquid and combined with nicotine, adsorbs the various composition in electronic cigarette liquid, reaches 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 that can uniformly discharge 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
It is similar, 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, electronics
Smoking set has following some principal characters：First, need not burn, greatly reduce because of tar caused by burning and harmful components, compare
Traditional cigarette harmfulness is smaller；Second, second-hand flue gas will not be produced, PE will not be had an impact, delayed to a certain extent
The contradiction of smoking and public place ban on opium-smoking and the opium trade is solved；Third, the physiological requirements of consumer can be adapted to and met to a certain extent.Electricity
Sub- cigarette develops by several generations, basically identical with traditional cigarette external form at present, and taste can realize variation, while electronic cigarette
In be free of tar, to human body injure it is 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 compared with regular-size cigarette, although
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 aspirating
Nicotine content is inconsistent, and stability is inadequate.Stimulation of the nicotine to throat is stronger when the 2nd, aspirating, and has throat hurt feeling.Such as：Chinese patent
CN104983063A (a kind of improved electronic cigarette liquid and preparation method thereof), electronics tobacco tar main component be electronic cigarette base fluid 10%~
90%, 1%~2% free nicotine, 1%~10% electronic cigarette essence, 0%~5% deionized water, surplus add glycerine, mixing
Completed electronic cigarette tobacco juice is obtained after 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 substituted using sparteine
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 cigarette
Alkali can be to people to enjoy, when people smoke tobacco leaf and its product, and primary is to obtain nicotine to expire people's physiological strength
The glamour of foot and cigarette perfume, therefore this patent has carried out free nicotine into the research in terms of salt and absorption, before solving free nicotine
The problems such as unstable afterwards and throat hurt feeling.Free nicotine and different organic acids and inorganic acid are subjected to salt-forming reaction, electronic cigarette
The existence form of nicotine is nicotine and the mixture of different nicotine salts in tobacco tar.
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
It 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
Lattice, turn into the preferred material of cigarette adsorbent, be at home and abroad widely used in cigarette market.Many passes existing at present
In research of the activated carbon as harm reduction adsorbent, but it is relatively fewer as the research of carrier adsorption nicotine, and activated carbon is by repairing
Decorations, can be dispersed in Alevaire.We design and are prepared for a kind of charcoal absorption of good dispersion property in this research
Material, nicotine carried out using sorbing material slow release method to stablize release.
The content of the invention
Present invention solves the technical problem that be, for the nicotine in existing electronic cigarette tobacco tar it is volatile, it is front and rear it is unstable with
And the problem of throat hurt feeling is stronger in aspiration procedure, propose nicotine when one kind can stablize release nicotine and cigarette perfume improves suction simultaneously
Mouthfeel effective ways.
The technical scheme is that, there is provided a kind of electronic cigarette liquid that can uniformly discharge cigarette perfume, the electronic cigarette liquid include
Nicotine, 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, carry out
Oxidation reaction, after the completion of oxidation reaction, remove excessive potassium permanganate, after obtained solid product is washed to neutrality with to first
Benzene sulfonic acid and polyethylene glycol carry out esterification, obtain modified activated carbon.
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 instead
Answer 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 50-200 parts p-methyl benzenesulfonic acid and 30-60 part polyethylene glycol, 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
Ultrasonic disperse, centrifugation in ionized water, until the pH of solution is neutrality, collects solution and be freeze-dried to obtain modified activated carbon.
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, the electronic cigarette liquid also contains nicotine salt.Nicotine salt be nicotine malate, nicotine citrate and
One or more in nicotine tartrate.
Further, the nicotine is prepared by following methods：Using offal or pipe tobacco as raw material, raw material is placed in organic
In acid solution, 2~6h, cooled and filtered are extracted at 70~90 DEG C, filtrate mass fraction is 40%~60% aqueous slkali
It is 10~12 to adjust pH value；This solution n-hexane or/and ethyl acetate are extracted, organic phase concentrates at low temperature, obtains nicotine.
Further, the organic acid is one or more of mixing in malic acid, citric acid, tartaric acid and lactic acid.
Further, component comprising following parts by weight：Alevaire 70-90 parts, nicotine 0.01-0.2 parts, aroma component
1-10 parts, modified activated carbon 0.01-0.1 parts.
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 compositions such as salt adsorb, and finally reach the effect of sustained release.
Because the structure of nicotine has a pyridine ring and a pyrrole ring, the easy matter of N atoms on the N atoms and pyridine ring of pyrrole ring
Sonization, N atoms wherein on pyrrole ring are easier to protonate, nicotine easily with H ions bindings, therefore most of cigarette in tobacco
Alkali 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.Malic acid, citric acid and tartaric acid may be selected
Salt-forming reaction is carried out with nicotine, is existed in the form of nicotine and nicotine salt, by obtained nicotine salt and nicotine in certain proportion
Allocated, the electronic cigarette liquid of different-style can also be obtained.
Combined the invention has the advantages that modified absorbent charcoal material is added in electronic cigarette liquid with nicotine, absorption electricity
The compositions such as the nicotine in sub- tobacco juice, reach the purpose of sustained release so that the equably release that nicotine can be stablized.
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, 100-250mL is added after 100-500mg activated carbon is mixed with potassium permanganate (500-2000mg)
In round-bottomed flask, after stirring, the 20-100mL concentrated sulfuric acids-concentrated phosphoric acid mixed acid solution (volume ratio 1 is added dropwise toward reaction bulb: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
10mL, polyethylene glycol 30mL；Build the back flow reaction device with oil water separator, back flow reaction 24 hours.After reaction terminates,
It is evaporated under reduced pressure and removes toluene, gained residue is poured into 500mL deionized waters, and after ultrasonic disperse and centrifugation, residual solids continue
It is washed with deionized, centrifugal treating, until the close neutrality of pH value of solution.Collect solution and be freeze-dried to obtain last modified outcome.
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 residue, filtrate adjust pH ＞ 11 with 40% KOH solution, then with 700 milliliters of n-hexane+ethyl acetate (5:1) extract 2 times,
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
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
Containing about 8mg nicotine, 2mg tartaric acid in liquid.Tartaric acid can form nicotine tartrate 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 electricity
Containing about 8mg nicotine, 2mg modified activated carbons in sub- tobacco juice.
Embodiment 5
Above-mentioned free nicotine, tartaric acid, modified activated carbon are dissolved in Alevaire (propane diols), electronic cigarette liquid is made, its
In in every gram of electronic cigarette liquid containing about 8mg nicotine, 1mg tartaric acid, 1mg modified activated carbons.
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 milliliters, suction duration 3 seconds, square wave, suction frequencies 30s, 200 mouthfuls of suction altogether, every 40 mouthfuls of flue gases are adsorbed onto on a filter disc,
Organic solvent extracts, nicotine content and situation of change in every 40 mouthfuls of analysis.Experimental result such as Fig. 1, in figure, each group of data are from a left side
It is followed successively by first 40 mouthfuls (1-40 mouths) to the right side, second 40 mouthfuls (41-80 mouths), the 3rd 40 mouthfuls (81-120 mouths),
4th 80 mouthfuls (121-200 mouths).According to the actual conditions of consumer, suck electronics mouth number not over 200 mouthful (one
It is secondary), due to being limited by electronic cigarette liquid total amount, the nicotine content of last electronic cigarette liquid can reduce substantially, therefore the 4th statistics
Last 80 mouthfuls.
Four kinds of nicotine form release conditions in flue gas are have studied, (A, B, C, D are embodiment 2, embodiment 4, C realities respectively
Apply example 3, the electronic cigarette liquid of D embodiments 5) electronic cigarette aspirates 200 mouthfuls altogether, from figure 1 it appears that second 40 mouthfuls of A groups sample
Decline 13.95%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second than first 40 mouthfuls and decline 9.20%；B group samples：Second 40 mouthfuls of ratio
First 40 mouthfuls decline 4.58%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second and decline 5.20%；C group samples：Second 40 mouthfuls of ratio
One 40 mouthfuls decline 8.26%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second and decline 8.82%, and last 80 mouthfuls of nicotine release is on the low side；D
Group sample：Second 40 mouthfuls of 40 mouthfuls of ratio first declines 5.76%, the 3rd 40 mouthfuls of 40 mouthfuls of ratio second and declines 5.87%.This 4
The most stable with B, D group nicotine content in kind sample, nicotine is using nicotine in the flue gas of modified activated carbon absorption in preceding 120 mouthfuls of phases
To stable, the sample for showing to add sorbing material in nicotine can relatively stablize release at first 120 mouthfuls or even first 200 mouthfuls.And A group samples
Product nicotine content in 80-120 mouth flue gases declines very fast.
Above-mentioned experiment shows, can be improved in electronic cigarette liquid with adding modified activated carbon or modified activated carbon+organic acid
The stability of nicotine, nicotine is set slowly stably to discharge.Because organic acid can not only be combined with nicotine, while can be pyrolyzed
Production is fragrant, and when being used cooperatively with modified activated carbon, the release variable quantity of nicotine is also more stable, it is possible to is partly lived instead of modified
Property charcoal be used for electronic cigarette liquid in.
Claims (8)
- A kind of 1. electronic cigarette liquid that can uniformly discharge cigarette perfume, it is characterised in that the electronic cigarette liquid include nicotine, aroma component, It is atomized 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, aoxidized React, after the completion of oxidation reaction, remove excessive potassium permanganate, after obtained solid product is washed to neutrality and to toluene sulphur Acid and polyethylene glycol carry out esterification, obtain 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, 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 until the purplish red decoloration of potassium permanganate, reactant mixture is centrifuged, gone Ion water washing is 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, 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 Ultrasonic disperse, centrifugation in ionized water, until the pH of solution is neutrality, collects solution and be 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 with it is dense The mix acid liquor of 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 active containing 0.1-10mg in every gram of electronic cigarette liquid Charcoal.
- 6. electronic cigarette liquid as claimed in claim 1, it is characterised in that the nicotine is prepared by following methods：With offal Or pipe tobacco is raw material, and raw material is placed in organic acid soln, 2~6h, cooled and filtered, filtrate matter are extracted at 70~90 DEG C It is 10~12 to measure the aqueous slkali that fraction is 40%~60% and adjust pH value；This solution n-hexane or/and ethyl acetate are extracted, it is organic Mutually concentrate at low temperature, obtain nicotine.
- 7. electronic cigarette liquid as claimed in claim 6, it is characterised in that the organic acid be malic acid, citric acid, tartaric acid and One or more of mixing in lactic acid.
- 8. electronic cigarette liquid as claimed in claim 1, it is characterised in that the component comprising following parts by weight：Alevaire 70-90 Part, nicotine 0.01-0.2 parts, aroma component 1-10 parts, modified activated carbon 0.01-0.1 parts.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610600661.7A CN107660817B (en) | 2016-07-27 | 2016-07-27 | Electronic cigarette liquid capable of uniformly releasing cigarette fragrance |
| CN202010907354.XA CN111920078B (en) | 2016-07-27 | 2016-07-27 | Modified activated carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610600661.7A CN107660817B (en) | 2016-07-27 | 2016-07-27 | Electronic cigarette liquid capable of uniformly releasing cigarette fragrance |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010907354.XA Division CN111920078B (en) | 2016-07-27 | 2016-07-27 | Modified activated carbon |
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| Publication Number | Publication Date |
|---|---|
| CN107660817A true CN107660817A (en) | 2018-02-06 |
| CN107660817B CN107660817B (en) | 2020-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610600661.7A Active CN107660817B (en) | 2016-07-27 | 2016-07-27 | Electronic cigarette liquid capable of uniformly releasing cigarette fragrance |
| CN202010907354.XA Active CN111920078B (en) | 2016-07-27 | 2016-07-27 | Modified activated carbon |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010907354.XA Active CN111920078B (en) | 2016-07-27 | 2016-07-27 | Modified activated carbon |
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| CN (2) | CN107660817B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110638082A (en) * | 2019-10-28 | 2020-01-03 | 武汉红金叶新材料科技有限公司 | Formulation suitable for heating non-combustion tobacco and preparation process thereof |
| 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 |
| CN113615862A (en) * | 2021-08-02 | 2021-11-09 | 深圳市真味生物科技有限公司 | Aromatic plant electronic atomized liquid and preparation method thereof |
| CN113854620A (en) * | 2021-09-02 | 2021-12-31 | 深圳市艾普生物科技有限公司 | Electronic cigarette liquid additive and preparation method and application thereof |
| RU2770830C1 (en) * | 2018-10-09 | 2022-04-22 | Джапан Тобакко Инк. | Method of producing tobacco flavoring liquid, tobacco flavoring liquid, method of producing an ester compound and a smoking article |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2770830C1 (en) * | 2018-10-09 | 2022-04-22 | Джапан Тобакко Инк. | Method of producing tobacco flavoring liquid, tobacco flavoring liquid, method of producing an ester compound and a smoking article |
| CN110638082A (en) * | 2019-10-28 | 2020-01-03 | 武汉红金叶新材料科技有限公司 | Formulation suitable for heating non-combustion tobacco and preparation process thereof |
| 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 |
| CN113615862A (en) * | 2021-08-02 | 2021-11-09 | 深圳市真味生物科技有限公司 | Aromatic plant electronic atomized liquid and preparation method thereof |
| CN113854620A (en) * | 2021-09-02 | 2021-12-31 | 深圳市艾普生物科技有限公司 | Electronic cigarette liquid additive and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107660817B (en) | 2020-10-30 |
| CN111920078B (en) | 2022-04-29 |
| CN111920078A (en) | 2020-11-13 |
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