CN104473321B - A kind of electronic smoke agent with tea perfume (or spice) and preparation method thereof - Google Patents
A kind of electronic smoke agent with tea perfume (or spice) and preparation method thereof Download PDFInfo
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- CN104473321B CN104473321B CN201410715919.9A CN201410715919A CN104473321B CN 104473321 B CN104473321 B CN 104473321B CN 201410715919 A CN201410715919 A CN 201410715919A CN 104473321 B CN104473321 B CN 104473321B
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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
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Abstract
A kind of electronic smoke agent with tea perfume (or spice) and preparation method thereof, belongs to electronic smoke agent technical field, comprises the steps: that tea leaf powder is broken to 10 ~ 100 orders by (1); (2) add organic solvent and carry out lixiviate; (3) leaching liquor reduced pressure concentration; (4) ethanol back dissolving, freezing dewaxing; (5) molecular clock.Its main component of gained tealeaves essential oil of the present invention is the volatile materials such as unrighted acid and terpene, can directly be atomized under the heating-up temperature of electronic cigarette, remain without high boiling substance, can use as Alevaire separately, also can use after propane diols or glycerine dilution.Described Alevaire in use, effectively can reduce the sweet soapy feeling of propane diols or glycerine, and give the delicate fragrance of electronic cigarette tealeaves, production technology is simple to operation, and production cost is lower, therefore has more the meaning and value of actual production simultaneously.
Description
Technical field
The invention belongs to electronic smoke agent technical field, be specifically related to a kind of electronic smoke agent with tea perfume (or spice) and preparation method thereof.
Background technology
Along with coming into effect of " Framework Convention on Tobacco Control ", smoking ban scope in public place, countries in the world progressively expands, and domestic and international tobacco consumption environment just profound change occurs.In recent years, electronic cigarette presents the gesture of growth fast, and world's electronic cigarette gross sales amount 2010 is 9.1 hundred million dollars, within 2011, is 12.8 hundred million dollars, within 2012, is 1,800,000,000 dollars, and within 2013, more than 2,500,000,000 dollars, average annual growth rate is up to about 40%.Wherein only at American market, within 2013, electronic cigarette gross sales amount is more than 1,000,000,000 dollars, increases nearly one times than last year.Tobacco juice for electronic smoke is generally formed by Alevaire, nicotine and flavor deployment, and conventional Alevaire is glycerine and propane diols.2009, FDA is in the research report of electronic cigarette, during 18 kinds of NJOYSmokingEverywhere electronic cigarettes are detected, find a kind of containing diethylene glycol (DEG), this may be the pollutant that in Alevaire, propane diols brings, and diethylene glycol (DEG) can cause kidney and nervous centralis infringement, mankind's oral lethal dose is about 1.0mL/kg.Although glycerine is nontoxic, propane diols is low toxicity, and a small amount of pollutant contained in the propane diols of different brackets still threatens to human health.Thus, reduce the consumption of propane diols or the Alevaire of development of new in Alevaire, the development for electronic cigarette is significant.
Tealeaves belongs to Theaceae Tea plant, arbor or shrub, widely cultivates in the many places of China.China's teas has green tea, black tea, yellow tea, the large class of white tea, blue or green tea and black tea six.Record according to " tea warp " Shennong's Herbal Compendium of Material Medica, tea flavour to cold, for drink is the most suitable, also pharmaceutically acceptable, can promote the production of body fluid quench one's thirst, spirit refreshing and eye-brightening, de-wearyly to overcome difficulties, clearing heat and detoxicating.Modern medicine and pharmacology achievement in research shows, containing the Multiple components such as Tea Polyphenols, alkaloid, protein, Tea Pigment, organic acid, tea saponin, vitamin and mineral matter in tealeaves, have anti-oxidant, scavenging free radicals, anti-inflammatory are antibacterial, radioresistance, Adjust-blood lipid and improve effect and the effects such as immunity of organisms.Meanwhile, tea extract is also widely used in the fields such as medicine, cosmetics, health products and food additives.
At present, the more concern Tea Polyphenols of the correlative study for tea extract, tea polysaccharide, alkaloidal extraction, and extracting method mostly is water extraction.Containing a large amount of water soluble ingredients such as carbohydrate, protein in water extraction gained medicinal extract, the oil-soluble ingredients loss with tealeaves feature perfume (or spice) is larger.In addition, containing a large amount of unrighted acids and terpene volatile oil component in tealeaves, these boiling point substances are lower, added in electronic cigarette cartridge, namely aerosolizable under lower heating-up temperature, also can give the delicate fragrance of electronic cigarette tealeaves simultaneously, thus can be used as Alevaire and use, thus reduce the use amount of propane diols and glycerine, and suppress the sweet soapy feeling of propane diols.
Summary of the invention
The object of the present invention is to provide a kind of electronic smoke agent with tea perfume (or spice) and preparation method thereof.
Based on above-mentioned purpose, this invention takes following technical scheme:
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that tea leaf powder is broken to 10 ~ 100 orders by (1); (2) add organic solvent and carry out lixiviate; (3) leaching liquor reduced pressure concentration, obtains tealeaves crude extract; (4) ethanol back dissolving, freezing dewaxing: the 95v% ethanol or the absolute ethyl alcohol that add 5 ~ 10 times of quality in gained tealeaves crude extract, fully stir and evenly mix, this solution is placed in 0 ~-20 DEG C, after insoluble matter is fully separated out, be separated, clear liquid reduced pressure concentration obtains tealeaves concentrate; (5) molecular clock: gained tealeaves concentrate can be separated by direct molecular clock, or add propane diols to dissolve, carry out molecular clock separation again after separation, the consumption adding propane diols is 1 ~ 3 times of tealeaves concentrate quality, described molecular clock condition: vacuum 10
-2~ 10
-3mbar, vapo(u)rizing temperature 50-140 DEG C, scraper plate rotating speed 150-300rpm, charging rate 1-5mL/min, collect light component after molecular clock is separated and namely obtain the electronic smoke agent with tea perfume (or spice).
Tealeaves in described step (1) is at least one in green tea, black tea, yellow tea, white tea, black tea, blue or green tea and reprocessing tea, and described reprocessing tea is a kind of reprocessing tea in green tea, black tea, yellow tea, white tea, black tea, blue or green tea or the reprocessing tea after two or more combination.
At least one in organic solvent benzinum in described step (2), ethyl acetate, ether, 95v% ethanol, absolute ethyl alcohol, feed liquid mass ratio is 1:6 ~ 10.
Lixiviate in described step (3) is the one in following method: surname extraction, each refluxing extraction 4 ~ 8 hours, extracts 1 ~ 2 time; Circumfluence distillation, extracts 1 ~ 2 time, each 1 ~ 3 hour; Ultrasonic assistant extracts, and ultrasonic frequency 30 ~ 60kHz, power 100 ~ 1000W, extraction time 30 ~ 60min, extraction temperature is 25 ~ 50 DEG C.
The electronic smoke agent of what said method obtained have tea perfume (or spice).
Maximum feature of the present invention is: provide a kind of Novel electric cigarette Alevaire, this Alevaire is from tealeaves, extract the volatile materials such as organic acid and terpene obtained, can directly be atomized under the heating-up temperature of electronic cigarette, remain without high boiling substance, directly can use, also can use after propane diols or glycerine dilution.Described Alevaire in use, effectively can reduce the sweet soapy feeling of existing Alevaire, gives the delicate fragrance of electronic cigarette tealeaves simultaneously.Production technology is simple to operation, and production cost is lower, therefore has more the meaning and value of actual production.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited thereto.
embodiment 1
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that green tea is crushed to 10 orders by (1); (2) add the ethyl acetate of 6 times of quality, circumfluence distillation 1h, extract 2 times; (3), after extraction terminates, leach leaching liquor with 400 order filter clothes, be evaporated to solvent-free taste, obtain tealeaves crude extract; (4) in step (3) gains, add the 95v% ethanol of 10 times of quality, fully stir and evenly mix, under-10 DEG C of conditions after freezing 12h, now insoluble matter is fully separated out, suction filtration, and clear liquid is evaporated to without alcohol taste, obtains tealeaves concentrate; (5) take above-mentioned concentrate, add the propane diols of 1 times of quality, mix rear centrifugal (4000rpm, 10min) and remove insoluble matter, molecular clock crossed by gained supernatant, and its condition is vacuum 10
-3mbar, vapo(u)rizing temperature 60 DEG C, scraper plate rotating speed 200rpm, charging rate 1.5mL/min, collect light component; Heavy constituent is molecular clock again, and vapo(u)rizing temperature is 90 DEG C, and other condition remains unchanged, and collects light component; Heavy constituent carries out molecular clock at 110 DEG C again, and other condition remains unchanged, and collects light component.
Take above-mentioned 60,90, the 110 DEG C of molecular clock light components obtained of 1.0g respectively, be diluted to 10wt% with propane diols, get 0.8g tri-kinds of light component infusion respectively in electronic cigarette cartridge.Smoke panel test through the above judging panel of 7 people, result shows: the amount of smoke of three kinds of light components is large, and the tealeaves delicate fragrance of 60,90 DEG C of light components is given prominence to, and 110 DEG C have light tea fragrant, greatly reduce the sweet soapy feeling of propane diols, above component all can use as the Alevaire of electronic cigarette.
embodiment 2
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that black tea powder is broken to 60 orders by (1); (2) accurately take a certain amount of tea-leaf power, wrap with filter paper, be placed in the apparatus,Soxhlet's of 1L volume, add the benzinum (60 ~ 90 DEG C) of 6 times of quality, termination 2L round-bottomed flask under apparatus,Soxhlet's, upper end connects condensing unit, and heating and refluxing extraction 8h extracts 1 time; (3) extract uses Rotary Evaporators decompression and solvent recovery after being cooled to room temperature, obtains tealeaves crude extract; (4) in crude extract, add the absolute ethyl alcohol of 8 times of quality, fully stir and evenly mix, be placed in freezing 24h under 0 DEG C of condition, now insoluble matter is fully separated out, suction filtration, and clear liquid is evaporated to without alcohol taste, obtains tealeaves concentrate; (5) take above-mentioned concentrate, be separated by molecular clock, its condition is vacuum 10
-2mbar, vapo(u)rizing temperature 80 DEG C, scraper plate rotating speed 300rpm, charging rate 5mL/min, collect light component.
Take the above-mentioned molecular clock light component of 0.8g, be directly all filled in electronic cigarette cartridge.Smoke panel test through the above judging panel of 7 people, evaluation result shows: compared with the electronic cigarette product on market, and amount of smoke is large, has obvious tealeaves delicate fragrance, and throat stimulates little, can be used as the substitute of existing Alevaire.
embodiment 3
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that white tea powder is broken to 100 orders by (1); (2) accurately take a certain amount of tea-leaf power, adopt ultrasonic method to extract, ultrasound condition: power 100W, frequency is 30kHz, and ultrasonic time and intermittent time are 3s/1s, extraction time 30min, Extraction solvent is 95v% ethanol, feed liquid mass ratio 1:10, and room temperature is extracted; (3) extraction terminates rear isolated by filtration, and filtrate reduced in volume is to 1/5 of original volume; (4) be placed on centrifugation (4000rpm, 20min) after-15 DEG C of freezing 15h in refrigerator, supernatant is evaporated to paste and obtains tealeaves concentrate; (5) take above-mentioned concentrate, be separated by molecular clock, its condition is vacuum 10
-2mbar, vapo(u)rizing temperature 120 DEG C, scraper plate rotating speed 140rpm, charging rate 1.5mL/min, collect light component.
Take the above-mentioned molecular clock light component of 1.0g, be diluted to 50wt% with propane diols, get 0.8g infusion in electronic cigarette cartridge.Smoke panel test through the above judging panel of 7 people, evaluation result shows: compared with the electronic smoke agent on market, and sweet soapy feeling reduces, and amount of smoke is moderate, has obvious tealeaves delicate fragrance, can be used as the substitute of existing Alevaire.
embodiment 4
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that black tea is crushed to 80 orders by (1); (2) accurately take a certain amount of tea-leaf power, adopt ultrasonic method to extract, ultrasound condition: power 1000W, frequency is 60kHz, and ultrasonic time and intermittent time are 3s/1s, and 50 DEG C are extracted 60min, and Extraction solvent is absolute ethyl alcohol, feed liquid mass ratio 1:8; (3) extraction terminates rear isolated by filtration, and filtrate reduced in volume is to 1/5 of original volume; (4) be placed on centrifugation (4000rpm, 20min) after-20 DEG C of freezing 15h in refrigerator, supernatant is evaporated to paste and obtains tealeaves concentrate; (5) take above-mentioned concentrate, be separated by molecular clock, its condition is vacuum 10
-2mbar, vapo(u)rizing temperature 140 DEG C, scraper plate rotating speed 150rpm, charging rate 1mL/min, collect light component.
Take the above-mentioned molecular clock light component of 1.0g, be diluted to 30wt% with propane diols, get 0.8g infusion in electronic cigarette cartridge.Smoke panel test through the above judging panel of 7 people, evaluation result shows: compared with the electronic smoke agent on market, and sweet soapy feeling reduces, and amount of smoke is moderate, has obvious tealeaves delicate fragrance, can be used as the substitute of existing Alevaire.
embodiment 5
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that black tea is crushed to 60 orders by (1); (2) accurately take a certain amount of tea-leaf power, wrap with filter paper, be placed in the apparatus,Soxhlet's of 1L volume, add the ether of 10 times of quality, lower termination 2L round-bottomed flask, upper end connects condensing unit, and 35 DEG C of heating and refluxing extraction 4h, extract 2 times; (3) use Rotary Evaporators decompression and solvent recovery after extract cooling, obtain tealeaves crude extract; (4) in crude extract, add the absolute ethyl alcohol of 5 times of quality, fully stir and evenly mix, freezing 24h under being placed in-10 DEG C of conditions, suction filtration immediately after taking out from refrigerator-freezer, clear liquid is evaporated to without alcohol taste, obtains tealeaves concentrate; (5) take above-mentioned concentrate, be separated by molecular clock, its condition is vacuum 10
-2mbar, vapo(u)rizing temperature 50 DEG C, scraper plate rotating speed 200rpm, charging rate 1.5mL/min, collect light component.
Take the above-mentioned molecular clock light component of 0.8g, be directly all filled in electronic cigarette cartridge.Smoke panel test through the above judging panel of 7 people, evaluation result shows: compared with the electronic cigarette product on market, and amount of smoke is large, has obvious tealeaves delicate fragrance, and throat stimulates little, can be used as the substitute of existing Alevaire.
embodiment 6
There is a preparation method for the electronic smoke agent of tea perfume (or spice), comprise the steps: that blue or green tea is crushed to 10 orders by (1); (2) add the ethyl acetate of 10 times of quality, circumfluence distillation 3h, extract 1 time; (3), after extraction terminates, leach leaching liquor with 400 order filter clothes, be evaporated to solvent-free taste, obtain tealeaves crude extract; (4) in crude extract, add the 95v% ethanol of 10 times of quality, fully stir and evenly mix, freezing 24h under-5 DEG C of conditions, filtrate reduced in volume, to without alcohol taste, obtains tealeaves concentrate; (5) take above-mentioned concentrate, add the propane diols of 3 times of quality, mix rear centrifugal (4000rpm, 10min) and remove insoluble matter, molecular clock crossed by gained supernatant, and its condition is vacuum 10
-3mbar, vapo(u)rizing temperature 60 DEG C, scraper plate rotating speed 200rpm, charging rate 1.5mL/min, collect light component.
Take the above-mentioned 60 DEG C of molecular clock light components obtained of 1.0g, glycerine is diluted to 50wt%, get 0.8g infusion in electronic cigarette cartridge, smoke panel test through the above judging panel of 7 people, result shows: the tealeaves delicate fragrance of 60 DEG C of light components is given prominence to, greatly reduce the sweet soapy feeling of glycerine, can use as the Alevaire of electronic cigarette.
Claims (5)
1. there is a preparation method for the electronic smoke agent of tea perfume (or spice), it is characterized in that, comprise the steps: that tea leaf powder is broken to 10 ~ 100 orders by (1); (2) add organic solvent and carry out lixiviate; (3) leaching liquor reduced pressure concentration, obtains tealeaves crude extract; (4) ethanol back dissolving, freezing dewaxing: the 95v% ethanol or the absolute ethyl alcohol that add 5 ~ 10 times of quality in gained tealeaves crude extract, fully stir and evenly mix, this solution is placed in 0 ~-20 DEG C, after insoluble matter is fully separated out, be separated, clear liquid reduced pressure concentration obtains tealeaves concentrate; (5) molecular clock: gained tealeaves concentrate can be separated by direct molecular clock, or add propane diols to dissolve, carry out molecular clock separation again after separation, the consumption adding propane diols is 1 ~ 3 times of tealeaves concentrate quality, described molecular clock condition: vacuum 10
-2~ 10
-3mbar, vapo(u)rizing temperature 50-140 DEG C, scraper plate rotating speed 150-300rpm, charging rate 1-5mL/min, collect light component after molecular clock is separated and namely obtain the electronic smoke agent with tea perfume (or spice).
2. the preparation method with the electronic smoke agent of tea perfume (or spice) according to claim 1, is characterized in that, the tealeaves in described step (1) is at least one in green tea, black tea, yellow tea, white tea, black tea and blue or green tea.
3. the preparation method with the electronic smoke agent of tea perfume (or spice) according to claim 1, it is characterized in that, organic solvent in described step (2) is at least one in benzinum, ethyl acetate, ether, 95v% ethanol, absolute ethyl alcohol, and feed liquid mass ratio is 1:6 ~ 10.
4. the preparation method with the electronic smoke agent of tea perfume (or spice) according to claim 1, is characterized in that, the lixiviate in described step (3) is the one in following method: surname extraction, each refluxing extraction 4 ~ 8 hours, extracts 1 ~ 2 time; Circumfluence distillation, extracts 1 ~ 2 time, each 1 ~ 3 hour; Ultrasonic assistant extracts, and ultrasonic frequency 30 ~ 60kHz, power 100 ~ 1000W, extraction time 30 ~ 60min, extraction temperature is 25 ~ 50 DEG C.
5. according to the electronic smoke agent with tea perfume (or spice) that the arbitrary described preparation method of Claims 1-4 obtains.
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Cited By (1)
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| CN105249524A (en) * | 2015-08-14 | 2016-01-20 | 贵州中烟工业有限责任公司 | Fragrance type heating nonflammable tobacco product and preparation method thereof |
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| CN107692318A (en) * | 2017-10-13 | 2018-02-16 | 上海烟草集团有限责任公司 | A kind of tobacco juice for electronic smoke and preparation method |
| CN110810581B (en) * | 2018-08-09 | 2023-10-13 | 湖南中烟工业有限责任公司 | Preparation process of tea extract |
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| CN105249524A (en) * | 2015-08-14 | 2016-01-20 | 贵州中烟工业有限责任公司 | Fragrance type heating nonflammable tobacco product and preparation method thereof |
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Address after: 450000 Yulin South Road, Henan, Zheng Dong, No. 16 South Road, Zhengzhou Patentee after: China Tobacco Henan Industrial Co., Ltd. Address before: 450000 Zhengzhou agricultural road, Henan, No. 29 Patentee before: China Tobacco Henan Industrial Co., Ltd. |