WO2013004160A1 - Method for preparing electronic cigarette liquid - Google Patents

Method for preparing electronic cigarette liquid Download PDF

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Publication number
WO2013004160A1
WO2013004160A1 PCT/CN2012/078053 CN2012078053W WO2013004160A1 WO 2013004160 A1 WO2013004160 A1 WO 2013004160A1 CN 2012078053 W CN2012078053 W CN 2012078053W WO 2013004160 A1 WO2013004160 A1 WO 2013004160A1
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Prior art keywords
electronic cigarette
cigarette liquid
extract
minutes
propylene glycol
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PCT/CN2012/078053
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French (fr)
Chinese (zh)
Inventor
郑俊祥
郑志炫
Original Assignee
Zheng Junxiang
Zheng Zhixuan
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Application filed by Zheng Junxiang, Zheng Zhixuan filed Critical Zheng Junxiang
Publication of WO2013004160A1 publication Critical patent/WO2013004160A1/en

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/167Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303Plant extracts other than tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/10Devices using liquid inhalable precursors

Definitions

  • the invention relates to a method for preparing an electronic cigarette liquid. It belongs to the field of chemical preparation technology.
  • Electronic cigarette liquid (or electronic cigarette liquid) is currently a popular cigarette replacement product. There have been many literatures or patent reports on the formulation, preparation process, and health care functions of electronic cigarette liquid.
  • An electronic simulated cigarette atomization liquid disclosed in Chinese Patent No. 200910104922.6 is prepared by blending 25-90 parts of polyethylene glycol, 9-50 parts of propylene glycol, and 0.3-52 parts of taste taste modifier. Flavor and fragrance blending products.
  • Smokers generally reflect that although electronic cigarettes and cigarettes feel like cigarettes in shape, feel, smoke, etc., in terms of aroma, taste, etc., the difference in feeling with cigarettes is relatively large, especially products formulated with various flavors and fragrances. They are difficult to accept or get used to their aromas and tastes. In addition, at present, the aroma components of the electronic cigarette liquid are difficult to retain for a long time, and the best can only be stored for about half a year, and the 'smoke flavor' is very light or almost absent. This is also a problem generally reflected by users. These shortcomings have greatly affected the quality of e-cigarettes and also restricted the popularity and popularity of e-cigarettes.
  • the object of the present invention is to provide a method for preparing an electronic cigarette liquid, which is directed to the odor of the electronic cigarette liquid, the difference in taste, and the short fragrance time.
  • the method makes the natural aroma component in the tobacco leaf enter the electronic cigarette liquid, so that the aroma and taste of the electronic cigarette liquid are basically from the tobacco leaf, can be closer to the aroma of the cigarette, can better cater to the consumer's cigarette smoking sensation, and can also enter the tobacco.
  • the natural aroma components in the liquid stay longer.
  • the preparation of the solvent is to measure the amount of electronic cigarette liquid by 30-80% of propylene glycol and / or polyethylene glycol and 0.1-o. 5% Tween 80, the two are stirred and mixed for 20-40 minutes to obtain a uniformly mixed solvent;
  • the cocoa bean extract is obtained by pulverizing cocoa beans to 20-60 mesh, into an extraction tank with a sandwich, adding 3-10 times of distilled water of cocoa powder, soaking the cocoa powder for 30-90 minutes, and heating to a temperature of 80-90 ° C, heat extraction for 2-6 hours, release and filter the extract, the filter residue is used for other purposes, the filtrate is concentrated under reduced pressure to a specific gravity of 1.1-1.4 extract, that is, the cocoa bean extract;
  • the propylene glycol or polyethylene glycol solvent and Tween 80 are all medicinal or edible grades, and propylene glycol and polyethylene glycol may be used singly or in combination.
  • the tobacco leaves are directly extracted under relatively mild conditions.
  • the aroma components of the tobacco leaves directly enter the extract, and the second is to extract the tobacco leaves under mild conditions, which will avoid complicated Loss and destruction of some volatile or temperature-sensitive tobacco aroma components in the process and high-temperature concentration conditions.
  • the viscosity of the solvent such as propylene glycol or polyethylene glycol is large. Has a certain moisturizing properties and other characteristics, will have a better retention of aroma components.
  • Example 1 It is planned to prepare 500 liters of electronic cigarette liquid. Weigh 50 kg of tobacco leaves and put them into the extraction tank with interlayer; measure 350 liters of propylene glycol and 1 liter of Tween 80 respectively, pour Tween 80 into propylene glycol and stir for 30 minutes, and add the mixture to the extraction tank. The tobacco leaves were soaked for 50 minutes, then heated to 50 ° C by steaming into the interlayer, and after immersion for 4 hours, the extract was discharged and filtered to obtain a filtrate, and 18 kg of cocoa bean extract was added to the filtrate, and the mixture was stirred for 30 minutes. To the filtrate, propylene glycol was added to make up 500 liters of the preparation, and the mixture was stirred and mixed for 35 minutes to obtain the electronic cigarette liquid.
  • Example 2 plans to prepare 500 liters of electronic cigarette liquid. Weigh 50 kilograms of tobacco leaves and put them into the extraction tank with interlayer; firstly weigh propylene glycol and polyethylene glycol 380 liters in a ratio of 1:1, then weigh 1.5 liters of Tween 80 and pour Tween 80 Into the mixture of propylene glycol and polyethylene glycol and stirred for 40 minutes, added to the extraction tank soaked tobacco leaves for 60 minutes, then
  • the steam was heated to 60 ° C in the interlayer, and after immersion for 6 hours, the extract was discharged and filtered to obtain a filtrate.
  • 20 kg of cocoa bean extract was added to the filtrate, and the mixture was stirred for 40 minutes; then polyethylene was added to the filtrate.
  • the diol was made up to 500 liters and stirred for 30 minutes to obtain the electronic cigarette liquid.

Abstract

A method for preparing an electronic cigarette liquid. A tobacco of 5% to 20% w/v of the volume of the electronic cigarette liquid is weighed and put into an extraction canister. A prepared solvent is added into the extraction canister to soak the tobacco for 30 to 100 minutes, then heated to a temperature between 40°C and 60°C, and subjected to a warm-soaked extraction for two to eight hours before an extract solution is filtered. A cocoa extract of 1% to 10% w/v of the volume of the electronic cigarette liquid is added to the extract solution, which is then stirred and mixed for 20 to 40 minutes. Propylene glycol or polyethylene glycol is used to fill up to 100% by volume of the electronic cigarette liquid for which the preparation is intended, and then a product is acquired by stirring and mixing. The preparation method allows the natural aroma of the tobacco to be introduced into the electronic cigarette liquid, thereby allowing the aroma and taste of the liquid cigarette liquid to originate basically from the tobacco, thus mimicking closely the aroma of cigarettes for improved catering to the perception of smoking of a consumer, and allowing prolonged period of fragrance for natural aroma ingredients introduced into the electronic cigarette liquid.

Description

一种电子烟液的制备方法Method for preparing electronic cigarette liquid
技术领域 Technical field
本发明涉及一种电子烟液的制备方法。属于化工制备技术领域。 The invention relates to a method for preparing an electronic cigarette liquid. It belongs to the field of chemical preparation technology.
背景技术 Background technique
电子烟液(或称电子烟雾化液)是目前流行的香烟替代产品。关于电子烟液的调配处方、制备过程,以及其保健功能等方面,已经有许多的文献或专利报道。中国专利200910104922.6公开的一种电子模拟香烟雾化液,以聚乙二醇25-90份,丙二醇9-50份,以及口感味道调节剂0.3-52份调配而成,属于典型的香精香料调配产品。中国专利200910310536.2公开的电子香烟雾化液,以烟叶提取物3-5%w/v,烟草香精3-5%w/v,烟碱0-3%w/v,稳定剂0.2-1%w/v,增稠剂3-8%w/v,纯水5-10%w/v,丙二醇50-70%w/v,以及其它如磷酸可待因、扑尔敏等调配而成,虽然使用了烟叶提取物,但仍然是模仿香烟口味以烟叶提取物与其它香精香料调配的产品。由于越来越多的吸烟者开始接受使用电子烟代替香烟,用于这些电子烟的电子烟液的一些不足也就越来越明显。吸烟者普遍反映,电子烟与香烟相比,虽然形状、手感、烟雾等感觉像香烟,但在香气、口味等方面,与品香烟的感觉差距比较大,尤其以各种香精香料调配成的产品,他们难以接受或习惯其香气和口味。另外,目前电子烟液的香气成分难以长期保留,最好的也只能存放半年左右,'烟味'就很淡或几乎没有了,这也是使用者普遍反映的问题。这些不足,大大影响了电子烟的品质,同时也制约着电子烟的普及和流行。 Electronic cigarette liquid (or electronic cigarette liquid) is currently a popular cigarette replacement product. There have been many literatures or patent reports on the formulation, preparation process, and health care functions of electronic cigarette liquid. An electronic simulated cigarette atomization liquid disclosed in Chinese Patent No. 200910104922.6 is prepared by blending 25-90 parts of polyethylene glycol, 9-50 parts of propylene glycol, and 0.3-52 parts of taste taste modifier. Flavor and fragrance blending products. The electronic cigarette atomization liquid disclosed in Chinese Patent No. 200910310536.2, with tobacco leaf extract 3-5% w/v, tobacco flavor 3-5% w/v, nicotine 0-3% w/v, stabilizer 0.2 -1% w/v, thickener 3-8% w/v, pure water 5-10% w/v, propylene glycol 50-70% w/v, and other formulations such as codeine phosphate, chlorpheniramine, etc. Although it uses tobacco leaf extract, it is still a product that mimics the taste of cigarettes and blends tobacco leaf extract with other flavors and fragrances. As more and more smokers begin to accept the use of electronic cigarettes instead of cigarettes, some of the shortcomings of electronic cigarettes used in these electronic cigarettes are becoming more and more obvious. Smokers generally reflect that although electronic cigarettes and cigarettes feel like cigarettes in shape, feel, smoke, etc., in terms of aroma, taste, etc., the difference in feeling with cigarettes is relatively large, especially products formulated with various flavors and fragrances. They are difficult to accept or get used to their aromas and tastes. In addition, at present, the aroma components of the electronic cigarette liquid are difficult to retain for a long time, and the best can only be stored for about half a year, and the 'smoke flavor' is very light or almost absent. This is also a problem generally reflected by users. These shortcomings have greatly affected the quality of e-cigarettes and also restricted the popularity and popularity of e-cigarettes.
发明内容 Summary of the invention
本发明的目的是针对电子烟液存在的香气、口味差,以及留香时间短等不足,提供一种电子烟液的制备方法。该法使烟叶中的天然香气成分进入电子烟液,使电子烟液的香气、口味基本是来自烟叶的,能更接近香烟的香气,更能迎合消费者的品烟感觉,还能使进入烟液中的天然香气成分留香时间更长。 The object of the present invention is to provide a method for preparing an electronic cigarette liquid, which is directed to the odor of the electronic cigarette liquid, the difference in taste, and the short fragrance time. The method makes the natural aroma component in the tobacco leaf enter the electronic cigarette liquid, so that the aroma and taste of the electronic cigarette liquid are basically from the tobacco leaf, can be closer to the aroma of the cigarette, can better cater to the consumer's cigarette smoking sensation, and can also enter the tobacco. The natural aroma components in the liquid stay longer.
本发明按以下技术方案实施 The invention is implemented according to the following technical solutions
按计划制备一定量的电子烟液,称取电子烟液量(体积)5-20%(w/v)的烟叶(重量)投入提取罐,将配制好的溶媒加入到提取罐中浸泡烟叶30-lOO分钟,加热至40-60℃温浸提取2-8小时,过滤提取液得滤液,向滤液中加入电子烟液量的1-10%(w/v)的可可豆提取物,搅拌混合20-40分钟;再以丙二醇或聚乙二醇补足到lOO%计划制备的电子烟液体积,搅拌混合均匀即得产品。 Prepare a certain amount of electronic cigarette liquid as planned, weigh the tobacco (weight) of 5-20% (w/v) of the electronic cigarette liquid volume into the extraction tank, and add the prepared solvent to the extraction tank to soak the tobacco leaf 30. -100 minutes, heated to 40-60 ° C for 2-8 hours, the filtrate is filtered to obtain the filtrate, and the filtrate is added with 1-10% (w / v) of cocoa bean extract of the electronic cigarette liquid, stirred and mixed 20-40 minutes; then propylene glycol or polyethylene glycol to make up the volume of 100% of the electronic cigarette liquid prepared by the plan, stir and mix to obtain the product.
所述的溶媒的配制是分别量取电子烟液量30-80%的丙二醇和/或聚乙二醇及0.1-o.5%的吐温80,将二者搅拌混合20-40分钟,得到混合均匀的溶媒; The preparation of the solvent is to measure the amount of electronic cigarette liquid by 30-80% of propylene glycol and / or polyethylene glycol and 0.1-o. 5% Tween 80, the two are stirred and mixed for 20-40 minutes to obtain a uniformly mixed solvent;
所述的可可豆提取物,是将可可豆粉碎至20-60目,投入带夹层的提取罐,加入可可豆粉重量的3-10倍蒸馏水,浸泡可可豆粉30-90分钟,加热升温至80-90℃,保温提取2-6小时,放出并过滤提取液,滤渣留作它用,滤液减压浓缩至比重为1.1-1.4的浸膏,即得可可豆提取物; The cocoa bean extract is obtained by pulverizing cocoa beans to 20-60 mesh, into an extraction tank with a sandwich, adding 3-10 times of distilled water of cocoa powder, soaking the cocoa powder for 30-90 minutes, and heating to a temperature of 80-90 ° C, heat extraction for 2-6 hours, release and filter the extract, the filter residue is used for other purposes, the filtrate is concentrated under reduced pressure to a specific gravity of 1.1-1.4 extract, that is, the cocoa bean extract;
所述的丙二醇或聚乙二醇溶媒及吐温80,均为药用或食用级别,丙二醇和聚乙二醇可以单独用,也可以混合用。 The propylene glycol or polyethylene glycol solvent and Tween 80 are all medicinal or edible grades, and propylene glycol and polyethylene glycol may be used singly or in combination.
与公知技术相比的优点及积极效果 Advantages and positive effects compared to known techniques
以含吐温80的丙二醇或聚乙二醇溶媒作提取液,在比较温和的条件下直接提取烟叶,一是烟叶的香气成分直接进入提取液,二是在温和条件下提取烟叶,会避免复杂工序及高温浓缩条件下对某些易挥发或对温度比较敏感的烟叶香气成分的损失和破坏,另外,与其它常用的提取香气成分的溶媒比较,由于丙二醇或聚乙二醇等溶媒粘度大、有一定的保湿性能等特点,对香气成分会有更好的保留作用。本发明的产品经过大量客户使用后,一致反映口味接近香烟的口味,他们更喜欢这种产品,而且产品存放二至三年,香气仍然能很好的保留。 Using propylene glycol or polyethylene glycol solvent containing Tween 80 as the extract, the tobacco leaves are directly extracted under relatively mild conditions. First, the aroma components of the tobacco leaves directly enter the extract, and the second is to extract the tobacco leaves under mild conditions, which will avoid complicated Loss and destruction of some volatile or temperature-sensitive tobacco aroma components in the process and high-temperature concentration conditions. In addition, compared with other commonly used solvents for extracting aroma components, the viscosity of the solvent such as propylene glycol or polyethylene glycol is large. Has a certain moisturizing properties and other characteristics, will have a better retention of aroma components. After a large number of customers use the products of the present invention, they consistently reflect that the taste is close to the taste of the cigarette. They prefer the product, and the product is stored for two to three years, and the aroma is still well preserved.
具体实施方式 detailed description
实例1:计划制备500升的电子烟液。称取50公斤烟叶,投入带夹层的提取罐中;分别量取350升丙二醇和1升吐温80,将吐温80倒入丙二醇中并搅拌混合30分钟,将此混合液加入至提取罐中浸泡烟叶50分钟,然后向夹层中通入蒸汽加热升温至50℃,保温浸提4小时后,放出提取液并过滤得滤液,向滤液中加入18公斤可可豆提取物,搅拌混合30分钟,再向滤液中加入丙二醇补足至计划制备的500升,再搅拌混合35分钟,即得所述电子烟液。 Example 1: It is planned to prepare 500 liters of electronic cigarette liquid. Weigh 50 kg of tobacco leaves and put them into the extraction tank with interlayer; measure 350 liters of propylene glycol and 1 liter of Tween 80 respectively, pour Tween 80 into propylene glycol and stir for 30 minutes, and add the mixture to the extraction tank. The tobacco leaves were soaked for 50 minutes, then heated to 50 ° C by steaming into the interlayer, and after immersion for 4 hours, the extract was discharged and filtered to obtain a filtrate, and 18 kg of cocoa bean extract was added to the filtrate, and the mixture was stirred for 30 minutes. To the filtrate, propylene glycol was added to make up 500 liters of the preparation, and the mixture was stirred and mixed for 35 minutes to obtain the electronic cigarette liquid.
实例2计划制备500升的电子烟液。称取50公斤烟叶,投入带夹层的提取罐中;先量按1:1的比例量取丙二醇和聚乙二醇380升混合,再量取1.5升吐温80,将吐温80倒入丙二醇和聚乙二醇混合液中并搅拌混合40分钟,加入至提取罐中浸泡烟叶60分钟,然后 Example 2 plans to prepare 500 liters of electronic cigarette liquid. Weigh 50 kilograms of tobacco leaves and put them into the extraction tank with interlayer; firstly weigh propylene glycol and polyethylene glycol 380 liters in a ratio of 1:1, then weigh 1.5 liters of Tween 80 and pour Tween 80 Into the mixture of propylene glycol and polyethylene glycol and stirred for 40 minutes, added to the extraction tank soaked tobacco leaves for 60 minutes, then
向夹层中通入蒸汽加热升温至60℃,保温浸提6小时后,放出提取液并过滤得滤液,向滤液中加入20公斤可可豆提取物,搅拌混合40分钟;再向滤液中加入聚乙二醇补足至500升,搅拌混合30分钟,即得所述电子烟液。 The steam was heated to 60 ° C in the interlayer, and after immersion for 6 hours, the extract was discharged and filtered to obtain a filtrate. 20 kg of cocoa bean extract was added to the filtrate, and the mixture was stirred for 40 minutes; then polyethylene was added to the filtrate. The diol was made up to 500 liters and stirred for 30 minutes to obtain the electronic cigarette liquid.

Claims (4)

  1. 一种电子烟液的制备方法,其特征在于:其按以下技术方案实施,称取电子烟液量5-20%w/v的烟叶投入提取罐,将配制好的溶媒加入到提取罐中浸泡烟叶30-100分钟后加热至40-60℃温浸提取2-8小时,过滤提取液,向滤液中加入电子烟液量的1-10%w/v的可可豆提取物,搅拌混合20-40分钟,再以丙二醇或聚乙二醇补足到100%计划制备的电子烟液体积,搅拌混合均匀即得产品。The invention relates to a method for preparing an electronic cigarette liquid, which is characterized in that it is implemented according to the following technical scheme, and the tobacco leaves with the amount of electronic cigarette liquid 5-20% w/v are weighed into an extraction tank, and the prepared solvent is added to the extraction tank for soaking. After 30-100 minutes, the tobacco leaves are heated to 40-60 ° C for 2-8 hours, and the extract is filtered. To the filtrate, 1-10% w/v of cocoa bean extract is added to the filtrate, and the mixture is stirred and mixed 20- 40 minutes, then propylene glycol or polyethylene glycol to make up 100% of the planned preparation of e-liquid volume, stir and mix to obtain the product.
  2. 根据权利要求1所述的电子烟液的制备方法,其特征在于:所述的溶媒的配制是分别量取电子烟液体积量的30-80%的丙二醇和/或聚乙二醇及0.1-0.5%的吐温80,将二者搅拌混合20-40分钟,得到混合均匀的溶媒。The method for preparing an electronic cigarette liquid according to claim 1, wherein the solvent is prepared by separately measuring 30-80% of the volume of the electronic cigarette liquid of propylene glycol and/or polyethylene glycol and 0. 1-0.5% Tween 80, and the two are stirred and mixed for 20-40 minutes to obtain a uniformly mixed solvent.
  3. 根据权利要求1所述的电子烟液的制备方法,其特征在于:所述的可可豆提取物,是将可可豆粉碎至20-60目,投入带夹层的提取罐,加入可可豆粉重量的3-10倍蒸馏水,浸泡可可豆粉30-90分钟,加热升温至80-90~C,保温提取2-6小时,放出并过滤提取液,滤液减压浓缩至比重为1.1-1.4的浸膏,即得可可豆提取物。The method for preparing an electronic cigarette liquid according to claim 1, wherein the cocoa bean extract is obtained by pulverizing cocoa beans to 20-60 mesh, into an extraction tank with a sandwich, and adding the weight of the cocoa powder. 3-10 times distilled water, soak the cocoa bean powder for 30-90 minutes, heat to 80-90~C, heat-extract for 2-6 hours, release and filter the extract, and concentrate the filtrate under reduced pressure to a specific gravity of 1.1-1. 4 of the extract, that is, the extract of cocoa beans.
  4. 根据权利要求1所述的电子烟液的制备方法,其特征在于:所述的丙二醇或聚乙二醇溶媒及吐温80,均为药用或食用级别,丙二醇和聚乙二醇单独用或混合用。The method for preparing an electronic cigarette liquid according to claim 1, wherein the propylene glycol or polyethylene glycol solvent and Tween 80 are all of a medicinal or edible grade, and propylene glycol and polyethylene glycol are used alone or Mixed.
PCT/CN2012/078053 2011-07-04 2012-07-02 Method for preparing electronic cigarette liquid WO2013004160A1 (en)

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CN2011101840686A CN102349699B (en) 2011-07-04 2011-07-04 Preparation method for electronic cigarette liquid
CN2011101840686 2011-07-04

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