CN106723303B - A kind of method that wet pulverizing prepares tobacco flavor electronics tobacco tar - Google Patents

Abstract

The invention provides a method for preparing tobacco-flavored electronic cigarette oil by wet pulverization, which includes the following steps: (1) Accurately weigh a certain amount of dry tobacco, pass through a 5-50 mesh sieve after primary pulverization, and add a certain amount of tobacco to the primary pulverization tobacco. proportion of the solvent, mixed evenly, added to the high-speed cutting wet pulverizer, pulverized under certain reaction conditions, and discharged after pulverization, the discharged liquid is the tobacco-flavored e-cigarette oil base oil; (2) The mass percentage is Stir and mix 50-100% of the tobacco-flavored e-liquid base oil and 0-50% by mass of flavors and fragrances to obtain tobacco-flavored e-liquid. Compared with the prior art, the method for preparing tobacco-flavored e-liquid by wet pulverization provided by the present invention is quick and easy, simple to operate, high in extraction rate, energy-saving and environment-friendly. The sensory quality of the e-liquid prepared from the tobacco-flavored base oil prepared by the method of the present invention is greatly improved, effectively reducing the sweet and greasy feeling in the mouth caused by the e-liquid, and alleviating dry mouth and tongue after smoking symptoms.

Description

A method for preparing tobacco-flavored electronic cigarette oil by wet pulverization

technical field

The invention relates to the technical field of e-liquid for electronic cigarettes, in particular to a method for preparing tobacco-flavored e-liquid by wet pulverization.

Background technique

In recent years, with the increasingly severe international tobacco control and the general improvement of consumers' health awareness, countries around the world have successively restricted the sales of traditional cigarettes through legislation, and the international cigarette sales have maintained a decline of 3%. Under this background, domestic and foreign tobacco companies continue to promote The development of new tobacco products, among which electronic cigarettes, as an important form of new tobacco products, has achieved rapid development. E-cigarette is a non-combustible tobacco substitute product, which has a similar appearance to cigarettes. Electronic cigarette liquid produces mist under the action of an electronic cigarette atomizer, which is similar to real smoke, satisfying the pleasure of consumers and usage habits, but it is essentially different from cigarettes. It does not burn, does not contain tar, carbon monoxide and other harmful substances.

According to actual consumer experience, although e-cigarettes feel like cigarettes in shape, feel, and smoke, the smoke produced by e-cigarette oil has a large gap with real cigarettes in terms of aroma and taste, which greatly affects the quality of e-cigarettes. Quality also restricts the popularization and popularity of electronic cigarettes. In order to solve this technical problem, most of the industry adopts adding tobacco extract to e-cigarette oil. Traditional tobacco extracts are mainly extracted from tobacco leaves or shredded tobacco with ethanol or water under reflux at a certain temperature, which makes it difficult to extract the burnt aroma in tobacco leaves. Patent 201410263756.5 provides a Maillard reaction product of tobacco leaf extract, but the reaction process of Maillard reaction is complicated, there are many intermediate products, and the influencing factors are difficult to control; patent 201410721776.2 provides a method for preparing light components of tobacco extract , the reaction has disadvantages such as complex operation, low extraction rate, and large loss of active ingredients, and the sensory quality of the extract prepared by the traditional method in the e-cigarette oil cannot well meet the requirements of consumers. At the same time, most consumers will experience discomfort such as dry mouth and tongue after smoking e-cigarettes, and even dizziness and nausea in severe cases. This problem also needs to be improved urgently.

Contents of the invention

In order to overcome the deficiencies of the prior art, the present invention provides a method for preparing tobacco-flavored e-liquid by wet pulverization. The preparation method is fast and simple, has high extraction rate and purity, and low cost. The specific preparation method includes the following steps:

(1) Accurately weigh 100 g of dry tobacco, pass it through a 5-50 mesh screen after primary crushing, add solvent to the primary crushed tobacco, the mass ratio of the tobacco to solvent is 1:5-10, mix well Put it into a high-speed cutting type wet pulverizer, pulverize under certain reaction conditions, and discharge the material after pulverization, and the discharged liquid is tobacco-flavored e-cigarette oil base oil; wherein the certain reaction conditions are the high-speed cutting type wet pulverizer The speed of the pulverizer is 2500~8000 r/min, the pulverization temperature is 5~60 ℃, and the pulverization time is 0.5~6 h;

(2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 50-100% and flavors and fragrances with a mass percentage of 0-50% to obtain tobacco-flavored e-liquid;

The tobacco-flavored e-cigarette oil base oil also includes a drug extract with the effect of promoting body fluid and quenching thirst, and the mass ratio of the drug extract to tobacco is 1-5:10; the drug extract having the effect of promoting body fluid and quenching thirst is composed of It is obtained by extracting one or two kinds of mulberry, pomegranate, grass jelly, ebony, olive, human face, vinegar willow fruit, golden club hammer, and yahuazi.

Preferably, in step (1), the solvent includes the following components, by mass percentage: 20-70% of glycerol, 20-75% of propylene glycol, 0-15% of ethanol, and the balance is deionized water Make up to 100% by weight.

Preferably, the speed of the high-speed cutting wet pulverizer is 4000~6000 r/min, specifically 4000~4500 r/min, 4000~5000 r/min, 4000~5500 r/min, 4500~5000 r/min /min, 4500~5500 r/min, 4500~6000 r/min, 5000~5500 r/min, 5000~6000 r/min, 5500~6000 r/min, 4000 r/min, 4200 r/min, 4500 r /min, 4800 r/min, 5000 r/min, 5200 r/min, 5500 r/min, 5800 r/min, 6000 r/min; crushing temperature is 10~25 ℃, specifically 10~15 ℃, 10 ~20 ℃, 15~20 ℃, 15~25 ℃, 20~25 ℃, 10 ℃, 12 ℃, 15 ℃, 18 ℃, 20 ℃, 22 ℃, 25 ℃; crushing time is 1~4 h, specific 1~2h, 1~3h, 2~3h, 2~4h, 3~4h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h.

Preferably, in step (1), the solvent includes the following components, by mass percentage: 30-50% of glycerol, 40-60% of propylene glycol, 5-10% of ethanol, and the balance is deionized water Make up to 100% by weight.

Preferably, the mass ratio of the medicinal extract having the effect of promoting body fluid and quenching thirst to tobacco is 2-4:10, such as 2:10, 2.5:10, 3:10, 3.5:10, 4:10.

Preferably, the tobacco is one of flue-cured tobacco, Burley tobacco, oriental tobacco, air-cured tobacco, cigar tobacco or yellow flower tobacco.

Another object of the present invention is to provide a tobacco-flavored electronic cigarette liquid prepared according to the method for preparing tobacco-flavored electronic cigarette liquid by wet pulverization.

Compared with the prior art, the method for preparing tobacco-flavored e-liquid by wet pulverization provided by the present invention is a fast, simple, efficient and energy-saving new method for preparing tobacco-flavored e-liquid. This method has the following advantages:

(1) The operation is simple, fast, and the time is short, and the biologically active components and aroma components of tobacco are retained to the greatest extent, which is conducive to the production of high-quality extracts;

(2) No longer undergoing heating and reflux treatment, which reduces the loss of active ingredients in the extraction process, especially the loss of aroma components, and improves the utilization rate of raw materials;

(3) Both the large particles are strictly limited, and over-crushing is avoided. The particle size distribution of the obtained tobacco ultrafine powder is uniform, which greatly increases the specific surface area of the ultrafine powder, and shortens the diffusion of tobacco components from the tobacco particles. The distance to the surface of the particle increases the leaching rate of tobacco content;

(4) The crushing is carried out in a closed system, which not only avoids the pollution of the environment by the fine powder, but also prevents the dust in the air from polluting the product.

In addition, compared with the e-liquid made of tobacco extract, the sensory quality of the tobacco powder e-liquid produced by this method has been greatly improved, and it can better meet the requirements of consumers, such as more delicate and smooth taste, realistic aroma, and no aftertaste. Irritation; and the e-liquid base oil is mixed with jellyfish, black plum and other ingredients that have the effect of promoting body fluid and quenching thirst, which can effectively reduce the sweetness and greasy feeling brought by solvents such as propylene glycol and glycerin, and relieve consumers after smoking e-cigarettes. Symptoms of dry mouth.

Detailed ways

Below in conjunction with specific embodiment, the present invention is further described:

Example 1

(1) Accurately weigh 100 g of dried flue-cured tobacco, pass through a 5-50 mesh screen after primary crushing, and add 500 g of solvent to the primary crushed flue-cured tobacco. The solvent includes the following components, calculated by mass percentage: glycerol 20%, propylene glycol 75%, ethanol 2%, the balance is made up to 100% by weight with deionized water, then add 20 g of mulberry and olive mixed extracts, mix well and add to a high-speed cutting wet pulverizer to control high-speed cutting The rotation speed of the type wet pulverizer is 4000 r/min, the pulverization temperature is 20 ℃, and the pulverization time is 6 h. After pulverization, the material is discharged, and the discharged liquid is the base oil of tobacco-flavored e-cigarette oil;

(2) Stir and mix the 50% by mass tobacco-flavored e-liquid base oil and 50% by mass flavor and fragrance to obtain tobacco-flavored e-liquid.

Example 2

(1) Accurately weigh 100 g of dried Burley tobacco, pass through a 5-50 mesh sieve after primary crushing, and add 1000 g of solvent to the primary crushed Burley tobacco. The solvent includes the following components, by mass percentage Total: 30% glycerol, 60% propylene glycol, 5% ethanol, the balance is made up to 100% by weight with deionized water, then add 10 g of pomegranate and human face mixed extract, mix well and add high-speed cutting type wet crushing In the machine, control the speed of the high-speed cutting wet pulverizer to 5000 r/min, the pulverization temperature to 25 °C, and the pulverization time to 2 h. After pulverization, the material is discharged, and the discharged liquid is the base oil of tobacco-flavored e-cigarette oil;

(2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 60% and the flavor and fragrance with a mass percentage of 40% to obtain a tobacco-flavored e-liquid.

Example 3

(1) Accurately weigh 100 g of dried oriental tobacco, pass through a 5-50 mesh screen after primary crushing, and add 600 g of solvent to the primary crushed oriental tobacco. The solvent includes the following components, calculated by mass percentage: Glycerol 50%, propylene glycol 30%, ethanol 15%, the balance is made up to 100% by weight with deionized water, then add 50 g of mixed extracts of grass jelly and vinegar willow fruit, mix well and add high-speed cutting wet crushing In the machine, the speed of the high-speed cutting wet pulverizer is controlled to be 8000 r/min, the pulverization temperature is 10 °C, and the pulverization time is 0.5 h. After pulverization, the material is discharged, and the discharged liquid is the tobacco-flavored e-cigarette oil base oil;

(2) Stir and mix the 70% by mass tobacco-flavored e-liquid base oil and 30% by mass flavor and fragrance to obtain tobacco-flavored e-liquid.

Example 4

(1) Accurately weigh 100 g of dried cigars, pass through a 5-50 mesh screen after primary crushing, and add 800 g of solvent to the primary crushed cigars. The solvent includes the following components, calculated by mass percentage: Glycerol 60%, propylene glycol 25%, ethanol 12%, and the balance is made up to 100% by weight with deionized water, then add 30 g of golden rod hammer mixed extract, mix well and add in high-speed cutting type wet pulverizer, control The speed of the high-speed cutting wet pulverizer is 6000 r/min, the pulverization temperature is 5°C, and the pulverization time is 3 h. After pulverization, the material is discharged, and the discharged liquid is the tobacco-flavored e-cigarette oil base oil;

(2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 80% and the flavor and fragrance with a mass percentage of 20% to obtain a tobacco-flavored e-liquid.

Example 5

(1) Accurately weigh 100 g of dry air-cured tobacco, pass through a 5-50 mesh screen after primary crushing, and add 700 g of solvent to the primary crushed air-cured tobacco. The solvent includes the following components, calculated by mass percentage: Glycerol 57%, propylene glycol 40%, and the balance is made up to 100% by weight with deionized water, then add 40 g of vinegar willow fruit and human face mixed extract, mix well and add to a high-speed cutting type wet pulverizer, control The speed of the high-speed cutting wet pulverizer is 5500 r/min, the pulverization temperature is 60 °C, and the pulverization time is 1 h. After pulverization, it is discharged without adding flavors and fragrances. The discharged liquid is tobacco-flavored e-liquid.

Example 6

(1) Accurately weigh 100 g of dried tobacco, pass through a 5-50 mesh screen after primary crushing, and add 550 g of solvent to the primary crushed tobacco. The solvent includes the following components, calculated by mass percentage: Glycerol 50%, propylene glycol 35%, ethanol 3%, the balance is made up to 100% by weight with deionized water, then add 15 g of pomegranate extract, mix well and add to a high-speed cutting wet pulverizer to control high-speed cutting The rotation speed of the type wet pulverizer is 4500 r/min, the pulverization temperature is 55 ℃, and the pulverization time is 2.5 h. After pulverization, the material is discharged, and the discharged liquid is the tobacco-flavored e-cigarette oil base oil;

(2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 90% and the flavor and fragrance with a mass percentage of 10% to obtain a tobacco-flavored e-liquid.

Example 7

(1) Accurately weigh 100 g of dried cigars, pass through a 5-50 mesh screen after primary crushing, and add 750 g of solvent to the primary crushed cigars. The solvent includes the following components, calculated by mass percentage: 70% glycerol, 20% propylene glycol, 8% ethanol, and make up the balance to 100% by weight with deionized water, then add 25 g of mixed extracts of grass jelly and pomegranate, mix well and add to a high-speed cutting wet pulverizer , control the speed of the high-speed cutting wet pulverizer to 2500 r/min, the pulverization temperature to 22°C, and the pulverization time to 4 h. After pulverization, the material is discharged, and the discharged liquid is the base oil of tobacco-flavored e-cigarette oil;

(2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 65% and the flavor and fragrance with a mass percentage of 35% to obtain a tobacco-flavored e-liquid.

Example 8

(1) Accurately weigh 100 g of dried Burley tobacco, pass through a 5-50 mesh sieve after primary crushing, and add 500 g of solvent to the primary crushed Burley tobacco. The solvent includes the following components, by mass percentage Total: 45% glycerol, 42% propylene glycol, 10% ethanol, and make up the balance to 100% by weight with deionized water, then add 35 g of mixed extracts of black plum and twig flower, mix well and add high-speed cutting type wet crushing In the machine, the speed of the high-speed cutting wet pulverizer is controlled to be 3500 r/min, the pulverization temperature is 15 °C, and the pulverization time is 5 h. After pulverization, the material is discharged, and the discharged liquid is the tobacco-flavored e-cigarette oil base oil;

(2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 95% and the flavor and fragrance with a mass percentage of 5% to obtain a tobacco-flavored e-liquid.

Comparative example 1

Tobacco-flavored e-cigarette oil was prepared according to the ratio of the components in Example 1, except that the flue-cured tobacco extract was the Maillard reaction product of flue-cured tobacco, and the mixed extract of mulberry and olive was not added to the base oil. Concrete: (1) first take the flue-cured tobacco leaves and chop them up, heat and extract with water or 95% ethanol as a solvent, obtain the tobacco extract through hot filtration and refrigerated sedimentation filtration, and concentrate to obtain the tobacco leaf extract; (2) then weigh the weight ratio Tobacco paste: 5 g of tobacco paste mixture with amino acid content of 10-2:1, weigh 100 g of solvent, put the tobacco paste and amino acid into the solvent, and then heat at 80-120 °C for 3-12 h to obtain tobacco leaves. Maillard reaction product. Take by weighing 100 g of the above-mentioned flue-cured tobacco extract, add 500 g of solvent to the flue-cured tobacco extract, and the solvent includes the following components, by mass percentage: 20% of glycerol, 75% of propylene glycol, 2% of ethanol, and the balance is Deionized water is added to 100% by weight, and after mixing evenly, it becomes the tobacco-flavored e-cigarette base oil; the tobacco-flavored e-cigarette base oil with a mass percentage of 50% and the flavor and fragrance with a mass percentage of 50% are stirred and mixed evenly, That is, tobacco-flavored e-cigarette oil is obtained.

Comparative example 2

Tobacco-flavored electronic cigarette oil was prepared according to the ratio of the components in Example 2, except that the Burley tobacco extract was the light component of the Burley tobacco extract obtained from the Burley tobacco raw material through solvent extraction followed by molecular distillation, and the base The oil does not add pomegranate, human face mixed extracts. Specifically: crush the burley tobacco raw material and pass through a 80-100 mesh sieve, then add a solvent 4-10 times the mass of the burley tobacco raw material, extract at 50-80 °C for 1-3 h, cool to 20-30 °C and filter The filtrate is obtained; the filtrate is concentrated under reduced pressure to 1/10~1 times the mass of the Burley tobacco raw material, then frozen at -15~5 °C for 5~15 h, and filtered to obtain the Burley tobacco raw material extract; then add the Burley tobacco raw material to extract Dissolve 8-10 times the mass of propylene glycol in the product, filter and carry out molecular distillation under the conditions of 40-200 ℃ and 10-10 ⁵ Pa to obtain the light fraction of Burley tobacco extract. Take by weighing 100 g of the light component of the above-mentioned Burley tobacco extract, add 1000 g of solvent to the light component of the Burley tobacco extract, and the solvent includes the following components, by mass percentage: glycerol 30%, propylene glycol 60%, ethanol 5%, the balance is made up to 100% by weight with deionized water, and after mixing evenly, it becomes the base oil of tobacco-flavored e-liquid; The percentage is 40% flavor and fragrance, stir and mix well to get tobacco-flavored e-liquid.

The e-cigarette liquids in the above examples and comparative examples were added to the e-cigarette device to evaluate the sensory effect respectively.

The sensory effect evaluation method includes the following steps:

(1) Set up six evaluation indicators, including irritation, satisfaction, dryness, characteristic style, tobacco fragrance and aroma volume, and assign different scores according to the degree of influence of each evaluation index on the sensory quality of e-liquid.

The irritation refers to the discomfort caused by inhaling the smoke generated by the atomization of e-cigarette oil on the sensory organs, including the mouth, throat and nasal cavity.

The sense of satisfaction refers to the comprehensive experience on sensory organs of the strength, concentration and aroma of smoke produced by atomization of e-cigarette oil.

The dry feeling refers to the influence of smoke produced by atomization of e-cigarette oil on the dryness of the mouth after inhalation and exhalation.

The characteristic style refers to: the main sensory difference performance of an e-liquid for e-cigarettes in terms of pleasure, which is different from other e-liquids for e-cigarettes of the same kind.

The tobacco fragrance refers to: the smell of the original fragrance of tobacco is felt by the senses during the smoking process.

The amount of aroma refers to the amount of pleasant breath measured through the oral cavity and nasal cavity during the inhalation process.

(2) Set up 10 e-cigarette smokers, each with a sensory quality evaluation form for e-cigarette oil, adopt the scoring method of dark evaluation, and use the overall cycle evaluation method to smoke e-cigarette oil, according to Table 1 The meaning of the score values of the 6 sensory quality evaluation indicators, the full score of each item is 9 points, the full score is 54 points, each item is divided into a scoring unit, and the meaning of each score is shown in Table 1.

Table 1 Score value meaning table of sensory quality evaluation index of e-cigarette oil

Score irritant satisfaction dry feeling characteristic style Tobacco incense Aroma 9 none very good very light very pleasant very good very sufficient 8 seems to have it is good light happy it is good adequate 7 slight better lighter more pleasant better more adequate 6 slightly slightly better still light slightly pleasant slightly better slightly sufficient 5 Have generally middle generally generally generally 4 slightly larger slightly worse slightly heavier slightly unhappy slightly worse slightly 3 larger poor heavier less pleasant poor slight 2 Big Difference Heavy unhappy Difference seems to have 1 very big very poor very heavy very unpleasant very poor none

(3) Statistics of the results: the evaluation results of all appraisers are valid, and the arithmetic average of the individual evaluation results of each appraiser is calculated, and the results are kept to one decimal place, and the arithmetic average of each individual item is added. The total score is obtained, and the result is rounded to one decimal place.

The e-cigarette oil prepared in Examples 1-8 and the e-cigarette oil prepared in Comparative Examples 1-2 were added to the electronic cigarette for sensory quality evaluation. The specific evaluation results are shown in Table 2. The scores of each evaluation index in Table 2 are the arithmetic mean scores of the effective scores of 10 reviewers.

Table 2 Evaluation results of sensory effect of e-cigarette oil

It can be seen from Table 2 that compared with the two comparative examples, the total score of the e-cigarette oil of the present invention is higher, and the advantages are mainly reflected in: (1) The sensory quality of the overall smoke after adding tobacco extract is good, and the tobacco itself The aroma is rich and pure, and the smoke is harmonious and natural. This is because the tobacco extract prepared by wet pulverization retains the active ingredients of tobacco to the greatest extent and the extraction rate of tobacco content is high; (2) smoking the smoke of the present invention The feeling of dryness after oiling is significantly reduced, which is because the extracts such as grass jelly and black plum added to the e-cigarette base oil have the effect of promoting body fluid and quenching thirst.

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention to other forms. Any skilled person who is familiar with this profession may use the technical content disclosed above to change or modify the equivalent of equivalent changes. Example. However, any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims (6)

1. A method for preparing tobacco flavor electronic cigarette oil by wet pulverization, is characterized in that, comprises the following steps: (1) Accurately weigh 100 g of dry tobacco, pass it through a 5-50 mesh screen after primary crushing, add solvent to the primary crushed tobacco, the mass ratio of the tobacco to solvent is 1:5-10, mix well Put it into a high-speed cutting type wet pulverizer, pulverize under certain reaction conditions, and discharge the material after pulverization, and the discharged liquid is tobacco-flavored e-cigarette oil base oil; wherein the certain reaction conditions are the high-speed cutting type wet pulverizer The speed of the pulverizer is 2500~8000 r/min, the pulverization temperature is 5~60 ℃, and the pulverization time is 0.5~6 h; (2) Stir and mix the tobacco-flavored e-liquid base oil with a mass percentage of 50-100% and flavors and fragrances with a mass percentage of 0-50% to obtain tobacco-flavored e-liquid; The tobacco-flavored e-cigarette oil base oil also includes a drug extract with the effect of promoting body fluid and quenching thirst, and the mass ratio of the drug extract to tobacco is 1-5:10; the drug extract having the effect of promoting body fluid and quenching thirst is composed of It is obtained by extracting one or two kinds of mulberry, pomegranate, grass jelly, ebony, olive, human face, vinegar willow fruit, golden club hammer, and yahuazi. 2. A method for preparing tobacco-flavored e-cigarette liquid by wet pulverization according to claim 1, characterized in that, in step (1), the solvent includes the following components, by mass percentage: glycerin Alcohol 20~70%, Propylene Glycol 20~75%, Ethanol 0~15%, and the balance is made up to 100% by weight with deionized water. 3. A method for preparing tobacco-flavored e-liquid by wet pulverization as claimed in claim 1, wherein the speed of the high-speed cutting wet pulverizer is 4000~6000 r/min, and the pulverization temperature is 10 ~25 ℃, crushing time is 1~4 h. 4. A method for preparing tobacco-flavored e-cigarette liquid by wet pulverization as claimed in claim 2, characterized in that, in step (1), the solvent includes the following components, by mass percentage: glycerin Alcohol 30~50%, propylene glycol 40~60%, ethanol 5~10%, and the balance is made up to 100% by weight with deionized water. 5. A method for preparing tobacco-flavored electronic cigarette oil by wet pulverization according to any one of claims 1-4, wherein the tobacco is flue-cured tobacco, burley tobacco, oriental tobacco, air-cured tobacco, cigar tobacco or A kind of yellow flower smoke. 6. A tobacco-flavored electronic cigarette liquid prepared according to a method for preparing tobacco-flavored electronic cigarette liquid by wet pulverization according to any one of claims 1-4.