CN110628509A - Molecular distillation refining processing method of tobacco essential oil product - Google Patents
Molecular distillation refining processing method of tobacco essential oil product Download PDFInfo
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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
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/12—Molecular distillation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The invention relates to a molecular distillation refining processing method of a tobacco essential oil product, which comprises the following steps: freezing alcohol precipitation, solvent removal, distillation refining and finished product dissolution. The tobacco essential oil product prepared by the method has transparent and clear appearance, good solubility in ethanol and ODO, low aroma substances and proper middle boiling point, and is suitable for blending cigarette essence. The tobacco essential oil product prepared by the method has typical Chinese flue-cured tobacco-like aroma, obvious fresh and sweet aroma and strong natural feeling, and the blended essence is stored at normal temperature for 6 months without weakening the aroma and changing the aroma characteristics, so that the tobacco essential oil product is a good cigarette essence product and has a very wide application prospect.
Description
Technical Field
The invention belongs to the technical field of natural plant extraction and separation, and particularly relates to a molecular distillation refining processing method of a tobacco essential oil product.
Background
The tobacco leaves have complex aroma components, are classified according to different aroma groups, and can be generally classified into acids, alcohols, ketones, aldehydes, esters, lactones, phenols, nitrogen heterocycles, furans, amides, ethers and hydrocarbons. The tobacco leaf aroma substance comprises volatile aroma components with simple molecular structures and also comprises aroma precursors with complex molecular structures. The organic acids, phenols, lipoids, sterols and terpenoids of the tobacco not only have important influence on the fragrance of the tobacco, but also are most of aromatic substances in the conversion and degradation products of the organic acids, the phenols, the lipoids, the sterols and the terpenoids, and most of heterocyclic compounds are converted from related substances and are special aromatic substances.
Because of the wide variety of tobacco flavor substances, the flavor components of tobacco need to be separated and purified in multiple stages. Some separation techniques such as distillation, extraction, chromatography, adsorption, crystallization, ion exchange, etc. by equilibrium separation; molecular distillation by means of rate separation, ultrafiltration, electrodialysis, reverse osmosis, etc.
The molecular distillation technology is a special liquid-liquid separation technology under high vacuum degree (absolute pressure less than 0.133 Pa). The continuous distillation method is suitable for separating high boiling point, easily oxidized system, high viscosity and heat sensitivity.
Because the mean free path of light molecules is larger than that of heavy molecules, the molecular distillation separates the mixture by utilizing the property that the mean free paths of different molecules are different after the different molecules escape from the liquid level, and the molecular distillation device has the advantages of short heating time, high working vacuum degree, high separation degree, low cost and the like, and the prior molecular distillation technology is widely applied to the fields of chemical industry, food, medicine, spice and the like.
In recent years, the traditional tobacco products affect human health to a certain extent, and with the enhancement of the global smoking control and the emergence of a series of smoking control policies, the structure of the tobacco products is developing towards diversification. The novel tobacco products are mainly divided into electronic cigarettes, low-temperature cigarettes, smokeless tobacco products and the like. The new tobacco product is an electronic device that delivers nicotine to the respiratory system by means of electronic heating. Compared with the traditional cigarette, the content of nicotine added into the electronic cigarette is controllable, and smokers can get rid of the dependence on cigarettes by gradually reducing the addition amount of nicotine to achieve the purpose of quitting smoking. The low-temperature cigarette heats the tobacco shreds by using a special heat source, and the nicotine and the fragrant substances in the tobacco shreds are baked at the temperature lower than 500 ℃, so that the low-temperature cigarette not only can meet the requirements of consumers, but also can reduce the harmful ingredients in the smoke. At present, novel tobacco products in China are in a primary stage, and the technology for extracting and separating the tobacco flavor substances is also in a research and simulation stage.
At present, carriers of various tobacco essence products are mainly ethanol or ODO, and in the preparation process of the tobacco essence products, raw materials are required to be completely dissolved in the ethanol or ODO, are clear and transparent, and cannot have layering, suspended matters or precipitates; it is also desirable to have good aroma performance. The tobacco essence products in the current market have the problems of poor solubility, poor aroma and the like.
The novel tobacco product additive obtained by using the molecular distillation technology can effectively enrich nicotine and aroma components in tobacco leaves and has good aroma quality; the boiling point of the components is between 150 and 300 ℃, and the tobacco is suitable for use in tobacco products.
Disclosure of Invention
The tobacco essential oil product prepared by the method has transparent and clear appearance, good solubility in ethanol and ODO, low aroma substances and proper middle boiling point, and is suitable for blending cigarette essence.
According to the technical scheme provided by the invention, the molecular distillation refining processing method of the tobacco essential oil product comprises the following steps:
a. adding an ethanol solution with the concentration of 92-98% vol into a tobacco extract serving as a raw material, wherein the volume ratio of the tobacco extract to the ethanol solution is 1: 4.5-7.5, uniformly mixing, and then placing the ethanol solution into a refrigerator with the temperature of-20-0 ℃ for freezing and alcohol precipitation, wherein the alcohol precipitation time is 8-12 hours, so as to obtain an alcohol precipitate;
b. taking out the supernatant in the frozen alcohol precipitate obtained in the step a from the alcohol precipitate, continuously distilling to remove the solvent under reduced pressure by using a rotary evaporator, and continuously removing the solvent by using an oil pump pressure reducing device to obtain a tobacco essential oil crude product; wherein the rotating speed of the rotary evaporator is 65-85 r/min, the vacuum degree is 75-55 mabr, the temperature is 35-55 ℃, and the time is 4.5-6.5 hours; the vacuum degree of the oil pump pressure reducing device is 10.5-5.5 mabr, the temperature is 25-35 ℃, and the time is 1.5-2.5 hours;
c. refining the tobacco essential oil crude product obtained in the step b by using molecular distillation equipment, wherein the material sample introduction temperature is 30-70 ℃, the temperature of a wiped film evaporator is 80-130 ℃, the temperature of a condenser is 10-30 ℃, the vacuum degree is 0.01-1 mbar, and the rotating speed of the wiped film evaporator is 200-300 r/min, so that the obtained evaporated product is the tobacco essential oil;
d. and d, dissolving the pure tobacco essential oil product obtained in the step c in an essential oil solvent, wherein the volume ratio of the pure tobacco essential oil product to the essential oil solvent is 1: 100-300, and thus obtaining the tobacco essential oil product with typical tobacco fragrance and capable of being used for blending the cigarette bead-blasting essence.
Preferably, the method comprises the following steps: in the step a, the tobacco extract is frozen and precipitated with alcohol for 9-11 hours at the temperature of-15 to-5 ℃.
Further preferably: in the step a, the tobacco extract is frozen and precipitated with alcohol for 9.5 to 10.5 hours at the temperature of between 12 ℃ below zero and 8 ℃ below zero.
Preferably, the method comprises the following steps: in the step c, when molecular distillation equipment is used for refining, the material sample introduction temperature is 35-65 ℃, the temperature of the wiped film evaporator is 105-125 ℃, the temperature of the condenser is 15-25 ℃, the vacuum degree is 0.03-0.07 mbar, and the rotating speed of the wiped film evaporator is 220-280 r/min.
Further preferably: in the step c, when molecular distillation equipment is used for refining, the material sample introduction temperature is 40-50 ℃, the temperature of the wiped film evaporator is 108-118 ℃, the temperature of the condenser is 18-22 ℃, the vacuum degree is 0.04-0.06 mbar, and the rotating speed of the wiped film evaporator is 240-260 r/min.
Preferably, the method comprises the following steps: in the step d, the essential oil solvent is 92-98% vol ethanol solution or caprylic-capric glyceride.
Preferably, the method comprises the following steps: in the step d, the volume ratio of the pure tobacco essential oil to the essential oil solvent is 1: 150-250.
Further preferably: in the step d, the volume ratio of the pure tobacco essential oil to the essential oil solvent is 1: 180-220.
The tobacco essential oil product prepared by the method has transparent and clear appearance, good solubility in ethanol and ODO, low aroma substances and proper middle boiling point, and is suitable for blending cigarette essence. The tobacco essential oil product prepared by the method has typical Chinese flue-cured tobacco-like aroma, obvious fresh and sweet aroma and strong natural feeling, and the blended essence is stored at normal temperature for 6 months without weakening the aroma and changing the aroma characteristics, so that the tobacco essential oil product is a good cigarette essence product and has a very wide application prospect.
Detailed Description
The principle of the invention is as follows:
in the invention, the freezing alcohol precipitation is adopted for the basic purpose of removing most of macromolecular substances without aroma contribution in the extracting solution, such as saccharides, amino acids and lipid wax substances, reducing the difficulty of refining subsequent products and improving the quality of the products.
Freezing alcohol precipitation is used for enriching limited essential oil in natural extract according to different solubility of different substances in ethanol. The effective essential oil components in the natural extract are easily dissolved in low-temperature ethanol; while the non-aroma components in the extract are difficult to dissolve in the low-temperature ethanol, so that the effective essential oil components and the non-aroma components are separated.
In the invention, if the temperature of freezing alcohol precipitation is lower than-20 ℃, the effective essential oil components dissolved in the ethanol become less, and the fragrance is not full enough; if the temperature of freezing alcohol precipitation is higher than 0 ℃, more non-aroma components dissolved in the ethanol are increased, and the quality of the product is influenced; therefore, the temperature of freezing alcohol precipitation is feasible to be-20 to 0 ℃. Likewise, if the time of freezing alcohol precipitation is less than 8 hours, the ethanol will have more dissolved non-aroma components; if the freezing alcohol precipitation time is longer than 12 hours, the effective essential oil dissolved in the ethanol is reduced; therefore, the freezing alcohol precipitation time is 8-12 hours.
In the present invention, it is necessary to continue removing the solvent by using the oil pump vacuum apparatus after the solvent is continuously distilled off, because the organic reagent in the residue must be removed as much as possible, otherwise the evaluation of the aroma is affected.
Molecular distillation (also called short-path distillation, abbreviated as SD) is a thermal separation technical process working under the pressure of 1-0.001 mbar, and the molecular distillation is very suitable for thermosensitive and high-boiling-point substances due to the low boiling temperature.
The working process of molecular distillation is as follows: the material is fed from the top of evaporator, and is continuously and uniformly distributed on the heating surface by means of material-liquid distributor on the rotor, then the material-liquid is scraped into a layer of ultrathin turbulent liquid film by means of film-scraping device, and said liquid film can be spirally fed downwards. In the process, light molecules escaping from the heating surface are condensed into liquid on an internal condenser through a short route and almost without molecular collision, are left along the condenser, flow out of the equipment through a gear pump at the bottom of the equipment and can be collected; the residual liquid, i.e. the heavy molecules, is collected at the lower part of the wiped film evaporator and flows out of another gear pump and is collected.
The working temperature of molecular distillation is low, so that effective components can be evaporated from the mother liquor at a temperature far lower than the boiling point of the materials, and the change of heat-sensitive substances in the natural fragrant raw materials is avoided; the distillation process is irreversible, the material reflux phenomenon in the common distillation process is avoided, and the product refining processing time is effectively shortened; the vacuum degree during molecular distillation is high, and materials are not easy to oxidize and damage; the heating time of the material is short, and the heating is generally completed within a few seconds to tens of seconds, so that the chance of thermal decomposition of the material is reduced; the paint is non-toxic, harmless and free of secondary pollution, ensures the product quality and is environment-friendly; the energy consumption in the production and processing process is low, the processing time is short, and the processing cost is effectively saved; therefore, the use effect of molecular distillation in the refining processing process of the tobacco essential oil is very obvious.
In the invention, when the material injection temperature is lower than 30 ℃, the fluidity of the material is poor, and the phenomenon of uneven film scraping is possible, so that the evaporation of effective components in the product is influenced, and the yield and the quality of the product are reduced; when the sample introduction temperature of the material is higher than 70 ℃, the fluidity of the material is almost not changed any more, and the energy consumption is increased due to the increase of the sample introduction temperature; therefore, the injection temperature is feasible at 30-70 ℃.
In the invention, when the temperature of the wiped film evaporator is lower than 80 ℃, incomplete evaporation of effective essential oil can be caused, and the yield and quality of products are influenced; when the temperature of the wiped film evaporator is higher than 130 ℃, coke breeze is generated, and the product quality is seriously influenced; therefore, the temperature of the wiped film evaporator is feasible within the range of 80-130 ℃.
In the invention, when the temperature of the condenser is lower than 10 ℃, the evaporated effective essential oil can be condensed into solid on the condenser, thereby influencing the normal condensation of subsequent materials; when the temperature of the condenser is higher than 30 ℃, effective essential oil cannot be normally condensed, so that the loss of products is caused; therefore, the temperature of the condenser is feasible to be 10-30 ℃.
In the invention, when the vacuum degree of the equipment is higher than 0.01mbar, the evaporated non-aroma components are increased, which affects the quality of the product; when the vacuum degree of equipment is lower than 1mbar, the effective essential oil evaporation amount is insufficient, so that the product yield is reduced, and the fragrance is not full enough; therefore, the vacuum degree of the equipment is feasible within 0.01-1 mbar.
In the invention, when the rotating speed of the film scraper is lower than 200r/min, a liquid film formed on the material on the evaporator is thickened, effective essential oil cannot be completely evaporated, and the product yield is reduced; after the rotating speed of the film scraper is higher than 300r/min, a liquid film formed on the evaporator by the materials is too thin, and redundant non-aroma components are evaporated out, so that the product quality is influenced; therefore, the rotating speed of the film scraper is 200-300 r/min.
Ethanol and ODO are the main carriers of cigarette essence, and the solution is colorless, transparent and clear after the tobacco essential oil refined by molecular distillation is dissolved in the ethanol and ODO, and has no layering, suspension or precipitation. Can be effectively used for preparing the tobacco essence.
In the invention, when the using amount of the ethanol or ODO is less than 100 parts, the fragrance of the tobacco essential oil product is too thick and heavy, and the fragrance of other raw materials in the tobacco essence can be covered; when the amount of the ethanol or ODO is more than 300 parts, the aroma of the tobacco essential oil product is too thin, and the characteristic of the tobacco essential oil product is not obvious. Therefore, the blending ratio of the tobacco essential oil to the ODO is properly 1: 100-300.
The present invention will be further described with reference to the following specific examples.
Example 1
a. Taking tobacco extract which is produced by Yunnan Yunxi spice limited company and is sold as a commodity as a raw material, adding an ethanol solution with the concentration of 95 percent vol, uniformly mixing, and putting the ethanol solution into a refrigerator with the temperature of-10 ℃ for freezing and alcohol precipitation for 10 hours to obtain an alcohol precipitate;
b. taking the supernatant of the frozen alcohol precipitate obtained in the step a out of the alcohol precipitate, then continuously distilling off the solvent under reduced pressure by a rotary evaporator sold under the trade name RE-2000B by Zhengzhou Ketai laboratory instruments Co., Ltd, and then completely removing the solvent by using an oil pump pressure reducing device sold under the trade name vacuubrand by BD SENSOR, Germany to obtain a crude tobacco essential oil product;
c. refining the crude tobacco essential oil obtained in the step b by using molecular distillation equipment which is manufactured by Germany VTA and has the trade name of VKL-70, wherein the molecular distillation has the following set process parameters: the material sample introduction temperature is 40 ℃, the temperature of a wiped film evaporator is 110 ℃, the temperature of a condenser is 20 ℃, the vacuum degree is 0.05mbar, the rotating speed of the wiped film evaporator is 250r/min, and the distillate of the wiped film evaporator at the temperature of 110 ℃ is intercepted, so that the tobacco essential oil is obtained;
d. and d, dissolving the pure tobacco essential oil product obtained in the step c in 95% vol ethanol to obtain a tobacco essential oil product with typical tobacco fragrance and capable of being used for blending tobacco essence. The weight ratio of the tobacco essential oil to 95% vol ethanol is 1: 200. Obtaining the tobacco essential oil product with the typical Chinese style flue-cured tobacco style.
Example 2
a. Taking tobacco extract which is produced by Yunnan Yunxi spice limited company and is sold as a commodity as a raw material, adding an ethanol solution with the concentration of 95 percent vol, uniformly mixing, and putting the ethanol solution into a refrigerator with the temperature of-12 ℃ for freezing and alcohol precipitation for 11 hours to obtain an alcohol precipitate;
b. taking the supernatant of the frozen alcohol precipitate obtained in the step a out of the alcohol precipitate, then continuously distilling off the solvent under reduced pressure by a rotary evaporator sold under the trade name RE-2000B by Zhengzhou Ketai laboratory instruments Co., Ltd, and then completely removing the solvent by using an oil pump pressure reducing device sold under the trade name vacuubrand by BD SENSOR, Germany to obtain a crude tobacco essential oil product;
c. refining the crude tobacco essential oil obtained in the step b by using molecular distillation equipment which is manufactured by Germany VTA and has the trade name of VKL-70, wherein the molecular distillation has the following set process parameters: the material sample introduction temperature is 35 ℃, the temperature of the wiped film evaporator is 105 ℃, the temperature of the condenser is 25 ℃, the vacuum degree is 0.04mbar, and the rotating speed of the wiped film evaporator is 270 r/min. Intercepting the distillate at 105 deg.C to obtain tobacco essential oil;
d. and d, dissolving the pure tobacco essential oil product obtained in the step c in caprylic capric acid glyceride (ODO) to obtain a tobacco essential oil product with typical tobacco fragrance and capable of being used for blending the cigarette bead-blasting essence, wherein the weight ratio of the tobacco essential oil to the ODO is 1:220, and thus the tobacco essential oil product with a typical Chinese style flue-cured tobacco style is obtained.
Example 3
a. Taking tobacco extract which is produced by Yunnan Yunxi spice limited company and is sold as a commodity as a raw material, adding an ethanol solution with the concentration of 95 percent vol, uniformly mixing, and then placing the ethanol solution into a refrigerator with the temperature of-11 ℃ for freezing and alcohol precipitation for 9 hours to obtain an alcohol precipitate;
b. taking the supernatant of the frozen alcohol precipitate obtained in the step a out of the alcohol precipitate, then continuously distilling off the solvent under reduced pressure by a rotary evaporator sold under the trade name RE-2000B by Zhengzhou Ketai laboratory instruments Co., Ltd, and then completely removing the solvent by using an oil pump pressure reducing device sold under the trade name vacuubrand by BD SENSOR, Germany to obtain a crude tobacco essential oil product;
c. refining the crude tobacco essential oil obtained in the step b by using molecular distillation equipment which is manufactured by Germany VTA and has the trade name of VKL-70, wherein the molecular distillation has the following set process parameters: the material sample introduction temperature is 35 ℃, the wiped film evaporator temperature is 115 ℃, the condenser temperature is 25 ℃, the vacuum degree is 0.06mbar, and the wiped film evaporator rotating speed is 240 r/min. Intercepting the distillate at 115 deg.C to obtain tobacco essential oil.
d. And d, dissolving the pure tobacco essential oil product obtained in the step c in 95% ethanol to obtain a tobacco essential oil product with typical tobacco fragrance and capable of being used for blending the cigarette bead-blasting essence, wherein the weight ratio of the tobacco essential oil to the 95% vol ethanol is 1:230, and thus the tobacco essential oil product with a typical Chinese style flue-cured tobacco type style is obtained.
Example 4
a. Taking tobacco extract which is produced by Yunnan Yunxi spice limited company and is sold as a commodity as a raw material, adding an ethanol solution with the concentration of 95 percent vol, uniformly mixing, and putting the ethanol solution into a refrigerator with the temperature of-12 ℃ for freezing and alcohol precipitation for 11 hours to obtain an alcohol precipitate;
b. taking the supernatant of the frozen alcohol precipitate obtained in the step a out of the alcohol precipitate, then continuously distilling off the solvent under reduced pressure by a rotary evaporator sold under the trade name RE-2000B by Zhengzhou Ketai laboratory instruments Co., Ltd, and then completely removing the solvent by using an oil pump pressure reducing device sold under the trade name vacuubrand by BD SENSOR, Germany to obtain a crude tobacco essential oil product;
c. refining the crude tobacco essential oil obtained in the step b by using molecular distillation equipment which is manufactured by Germany VTA and has the trade name of VKL-70, wherein the molecular distillation has the following set process parameters: the material sample introduction temperature is 42 ℃, the temperature of a wiped film evaporator is 110 ℃, the temperature of a condenser is 22 ℃, the vacuum degree is 0.04mbar, the rotating speed of the wiped film evaporator is 230r/min, and the distillate of the wiped film evaporator at the temperature of 110 ℃ is intercepted, so that the tobacco essential oil is obtained;
d. and d, dissolving the pure tobacco essential oil product obtained in the step c in 95% ethanol to obtain a tobacco essential oil product with typical tobacco fragrance and capable of being used for blending the cigarette bead-blasting essence, wherein the weight ratio of the tobacco essential oil to the 95% vol ethanol is 1:210, and thus the tobacco essential oil product with a typical Chinese style flue-cured tobacco type style is obtained.
Example 5
a. Taking tobacco extract which is produced by Yunnan Yunxi spice limited company and is sold as a commodity as a raw material, adding an ethanol solution with the concentration of 95 percent vol, uniformly mixing, and putting the ethanol solution into a refrigerator with the temperature of-8 ℃ for freezing and alcohol precipitation for 9 hours to obtain an alcohol precipitate;
b. taking the supernatant of the frozen alcohol precipitate obtained in the step a out of the alcohol precipitate, then continuously distilling off the solvent under reduced pressure by a rotary evaporator sold under the trade name RE-2000B by Zhengzhou Ketai laboratory instruments Co., Ltd, and then completely removing the solvent by using an oil pump pressure reducing device sold under the trade name vacuubrand by BD SENSOR, Germany to obtain a crude tobacco essential oil product;
c. refining the crude tobacco essential oil obtained in the step b by using molecular distillation equipment which is manufactured by Germany VTA and has the trade name of VKL-70, wherein the molecular distillation has the following set process parameters: the material sample introduction temperature is 35 ℃, the temperature of a wiped film evaporator is 108 ℃, the temperature of a condenser is 18 ℃, the vacuum degree is 0.03mbar, the rotating speed of the wiped film evaporator is 280r/min, and the distillate of the wiped film evaporator at the temperature of 108 ℃ is intercepted, so that the tobacco essential oil is obtained;
d. and d, dissolving the pure tobacco essential oil product obtained in the step c in 95% ethanol to obtain a tobacco essential oil product with typical tobacco fragrance and capable of being used for blending the cigarette bead-blasting essence, wherein the weight ratio of the tobacco essential oil to the 95% vol ethanol is 1:200, and thus the tobacco essential oil product with a typical Chinese style flue-cured tobacco type style is obtained.
The tobacco essence obtained by compounding the tobacco essential oil mixed with a proper amount of 95% vol ethanol or ODO with other fragrant raw materials can be subjected to smoking sensory evaluation.
The weight percentage of each main component in the raw material which is produced by Yunnan Yunxi spice limited company and is named as tobacco extract is shown in table 1. The weight percentage of each main component in the tobacco essential oil products obtained after the treatment by the methods of examples 1 to 3 is shown in table 1.
TABLE 1
As can be seen from the analysis results in Table 1, the tobacco essential oil prepared by the invention effectively enriches the main aroma components and nicotine substances in the tobacco. Meanwhile, harmful substances such as tar polycyclic aromatic hydrocarbon and the like are separated, and the aromatic oil can be directly applied to flavoring of tobacco products.
The invention has the greatest effect of providing a new refining method which has excellent performance and is suitable for all tobacco flavoring products, and the selection direction of tobacco flavor raw materials can be greatly expanded after popularization.
Claims (8)
1. A molecular distillation refining processing method of tobacco essential oil products is characterized by comprising the following steps:
a. adding an ethanol solution with the concentration of 92 ~ 98% vol into a tobacco extract serving as a raw material, wherein the volume ratio of the tobacco extract to the ethanol solution is 1:4.5 ~ 7.5.5, uniformly mixing, and then placing the ethanol solution into a refrigerator with the temperature of-20-0 ℃ for freezing and alcohol precipitation, wherein the alcohol precipitation time is 8-12 hours, so as to obtain an alcohol precipitate;
b. taking out the supernatant in the frozen alcohol precipitate obtained in the step a from the alcohol precipitate, continuously distilling to remove the solvent under reduced pressure by using a rotary evaporator, and continuously removing the solvent by using an oil pump pressure reducing device to obtain a tobacco essential oil crude product; wherein the rotating speed of the rotary evaporator is 65-85 r/min, the vacuum degree is 75-55 mabr, the temperature is 35-55 ℃, and the time is 4.5-6.5 hours; the vacuum degree of the oil pump pressure reducing device is 10.5-5.5 mabr, the temperature is 25-35 ℃, and the time is 1.5-2.5 hours;
c. refining the tobacco essential oil crude product obtained in the step b by using molecular distillation equipment, wherein the material sample introduction temperature is 30-70 ℃, the temperature of a wiped film evaporator is 80-130 ℃, the temperature of a condenser is 10-30 ℃, the vacuum degree is 0.01-1 mbar, and the rotating speed of the wiped film evaporator is 200-300 r/min, so that the obtained evaporated product is the tobacco essential oil;
d. and d, dissolving the pure tobacco essential oil product obtained in the step c in an essential oil solvent, wherein the volume ratio of the pure tobacco essential oil product to the essential oil solvent is 1: 100-300, and thus obtaining the tobacco essential oil product with typical tobacco fragrance and capable of being used for blending the cigarette bead-blasting essence.
2. The molecular distillation refining method of tobacco essential oil products as set forth in claim 1, characterized in that: in the step a, the tobacco extract is frozen and precipitated with alcohol for 9-11 hours at the temperature of-15 to-5 ℃.
3. The molecular distillation refining method of tobacco essential oil products as set forth in claim 2, characterized in that: in the step a, the tobacco extract is frozen and precipitated with alcohol for 9.5 to 10.5 hours at the temperature of between 12 ℃ below zero and 8 ℃ below zero.
4. The molecular distillation refining method of tobacco essential oil products as claimed in claim 1, wherein in the step c, when the refining is performed by using molecular distillation equipment, the material feeding temperature is 35-65 ℃, the temperature of the wiped film evaporator is 105-125 ℃, the temperature of the condenser is 15 ~ 25 ℃, the vacuum degree is 0.03-0.07 mbar, and the rotating speed of the wiped film evaporator is 220-280 r/min.
5. The molecular distillation refining method of tobacco essential oil products as claimed in claim 4, wherein in the step c, when the refining is performed by using molecular distillation equipment, the material feeding temperature is 40 ~ 50 ℃, the temperature of the wiped film evaporator is 108 ~ 118 ℃, the temperature of the condenser is 18-22 ℃, the vacuum degree is 0.04-0.06 mbar, and the rotating speed of the wiped film evaporator is 240-260 r/min.
6. The method for molecular distillation refining of tobacco essential oil product as claimed in claim 1, wherein in step d, the essential oil solvent is 92 ~ 98% vol ethanol solution or caprylic/capric glyceride.
7. The molecular distillation refining method of tobacco essential oil products as claimed in claim 1, wherein in the step d, the volume ratio of the pure tobacco essential oil to the essential oil solvent is 1:150 ~ 250.
8. The molecular distillation refining method of tobacco essential oil products as set forth in claim 7, characterized in that: in the step d, the volume ratio of the pure tobacco essential oil to the essential oil solvent is 1: 180-220.
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Application publication date: 20191231 |