CN111534377A - Separation method of tobacco leaf essential oil containing eluent - Google Patents
Separation method of tobacco leaf essential oil containing eluent Download PDFInfo
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- CN111534377A CN111534377A CN201911420154.5A CN201911420154A CN111534377A CN 111534377 A CN111534377 A CN 111534377A CN 201911420154 A CN201911420154 A CN 201911420154A CN 111534377 A CN111534377 A CN 111534377A
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- essential oil
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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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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention is suitable for the technical field of eluent separation, and provides a separation method of an eluent containing tobacco leaf essential oil, which comprises the steps of freezing the eluent containing the tobacco leaf essential oil to separate out crystals, and obtaining the frozen crystals after vacuum filtration; melting and freezing to obtain frozen liquid, and concentrating the frozen liquid at low temperature in vacuum to obtain essential oil liquid; molecular distillation of the essential oil liquid. The tobacco leaf essential oil is crystallized and separated from the eluent by freezing and crystallizing at a certain temperature, and then the first essential oil, the faint scent essential oil, the normal sweet essential oil and the caramel essential oil are obtained by vacuum low-temperature concentration and molecular distillation and separation at a specific temperature, so that the aim of separating the eluent containing the tobacco leaf essential oil is fulfilled.
Description
Technical Field
The invention belongs to the technical field of eluent separation, and particularly relates to a separation method of an eluent containing tobacco leaf essential oil.
Background
The tobacco leaf essential oil is volatile and semi-volatile substance extracted from tobacco leaf, and has special smell of tobacco. The content of essential oil in tobacco is very low, about 0.1%, and the content and components of essential oil in tobacco of different varieties, different parts, different modulation types and different regions are also different.
The traditional method for obtaining the tobacco leaf essential oil is to directly use tobacco leaves for steam distillation, but some heat-sensitive volatile components are damaged due to the fact that samples are subjected to azeotropy with water during extraction. An improved method based on a steam distillation method, called a gas co-distillation method, is developed later, and can prevent heat-sensitive components from being damaged, but the method is difficult to control due to the requirement of conditions such as constant gas, ice bath and the like, and is not popularized and used finally.
In addition, a method for extracting tobacco leaves by using an organic solvent and then separating and treating the extract to obtain tobacco leaf essential oil is also provided, but the method has low separation efficiency on the tobacco leaf essential oil.
Disclosure of Invention
The invention provides a separation method of tobacco leaf essential oil containing eluent, and aims to solve the problem of low separation efficiency of the existing separation method.
The invention is realized in such a way that the separation method of the tobacco leaf essential oil containing eluent comprises the following steps:
freezing the eluent containing the tobacco leaf essential oil to separate out crystals, and carrying out vacuum filtration to obtain frozen crystals a, wherein the freezing temperature is reduced from the normal temperature to-15 ℃ within 8 hours, and the temperature is kept for 16-20 hours;
the tobacco leaf essential oil in the eluent containing the tobacco leaf essential oil begins to crystallize at minus 8 ℃ and quickly crystallizes at minus 15 ℃, and experiments prove that the tobacco leaf essential oil has the best crystallization effect under the condition of minus 15 ℃, the crystallization rate is higher, the crystallization speed cannot be obviously improved when the temperature is lower than minus 15 ℃, and the temperature of minus 15 ℃ is the best crystallization temperature in the comprehensive view because more energy is consumed due to the lower temperature.
Melting the frozen crystals a to obtain frozen liquid b, and concentrating the frozen liquid b at low temperature in vacuum to obtain essential oil liquid c;
molecular distillation of the essential oil liquid c, collecting fractions at 118-122 ℃ to obtain top fragrant essential oil, collecting fractions at 148-152 ℃ to obtain fragrant essential oil, collecting fractions at 176-180 ℃ to obtain normal sweet essential oil, and collecting fractions at 196-200 ℃ to obtain caramel sweet essential oil.
After one essential oil is obtained by each distillation, the essential oil is put into the same distillation equipment again for heating distillation to obtain the next essential oil, and 4 distillation equipment can be arranged in series in the specific implementation process to form the whole process flow.
Still further, the operating temperature of the vacuum filtration is < -8 ℃.
During vacuum filtration, the environment temperature and the solid-liquid temperature of filtration are required to be lower than-8 ℃, so that the crystallized tobacco leaf essential oil is prevented from being melted into liquid and recovered along with the solvent, and the yield is reduced.
Furthermore, the pressure of the vacuum low-temperature concentration is 0.085Mpa to 0.09Mpa, and the temperature is 50 ℃ to 55 ℃.
Further, the pressure of the molecular distillation is 15Pa to 25 Pa.
Further, in the step of distilling to obtain the top essential oil and the fragrant essential oil, the relationship between the flow rate of the molecular distillation input liquid and the area of the heated plate is 20L/h/m2。
Further, in the step of distilling to obtain the normal sweet essential oil and the caramel sweet essential oil, the relationship between the flow rate of the molecular distillation input liquid and the area of the heated plate is 10L/h/m2。
Further, the step of recovering the solvent after obtaining the frozen crystals a by vacuum filtration is also included.
The separation method of the tobacco leaf essential oil containing eluent provided by the invention is characterized in that the tobacco leaf essential oil is crystallized and separated from the eluent through freezing crystallization at a certain temperature, and then the first essential oil, the fragrant essential oil, the normal sweet essential oil and the caramel essential oil are obtained through vacuum low-temperature concentration and molecular distillation separation at a specific temperature, so that the purpose of separating the tobacco leaf essential oil containing eluent is achieved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
The separation method of the tobacco leaf essential oil containing eluent provided by the embodiment of the invention comprises the following steps:
freezing the eluent containing the tobacco leaf essential oil to separate out crystals, carrying out vacuum filtration to obtain frozen crystals a, reducing the freezing temperature from the normal temperature to-15 ℃ within 8h, preserving the temperature for 16h, and recovering the solvent;
thawing the frozen crystals a to obtain frozen liquid b, and concentrating the frozen liquid b at 50 deg.C under 0.085Mpa in vacuum to obtain essential oil liquid c;
the pressure of the molecular distillation essential oil liquid c is controlled to be 20Pa, the rotating speed of a scraper is 240r/min, and the relation between the flow rate of the input liquid and the area of a heated plate is 20L/h/m2；
Collecting the distillate at 120 deg.C to obtain top essential oil;
collecting the distillate at 150 deg.C to obtain fragrant essential oil;
the flow rate of the liquid to be supplied was changed so that the relationship between the flow rate of the liquid to be supplied and the area of the heated plate was 10L/h/m2；
Collecting the distillate at 178 deg.C to obtain sweet essential oil;
collecting the fractions at a temperature of 198 deg.C to obtain the sweet tar.
Example two
The separation method of the tobacco leaf essential oil containing eluent provided by the embodiment of the invention comprises the following steps:
freezing the eluent containing tobacco leaf essential oil to separate out crystals, carrying out vacuum filtration to obtain frozen crystals a, reducing the freezing temperature from the normal temperature to-15 ℃ within 8h, preserving the temperature for 20h, and recovering the solvent;
melting the frozen crystal a to obtain a frozen liquid b, and concentrating the frozen liquid b at low temperature under vacuum at a pressure of 0.09Mpa and a temperature of 55 ℃ to obtain an essential oil liquid c;
molecular distillation of essential oil liquid c, control pressure of 25Pa, scraper rotation speed240r/min, the relationship between the flow rate of the input liquid and the area of the heated plate was 20L/h/m2；
Collecting the fractions at a temperature of 122 deg.C to obtain top essential oil;
collecting the distillate at 152 deg.C to obtain fragrant essential oil;
the flow rate of the liquid to be supplied was changed so that the relationship between the flow rate of the liquid to be supplied and the area of the heated plate was 10L/h/m2；
Collecting the distillate at 180 deg.C to obtain sweet essential oil;
collecting the fractions at 200 deg.C to obtain the final product.
EXAMPLE III
The separation method of the tobacco leaf essential oil containing eluent provided by the embodiment of the invention comprises the following steps:
freezing the eluent containing the tobacco leaf essential oil to separate out crystals, carrying out vacuum filtration to obtain frozen crystals a, reducing the freezing temperature from the normal temperature to-15 ℃ within 8h, preserving the temperature for 16h, and recovering the solvent;
thawing the frozen crystals a to obtain frozen liquid b, and concentrating the frozen liquid b at 50 deg.C under 0.085Mpa in vacuum to obtain essential oil liquid c;
the pressure of the molecular distillation essential oil liquid c is controlled to be 15P, the rotating speed of a scraper is 240r/min, and the relation between the flow rate of the input liquid and the area of a heated plate is 20L/h/m2；
Collecting the fractions at a temperature of 118 deg.C to obtain top essential oil;
collecting the distillate at 148 deg.C to obtain fragrant essential oil;
the flow rate of the liquid to be supplied was changed so that the relationship between the flow rate of the liquid to be supplied and the area of the heated plate was 10L/h/m2；
Collecting the distillate at 176 deg.C to obtain sweet essential oil;
collecting the fractions at a temperature of 196 deg.C to obtain the sweet tar.
Example four
The separation method of the tobacco leaf essential oil containing eluent provided by the embodiment of the invention comprises the following steps:
freezing the eluent containing the tobacco leaf essential oil to separate out crystals, carrying out vacuum filtration to obtain frozen crystals a, reducing the freezing temperature from the normal temperature to-15 ℃ within 8h, preserving the temperature for 16h, and recovering the solvent;
thawing the frozen crystals a to obtain frozen liquid b, and concentrating the frozen liquid b at 50 deg.C under 0.085Mpa in vacuum to obtain essential oil liquid c;
the essential oil liquid c is distilled by molecules, the control pressure is 25Pa, the rotating speed of a scraper is 240r/min, and the relation between the flow rate of the input liquid and the area of a heated plate is 20L/h/m2；
Collecting the fractions at 119 deg.C to obtain top essential oil;
collecting the distillate at 151 deg.C to obtain fragrant essential oil;
the flow rate of the liquid to be supplied was changed so that the relationship between the flow rate of the liquid to be supplied and the area of the heated plate was 10L/h/m2；
Collecting the fractions at 177 deg.C to obtain sweet essential oil;
collecting the fractions at 199 deg.C to obtain the final product.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. The separation method of the tobacco leaf essential oil containing eluent is characterized by comprising the following steps:
freezing the eluent containing the tobacco leaf essential oil to separate out crystals, and carrying out vacuum filtration to obtain frozen crystals a, wherein the freezing temperature is reduced from the normal temperature to-15 ℃ within 8 hours, and the temperature is kept for 16-20 hours;
melting the frozen crystals a to obtain frozen liquid b, and concentrating the frozen liquid b at low temperature in vacuum to obtain essential oil liquid c;
molecular distillation of the essential oil liquid c, collecting fractions at 118-122 ℃ to obtain top fragrant essential oil, collecting fractions at 148-152 ℃ to obtain fragrant essential oil, collecting fractions at 176-180 ℃ to obtain normal sweet essential oil, and collecting fractions at 196-200 ℃ to obtain caramel sweet essential oil.
2. The method of claim 1, wherein the vacuum filtration is performed at an operating temperature of < -8 ℃.
3. The method for separating an eluate containing essential oil of tobacco leaves according to claim 1, wherein the vacuum cryoconcentration is performed at a pressure of 0.085Mpa to 0.09Mpa and a temperature of 50 ℃ to 55 ℃.
4. The method for separating an eluate containing tobacco leaf essential oil according to claim 1, wherein the pressure of the molecular distillation is 15Pa to 25 Pa.
5. The method for separating an essential oil eluate containing tobacco leaves according to claim 1, wherein in the step of obtaining the top essential oil and the fragrant essential oil by molecular distillation, a relationship between a flow rate of an input liquid for molecular distillation and an area of the heated plate is 20L/h/m2。
6. The method for separating an eluate containing essential oil of tobacco leaves according to claim 1, wherein in the step of obtaining the normal-sweet essential oil and the caramel essential oil by molecular distillation, the relationship between the flow rate of the input liquid by molecular distillation and the area of the heated plate is 10L/h/m2。
7. The method for separating an eluate containing essential oil of tobacco leaves according to claim 1, further comprising a step of recovering the solvent after obtaining the frozen crystals a by vacuum filtration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911420154.5A CN111534377B (en) | 2019-12-31 | 2019-12-31 | Separation method of tobacco leaf essential oil containing eluent |
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| CN201911420154.5A CN111534377B (en) | 2019-12-31 | 2019-12-31 | Separation method of tobacco leaf essential oil containing eluent |
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| CN111534377A true CN111534377A (en) | 2020-08-14 |
| CN111534377B CN111534377B (en) | 2023-04-14 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001004245A1 (en) * | 1999-07-13 | 2001-01-18 | Danisco A/S | Process for separating essential oils from an essential oil-containing material |
| CN101898941A (en) * | 2010-07-27 | 2010-12-01 | 中山大学 | Method for purifying trans-anethole |
| CN104534746A (en) * | 2015-01-21 | 2015-04-22 | 云南中海路德科技有限公司 | Equipment for recycling heat energy and aroma substances from tobacco processing waste gas |
| CN104818117A (en) * | 2015-03-31 | 2015-08-05 | 川渝中烟工业有限责任公司 | Tobacco branch essential oil prepared from tobacco waste and its preparation method and use |
| WO2015199698A1 (en) * | 2014-06-26 | 2015-12-30 | Swan Lew | Essential oil distillation systems, devices, and methods |
-
2019
- 2019-12-31 CN CN201911420154.5A patent/CN111534377B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001004245A1 (en) * | 1999-07-13 | 2001-01-18 | Danisco A/S | Process for separating essential oils from an essential oil-containing material |
| CN101898941A (en) * | 2010-07-27 | 2010-12-01 | 中山大学 | Method for purifying trans-anethole |
| WO2015199698A1 (en) * | 2014-06-26 | 2015-12-30 | Swan Lew | Essential oil distillation systems, devices, and methods |
| CN104534746A (en) * | 2015-01-21 | 2015-04-22 | 云南中海路德科技有限公司 | Equipment for recycling heat energy and aroma substances from tobacco processing waste gas |
| CN104818117A (en) * | 2015-03-31 | 2015-08-05 | 川渝中烟工业有限责任公司 | Tobacco branch essential oil prepared from tobacco waste and its preparation method and use |
Non-Patent Citations (2)
| Title |
|---|
| 姚文等: "SOT溶剂体系从烟渣中萃取茄尼醇的研究", 《矿冶》 * |
| 瞿新华: "植物精油的提取与分离技术", 《安徽农业科学》 * |
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| CN111534377B (en) | 2023-04-14 |
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