CN112094697A - Extraction method of citrus essential oil - Google Patents
Extraction method of citrus essential oil Download PDFInfo
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- CN112094697A CN112094697A CN202010920276.7A CN202010920276A CN112094697A CN 112094697 A CN112094697 A CN 112094697A CN 202010920276 A CN202010920276 A CN 202010920276A CN 112094697 A CN112094697 A CN 112094697A
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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
Abstract
The invention provides a method for extracting citrus essential oil, which comprises the steps of sequentially carrying out extraction treatment, liquid-solid separation treatment, gas-liquid separation treatment and pressurization reflux treatment on plant tissues. According to the extraction method of the citrus essential oil, the material does not need to be freeze-dried in advance, but plant tissues from citrus are directly used as raw materials, so that the production time is saved, and the cost is reduced; the extraction treatment and the liquid-solid separation treatment are controlled to be carried out in the same temperature range and the same pressure range, the highest pressure of the gas-liquid separation treatment is controlled to be lower than the lowest pressure of the liquid-solid separation treatment, so that a gaseous extracting agent is obtained through the gas-liquid separation treatment, the gaseous extracting agent forms a liquid extracting agent through the pressurization backflow device and then flows back into the extraction device, the extraction agent is directly recycled, the loss and the production cost of the extracting agent are reduced, and the production efficiency is further improved.
Description
Technical Field
The invention relates to the technical field of natural spice extraction, in particular to a method for extracting citrus essential oil.
Background
The citrus essential oil is a common essential oil variety in the market, has fresh smell, has the functions of resisting bacteria and diminishing inflammation and stimulating the central nervous system to stimulate vitality and activate thinking, and is particularly suitable for urban workplace people under pressure for a long time.
Essential oils can be extracted from citrus plant tissue by steam distillation, squeezing or solvent extraction. However, the steam distillation method and the pressing method have long operation time, low yield and low product purity, and cannot ensure good quality of finished products.
Chinese patent application publication No. CN103122277A discloses a method for extracting natural perfume with dimethyl ether, which uses dimethyl ether as a perfume extractant to extract freeze-dried materials, and recovers the dimethyl ether in the extract. However, in the method, the freeze-dried material is used as a raw material, time and cost are consumed for carrying out freeze-drying treatment on the initial raw material, the dimethyl ether is recovered into the solvent tank, and the recovered dimethyl ether needs to be introduced into the extraction tank again for extraction after being heated and pressurized, which is obviously not beneficial to the improvement of production efficiency and the reduction of cost.
Therefore, there is a need to design a new extraction method of essential oil from citrus plants to avoid the above problems in the prior art.
Disclosure of Invention
The invention aims to provide an extraction method of citrus essential oil, which aims to improve the production efficiency and reduce the cost.
In order to achieve the above object, the extraction method of citrus essential oil according to the present invention comprises:
s0: providing extraction equipment, plant tissues derived from citrus plants and an extracting agent, wherein the extraction equipment comprises an extraction device, a separation device and a pressurizing and refluxing device, and the water content of the plant tissues is not lower than 5%;
s1: extracting the plant tissue by a liquid extracting agent in the extraction device to obtain an extraction mixture;
s2: carrying out liquid-solid separation treatment and gas-liquid separation treatment on the extraction mixture through the separation device to obtain a liquid extraction product and a gaseous extraction agent;
s3: carrying out pressurization backflow treatment on the gaseous extracting agent in the pressurization backflow device to enable the formed liquid extracting agent to flow back into the extraction device;
controlling the extraction treatment and the liquid-solid separation treatment to be carried out in the same temperature range and the same pressure range, and controlling the highest pressure of the gas-liquid separation treatment to be lower than the lowest pressure of the liquid-solid separation treatment.
The extraction method of the citrus essential oil has the beneficial effects that: the plant tissue which is derived from citrus and has the water content of not less than 5 percent is directly used as the raw material without adopting freeze-drying or drying materials, so that the production time is saved, and the cost is reduced; the extraction treatment and the liquid-solid separation treatment are controlled to be carried out in the same temperature range and the same pressure range, the highest pressure of the gas-liquid separation treatment is controlled to be lower than the lowest pressure of the liquid-solid separation treatment, so that a gaseous extracting agent is obtained through the gas-liquid separation treatment, the gaseous extracting agent forms a liquid extracting agent through the pressurization backflow device and then flows back into the extraction device, the extraction agent is directly recycled, the loss and the production cost of the extracting agent are reduced, and the production efficiency is further improved.
Preferably, the extractant is a single-component extractant and is in a gaseous state at normal temperature and normal pressure. The beneficial effects are that: is favorable for rapidly realizing the recycling of the extracting agent.
Further preferably, the extraction treatment and the liquid-solid separation treatment are both carried out under a pressure of 0.2-1.5 megapascals and at a temperature of 0-60 ℃, and the mass ratio of the plant tissue to the extractant is 0.1:1-5: 1. The beneficial effects are that: the extraction efficiency is improved.
Further preferably, the gas-liquid separation treatment is performed at a temperature of from-20 to 40 degrees centigrade and at a pressure of from 0.1 to 1.0 mpa. The beneficial effects are that: is helpful for reducing the material loss caused by the volatilization of the essential oil.
It is further preferred that the liquid extractant formed by the pressure-increasing reflux treatment has the same temperature as the liquid extractant in the extraction apparatus.
Further preferably, the extractant is any one of dimethyl ether, petroleum ether, ethanol, acetone, butane and freon.
Preferably, in step S0, an original plant tissue is obtained from the citrus plant, and the plant tissue is obtained by washing the original plant tissue. The beneficial effects are that: the freeze-drying treatment is not needed, the production efficiency is improved, and the cost is reduced.
Further preferably, the original plant tissue is at least one of fruit, pericarp, leaf, flower, stem, seed, bark and root.
Preferably, any two of the extraction device, the separation device and the pressure-increasing reflux device are communicated with each other, and the extraction treatment, the liquid-solid separation treatment, the gas-liquid separation treatment and the pressure-increasing reflux treatment are performed by continuous operation to form a cyclic treatment process. The beneficial effects are that: is convenient for improving the extraction effect through continuous production.
Further preferably, a pumping device is disposed between the extraction device and the separation device, and after the step S1 is finished, the extraction mixture is introduced into the separation device through the pumping device.
It is further preferred that the pressure of the liquid-solid separation process is controlled to be lower than the pressure of the extraction process so that the extraction mixture is introduced into the separation device by means of a pressure difference.
Preferably, a conduction device is further arranged between any two of the extraction device, the separation device and the pressure-boosting reflux device, and the cyclic treatment process is converted into an intermittent treatment process by controlling the on-off of the conduction device. The beneficial effects are that: the extraction effect is convenient to improve through intermittent production.
Preferably, the separation device is provided with a filtering device, and in the step S2, the solid substances are intercepted by the filtering device.
Preferably, the extraction equipment further comprises a liquid-liquid separation device, and after the step S2 is finished, the liquid-liquid separation device is used for performing liquid-liquid separation treatment on the liquid extraction product to obtain crude essential oil.
Drawings
FIG. 1 is a flow chart of a method for extracting essential oil from citrus according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an extraction apparatus according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and similar words are intended to mean that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
In order to solve the problems in the prior art, the embodiment of the invention provides a method for extracting citrus essential oil, so that the production efficiency is improved and the cost is reduced.
FIG. 1 is a flow chart of an extraction method according to an embodiment of the present invention. Referring to fig. 1, the extraction method includes:
s0: providing an extraction apparatus, plant tissue derived from citrus, and an extraction agent, the extraction apparatus comprising an extraction device, a separation device, and a pressure-increasing reflux device;
s1: extracting the plant tissue by a liquid extracting agent in the extraction device to obtain an extraction mixture;
s2: carrying out liquid-solid separation treatment and gas-liquid separation treatment on the extraction mixture through the separation device to obtain a liquid extraction product and a gaseous extraction agent;
s3: and carrying out pressurization backflow treatment on the gaseous extracting agent in the pressurization backflow device so as to enable the formed liquid extracting agent to flow back into the extraction device.
In the embodiment of the invention, the extraction treatment and the liquid-solid separation treatment are controlled to be carried out in the same temperature range and the same pressure range so as to enable the extracting agent to be in a liquid state, the highest pressure of the gas-liquid separation treatment is controlled to be lower than the lowest pressure of the liquid-solid separation treatment, and the gaseous extracting agent is obtained after the gas-liquid separation treatment.
In some embodiments of the present invention, the pressure of the gas-liquid separation process is controlled to be lower than the pressure of the liquid-solid separation process, so as to obtain the gaseous extractant after the gas-liquid separation process.
The normal temperature refers to 20-25 ℃, and the normal pressure refers to 1 standard atmospheric pressure.
Fig. 2 is a schematic structural diagram of an extraction apparatus according to some embodiments of the invention.
Referring to fig. 2, the extraction apparatus 2 includes an extraction device 21, a separation device (not shown), and a pressure-increasing reflux device 24. The separation means (not shown) consists of a liquid-solid separation means 22 and a gas-liquid separation means 23.
The extraction device 21 is used for performing the extraction treatment on the plant tissue by the liquid extractant to obtain the extraction mixture and conveying the extraction mixture to the liquid-solid separation device 22; the liquid-solid separation device 22 is configured to perform the liquid-solid separation treatment on the extraction mixture, so as to discharge solid substances through the liquid-solid separation device 22, and convey obtained liquid substances to the gas-liquid separation device 23; the gas-liquid separation device 23 is configured to perform the gas-liquid separation treatment on the liquid substance to obtain the liquid extraction product and the gaseous extraction agent, and deliver the gaseous extraction agent to the pressure-boosting reflux device 24; the pressure-increasing reflux device 24 is used for performing the pressure-increasing reflux treatment on the gaseous extracting agent so as to enable the formed liquid extracting agent to reflux to the extracting device 21.
In the embodiment of the present invention, any two of the extraction device 21, the liquid-solid separation device 22, the gas-liquid separation device 23, and the pressure-increasing reflux device 24 are communicated with each other, so as to facilitate the extraction treatment, the liquid-solid separation treatment, the gas-liquid separation treatment, and the pressure-increasing reflux treatment to be performed in a continuous operation manner to form a cyclic treatment process, thereby improving the production efficiency and the extraction effect.
Specifically, referring to fig. 2, the extraction apparatus 21 includes an extraction tank 211, a feeding pipeline 213 disposed at the top of the extraction tank 211, and a first connecting pipeline 212; the liquid-solid separation device 22 includes a liquid-solid separation tank 221 and a second connecting line 222; the gas-liquid separation device 23 includes a gas-liquid separation tank 231 and a third connecting pipe 232; the pressure intensifying return device 24 includes a compressor 241 and a fourth connecting line 242.
The first connecting pipeline 212 connects the bottom of the extraction tank 211 and the top of the liquid-solid separation tank 221, and the second connecting pipeline 222 connects the side wall outlet of the liquid-solid separation tank 221 and the side wall inlet of the gas-liquid separation tank 231; the third connecting pipe 232 connects the outlet of the sidewall of the gas-liquid separation tank 231 and the inlet of the compressor 241; the fourth connection pipe 242 connects the outlet of the compressor 241 and the top of the extraction tank 211, thereby forming a circulation path.
Further, the extraction device 21, the liquid-solid separation device 22, the gas-liquid separation device 23, and the pressure-increasing reflux device 24 further include an extraction control device, a liquid-solid separation control device, and a gas-liquid separation control device, respectively, so as to control the temperature and pressure in the extraction tank 211, the liquid-solid separation tank 221, and the gas-liquid separation tank 231.
More specifically, the temperature of the extractant is controlled by using a heat exchanger, and the temperature of the extractant corresponds to the saturated vapor pressure of the extractant at the temperature, so that the temperature and the pressure of the extraction device, the liquid-solid separation device, the gas-liquid separation device and the pressure boosting reflux device are controlled. The usage and arrangement of the heat exchanger are well known to those skilled in the art, and are not described herein.
In some embodiments of the present invention, a conducting device is further disposed between any two of the extraction device 21, the separation device and the pressure-boosting reflux device 24. Specifically, referring to fig. 2, the first connection pipeline 212, the second connection pipeline 222, the third connection pipeline 232, and the fourth connection pipeline 242 are all provided with a conduction device 25, and the cyclic treatment process is converted into an intermittent treatment process by controlling the on/off of the conduction device 25.
In some embodiments of the invention, the conducting device is a shut-off valve or a regulating valve. When the conducting device is a regulating valve, the flow rate of the circulating substance between any two of the extraction device 21, the separation device and the pressure-increasing reflux device 24 can be controlled by the regulating valve during the circulating treatment.
In the embodiment of the present invention, the extraction tank 211 contains an extraction agent and the plant tissue, and during the extraction process, the connection between the feeding pipeline 213 and the outside of the extraction tank 211 is cut off, so that the extraction tank 211 can only be connected to the circulation path.
In some embodiments of the present invention, the extraction agent is a single-component extraction agent, is in a gaseous state at normal temperature and pressure, and is in a liquid state in the extraction device 21, so as to facilitate rapid recycling of the extraction agent.
Specifically, the extracting agent is any one of dimethyl ether, petroleum ether, ethanol, acetone, butane and freon.
The extractants used in examples 1-3 of the present invention were all dimethyl ether.
In some embodiments of the present invention, the amount of the extractant added is based on the ability to submerge the plant tissue after entering the extraction tank 211 and being in a liquid state. Specifically, the mass ratio of the plant tissues to the extracting agent is 0.5:1-5: 1.
In some embodiments of the invention, the plant tissue is derived from at least one of a fruit, a peel, a leaf, a flower, a stem, a seed, a bark, and a root of the citrus plant.
In some embodiments of the present invention, in step S0, original plant tissue is obtained from the citrus plant, and the plant tissue is obtained after washing the original plant tissue.
Specifically, the cleaning treatment includes: the original plant tissue is rinsed by using clear water to remove impurities such as dust or foreign matters, and then the plant tissue is obtained after removing the free water attached to the surface of the original plant tissue, so that the plant tissue does not need to be freeze-dried before extraction treatment, and the production time and the cost are saved.
More specifically, the method of drying in the shade or spin-drying is used to remove the free water on the surface of the original plant tissue.
In step S1 of some embodiments of the present invention, the extraction process is performed at 0-60 ℃ and under a pressure of 0.2-1.5 mpa to improve the extraction efficiency.
In step S1 of some embodiments of the present invention, when the extraction device 2 is intermittently processed by a plurality of the conducting devices 25, the extraction time, i.e. the time for which the plant tissue stays in the extraction tank 211, is 15-60 minutes.
When the extraction device 2 is performing a continuous process, the extraction time is 15-60 minutes.
In some embodiments of the present invention, the separation device is provided with a filtering device to intercept solid materials by the filtering device in the step S2. In particular, the filtering means is a screen and is arranged between the top and the side wall outlet inside the liquid-solid separation tank 221 to intercept solid matter, such as plant tissue debris, that may be entrained in the extraction mixture.
In step S2 of some embodiments of the present invention, the liquid-solid separation process is performed at 0-60 ℃ and under a pressure of 0.2-1.5 mpa to improve the separation efficiency.
In step S2 of some embodiments of the present invention, when the extraction device 2 performs the batch process through the plurality of conducting devices 25, the time of the liquid-solid separation process, i.e., the residence time of the extraction mixture in the liquid-solid separation tank 221, is 5 to 15 minutes.
When the extraction apparatus 2 performs a continuous process, the liquid-solid separation process takes 5 to 15 minutes.
In some embodiments of the present invention, a pumping device is disposed between the extraction device 21 and the separation device, and after the step S1 is finished, the extraction mixture is introduced into the separation device through the pumping device.
In particular, the first connection line 212 is provided with a pumping device by means of which the extraction mixture is introduced into the liquid-solid separation tank 221. More specifically, the pumping device is a slurry pump.
In some embodiments of the invention, the pressure of the liquid-solid separation process is controlled to be lower than the pressure of the extraction process such that the extraction mixture is introduced into the separation device by a pressure differential.
In some embodiments of the present invention, the gas-liquid separation process is performed at a temperature of-20 to 40 degrees celsius and a pressure of 0.1 to 1.0 mpa, so that the extractant in the liquid material from the liquid-solid separation device 22 is gasified into a gaseous extractant, and the resulting liquid extraction product including water and crude essential oil is left in the gas-liquid separation tank 231.
In step S2 of some embodiments of the present invention, when the extraction device 2 performs the intermittent treatment process by using a plurality of the conducting devices 25, the gas-liquid separation treatment time, that is, the time for the liquid substance to stay in the gas-liquid separation tank 231 is 30 to 60 minutes.
When the extraction apparatus 2 performs a continuous process, the gas-liquid separation process takes 30 to 60 minutes.
In step S3 of some embodiments of the present invention, the pressurized reflux process makes the liquid extractant formed by the gaseous extractant have the same temperature as the liquid extractant in the extraction apparatus 21, so as to enter the extraction tank 211 for direct application in the extraction process.
In some embodiments of the invention, when the extraction device 2 is continuously processed, the residence time of the plant tissue in the extraction means 21 is between 15 and 60 minutes.
The extraction process and the advantageous effects of the present invention are explained in detail below with reference to fig. 2, specifically by examples 1 to 3.
Example 1
Example 1 provides a first extraction method for obtaining citrus crude essential oil by means of batch treatment using said extraction device 2, comprising in particular:
selecting picked orange peel as original plant tissue, cleaning with clear water to remove solid impurities such as dust, and spin-drying to remove free water to obtain wet orange peel for use as plant tissue, wherein the water content of the wet orange peel is not less than 5%.
500 g of wet orange peel is put into the extraction tank 211, and the feeding line 213 and a shut-off valve (not shown) disposed in the first connection line 212 are closed; dimethyl ether is placed in the extraction tank 211 in advance and serves as an extracting agent, and the mass ratio of the dimethyl ether to the wet orange peel is 1: 1.
The temperature in the extraction tank 211 is controlled to be 5 degrees celsius by an extraction control device (not shown), and the corresponding pressure is 0.32 mpa, so as to perform the extraction treatment. The dimethyl ether is in a liquid state in the extraction tank 211 and can immerse wet orange peels so as to ensure the extraction efficiency and control the extraction time to be 30 minutes.
In the course of the extraction process, a shutoff valve (not shown) disposed in the second connection pipe 222 is closed, and a liquid-solid separation control device (not shown) controls the temperature in the liquid-solid separation tank 221 to be 5 degrees celsius, and the corresponding pressure is 0.32 mpa.
After the extraction process is completed, a shut-off valve (not shown) disposed in the first connection pipe 212 is opened, the extraction mixture formed in the extraction tank 211 is introduced into the liquid-solid separation tank 221 by a slurry pump (not shown), and then the shut-off valve (not shown) disposed in the first connection pipe 212 is closed.
The extraction mixture entering the liquid-solid separation tank 221 is subjected to the liquid-solid separation treatment at 5 degrees celsius, with a corresponding pressure of 0.32 mpa. The time of the liquid-solid separation treatment is controlled to be 5 minutes, and the dimethyl ether in the extraction mixture is in a liquid state and can still further extract plant tissues possibly carried in the extraction mixture in the liquid-solid separation tank 221.
In the process of the liquid-solid separation treatment, the shutoff valve provided in the third connecting line 232 is closed, and the temperature in the gas-liquid separation tank 231 is controlled to-5 degrees celsius by a gas-liquid separation control device (not shown), and the corresponding pressure is 0.23 mpa.
After the liquid-solid separation treatment is completed, a shut-off valve (not shown) arranged in the second connecting pipeline 222 is opened, the substances in the liquid-solid separation tank 221 are conveyed towards the gas-liquid separation tank 231 with the aid of an axial flow pump (not shown), and solid substances such as plant tissues and the like possibly entrained in the extraction mixture are intercepted by a screen mesh (not shown) arranged between the top and a side wall outlet in the liquid-solid separation tank 221, so that the liquid dimethyl ether and the essential oil in the liquid-solid separation tank 221 enter the gas-liquid separation tank 231; and then a shut-off valve (not shown) provided to the second connection line 222 is closed.
The liquid dimethyl ether and the essential oil that enter the gas-liquid separation tank 231 stay at a temperature of-5 ℃ and a pressure of 0.23 mpa for 40 minutes to complete the gas-liquid separation treatment. During the gas-liquid separation treatment, the dimethyl ether entering the gas-liquid separation tank 231 is converted into a gas state, while the crude orange oil and water are still in a liquid state and settle at the bottom of the gas-liquid separation tank 231, and the crude orange oil and the water phase can be separated by density difference, so that 7.5 g and 17.5 g of the crude orange oil and the water phase containing the water-soluble orange essential oil are respectively obtained.
After the gas-liquid separation treatment is completed, two shut-off valves (not shown) disposed in the third connecting pipeline 232 and the fourth connecting pipeline 242 are opened, the gaseous dimethyl ether is pressurized under the action of the compressor 241 to form liquid dimethyl ether, and the temperature of the liquid dimethyl ether is raised to 5 ℃, so as to flow back to the extraction tank 211 through the fourth connecting pipeline 242.
Example 2
Example 2 provides a second extraction method of crude citrus essential oil by means of batch treatment using said extraction device 2, said second extraction method being distinguished from said first extraction method by:
500 g of wet orange peel is taken and put into the extraction tank 211, and the mass ratio of dimethyl ether to the wet orange peel is 2: 1;
the temperature of the extraction treatment is 40 ℃, the corresponding pressure is 0.90 MPa, and the time is 30 minutes;
the temperature of the liquid-solid separation treatment is 40 ℃, the corresponding pressure is 0.90 MPa, and the time is 5 minutes;
the other operating steps are as described in example 1. After separation, 10.2 g and 19.5 g of crude orange oil and an aqueous phase containing water-soluble orange essential oil are obtained.
Example 3
Example 3 provides a third extraction method for obtaining citrus crude essential oil by batch treatment using the extraction device 2, wherein 500 g of wet orange peel is placed in the extraction tank 211, and the mass ratio of dimethyl ether to wet orange peel is 2: 1.
The operating conditions of the extraction unit and the liquid-solid separation unit were kept constant compared to the second extraction process, the temperature and corresponding pressure of the gas-liquid separation unit were higher than those of the gas-liquid separation unit in the second extraction process, the temperature of the gas-liquid separation treatment in the third extraction process was 30 degrees celsius, the corresponding pressure was 0.69 mpa, and the time was 20 minutes.
The other operating steps are as described in example 2. After separation, 9.4 g and 19.0 g of crude orange oil and an aqueous phase containing water-soluble orange essential oil are obtained.
The liquid extraction products obtained in the embodiments 1-3 of the invention are transparent orange, and have obvious water-oil stratification phenomenon. Wherein the oil phase material has a density lower than water and a viscosity higher than that of the water phase material, and has an obvious orange sweet taste. The water phase substance is light yellow and also has orange sweet taste.
The above examples further illustrate: under the condition that other operation conditions are not changed, the dosage of the extracting agent is increased, the extraction temperature is increased, and the yield of the essential oil of the oranges and the water-soluble substances in the oranges can be increased. When the mass ratio of the extracting agent to the orange peel raw material is from 1:1 is increased to 2: 1. when the extraction temperature is increased from 5 ℃ to 40 ℃, the yields of the orange essential oil and the water phase substances are respectively increased by 36 percent and 11.4 percent; under the condition that other operation conditions are not changed, the temperature of the gas-liquid separation operation is increased, and although the gas-liquid separation time can be shortened, the separated orange essential oil and the separated water-phase substance are respectively reduced by 7.8 percent and 2.6 percent.
In some embodiments of the present invention, the extraction apparatus 2 further includes a liquid-liquid separation device, the liquid-liquid separation device is connected to the gas-liquid separation tank 231 of the gas-liquid separation device 23, and after the step S2 is finished, the liquid-liquid separation device performs liquid-liquid separation on the liquid extraction product in the gas-liquid separation tank 231 to obtain crude essential oil and water-phase substances, where the water-phase substances include water-soluble orange essential oil.
Specifically, the crude essential oil and the water phase substance are obtained by adopting a gravity settling method or a centrifugal separation method.
Although the embodiments of the present invention have been described in detail hereinabove, it is apparent to those skilled in the art that various modifications and variations can be made to these embodiments. However, it is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention as described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (14)
1. A method for extracting essential oil from citrus plants is characterized by comprising the following steps:
s0: providing extraction equipment, plant tissues derived from citrus plants and an extracting agent, wherein the extraction equipment comprises an extraction device, a separation device and a pressurizing and refluxing device, and the water content of the plant tissues is not lower than 5%;
s1: extracting the plant tissue by a liquid extracting agent in the extraction device to obtain an extraction mixture;
s2: carrying out liquid-solid separation treatment and gas-liquid separation treatment on the extraction mixture through the separation device to obtain a liquid extraction product and a gaseous extraction agent;
s3: carrying out pressurization backflow treatment on the gaseous extracting agent through the pressurization backflow device so as to enable the formed liquid extracting agent to flow back into the extraction device;
controlling the extraction treatment and the liquid-solid separation treatment to be carried out in the same temperature range and the same pressure range, and controlling the highest pressure of the gas-liquid separation treatment to be lower than the lowest pressure of the liquid-solid separation treatment.
2. The extraction method according to claim 1, wherein the liquid extractant is a single-component extractant and is gaseous at normal temperature and pressure.
3. The extraction method according to claim 2, wherein the extraction treatment and the liquid-solid separation treatment are both performed at a pressure of 0.2 to 1.5 mpa and a temperature of 0 to 60 degrees celsius, and the mass ratio of the plant tissue to the extractant is 0.1:1 to 5: 1.
4. The extraction process according to claim 3, wherein the gas-liquid separation treatment is carried out at a pressure of 0.1 to 1.0 MPa and a temperature of-20 to 40 ℃.
5. The extraction process according to claim 4, wherein the liquid extractant formed by the pressure-enhanced reflux treatment has the same temperature as the liquid extractant in the extraction apparatus.
6. The extraction method according to claim 2, wherein the extraction agent is any one of dimethyl ether, petroleum ether, ethanol, acetone, butane and freon.
7. The extraction method according to claim 1, wherein in step S0, an original plant tissue is obtained from the citrus plant, and the plant tissue is obtained by washing the original plant tissue.
8. The extraction process of claim 7, wherein the original plant tissue is at least one of fruit, pericarp, leaf, flower, stem, seed, bark and root.
9. The extraction process according to claim 1, wherein any two of the extraction apparatus, the separation apparatus and the pressure-increasing reflux apparatus are communicated with each other, and the extraction process, the liquid-solid separation process, the gas-liquid separation process and the pressure-increasing reflux process are performed by a continuous operation to form a cyclic process.
10. The extraction method according to claim 9, characterized in that a pumping device is arranged between the extraction device and the separation device, and after the step S1 is finished, the extraction mixture is introduced into the separation device through the pumping device.
11. The extraction method according to claim 10, wherein in the step S2, the pressure of the liquid-solid separation process is controlled to be lower than the pressure of the extraction process so that the extraction mixture is introduced into the separation device by a pressure difference.
12. The extraction method according to claim 9, wherein a conducting device is further provided between any two of the extraction device, the separation device and the pressure-increasing reflux device, and the cyclic treatment process is converted into an intermittent treatment process by controlling the on/off of the conducting device.
13. The extraction method according to claim 9, wherein the separation device is provided with a filtering device, and in the step S2, the solid matter is intercepted by the filtering device.
14. The extraction method as claimed in claim 9, wherein the extraction equipment further comprises a liquid-liquid separation device, and after the step S2 is finished, the liquid-liquid separation device is used for performing liquid-liquid separation treatment on the liquid extraction product to obtain crude essential oil.
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| CN202010920276.7A CN112094697A (en) | 2020-09-04 | 2020-09-04 | Extraction method of citrus essential oil |
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| CN202010920276.7A CN112094697A (en) | 2020-09-04 | 2020-09-04 | Extraction method of citrus essential oil |
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