CN105754719A - A method for extracting volatile oil from agarwood leaves by simultaneous distillation and extraction technology - Google Patents

Abstract

The invention discloses a method for extracting volatile oil from agarwood leaves by adopting a simultaneous distillation extraction technology. The method combines two steps of distillation of agarwood leaf aqueous solution and solvent extraction into one. Most steps of the method are carried out in a simultaneous distillation extraction device. The operation is simple, convenient and practical, and easy to industrialize. In addition, the method enables water vapor containing agarwood leaf volatile oil to meet and fully contact with dichloromethane vapor above the simultaneous distillation extraction device, which is beneficial to the extraction of agarwood leaf volatile oil from the water vapor into the dichloromethane vapor, and is beneficial to reducing the use amount of the solvent, preventing the destruction and volatilization of the effective components in the volatile oil, thereby ensuring the value of the extract.

Description

A method for extracting volatile oil from agarwood leaves by simultaneous distillation and extraction technology

[technical field]

The patent of the present invention relates to a method for extracting volatile oil from agarwood leaves by using simultaneous distillation and extraction technology.

[Background technique]

Agarwood, the wood containing resin in Aquilariasinensis (Lour.) Gilg, a plant of the family Daphneaceae, is a traditional precious medicinal material and natural spice. The effect of strengthening yang and eliminating numbness has been used by traditional Chinese medicine to treat chest and abdominal distension and pain, stomach cold, vomiting and hiccups, kidney deficiency and dyspnea and other diseases. Due to the long cycle of agarwood and its slow growth, it generally takes more than 20 years to mature. At the same time, the wild resources of agarwood have been severely damaged by human over-harvesting for a long time. Agarwood leaves, as the non-medicinal part of Agarwood, can be picked twice a year in large quantities, and the output is relatively large. Pharmacological studies have shown that the volatile oil of agarwood leaves has anti-inflammatory and analgesic effects, hemostasis and facilitation, anti-oxidation and anti-aging effects. At the same time, it can also be used as a spice to make high-end perfumes, soaps, essences and cosmetics, etc., with high economic value.

At present, the commonly used methods for extracting the volatile oil of Agarwood leaves include steam distillation, solvent extraction, and _CO2 supercritical fluid extraction. The steam distillation method is easy to cause the destruction and volatilization of the active ingredients in the volatile oil, thereby reducing the value of the extract; the solvent extraction method needs to consume a large amount of high-purity organic solvent, and the extraction time is long, which is easy to cause environmental pollution; and _CO2 supercritical fluid Although the biological activity of the extraction method is not easy to be destroyed, and there is no residual organic solvent, the cost of equipment is large, the technical requirements are high, and it is not suitable for industrialization.

Therefore, it is necessary to solve the above problems.

[Content of the invention]

The invention overcomes the disadvantages of the above-mentioned technologies, and provides a method for extracting volatile oil from agarwood leaves by adopting simultaneous distillation and extraction technology. The method is simple, convenient and practical in operation, and is applicable to industrial production.

To achieve the above object, the present invention adopts the following technical solutions:

A method for extracting volatile oil from agarwood leaves by simultaneous distillation and extraction technology, comprising the following steps:

Step 101, pulverize agarwood leaves, pass through a sieve, put the agarwood leaf powder that has passed the sieve into the material bottle 28, and soak in water for a period of time to form an aqueous solution of agarwood leaves, and add dichloromethane into the solvent bottle 29;

Step 102, the material bottle 28 and the solvent bottle 29 are connected to the simultaneous distillation extraction device, and the simultaneous distillation extraction device is provided with an extraction/condensation chamber 20, a material bottle connecting pipe 21, a solution bottle connecting pipe 22, a condenser 23, a U-shaped condensate collecting pipe 24 and discharge valve 25, the condensate entering side of the U-shaped condensate collecting pipe 24 is communicated with the first return pipe 26 between the material bottle connecting pipe 21, and the U-shaped condensate collecting pipe 24 There is a second return pipe 27 connected between the non-condensate inlet side and the solution bottle connecting pipe 22. During work, first close the discharge valve 26 of the U-shaped condensate collecting pipe 24, and heat the material bottle 28 and the solvent bottle 29 respectively. , wherein, the heating temperature of the material bottle 28 is 90°C to 100°C, the heating temperature of the solvent bottle 29 is 60°C to 65°C, and the heating sequence is controlled so that the dichloromethane in the solvent bottle 29 is higher than that in the material bottle 28. Agarwood leaf aqueous solution evaporates earlier so that the steam of dichloromethane condenses and fills U-shaped condensate collecting pipe 24 to a certain height under the effect of condenser 23;

Step 103, during the distillation and extraction process, the condensate is continuously condensed to fill the U-shaped condensate collection pipe 24, and a layered water phase and methylene chloride phase are formed in the U-shaped condensate collection pipe 24, and the excess water phase passes through the first reflux Pipe 26 is refluxed in material bottle 28, and too much dichloromethane phase is refluxed in solvent bottle 29 by the second reflux pipe 27, stops the heating to material bottle 28 and solvent bottle 29 after continuous circulation distillation extraction for a period of time, then opens The discharge valve 25 collects the methylene chloride phase liquid in the lower floor in the U-shaped condensate collection pipe 24 with a solvent bottle 29;

Step 104, add excess anhydrous sodium sulfate to the collected dichloromethane phase liquid to dry, then centrifuge to take the upper layer liquid, and finally distill and concentrate until there is no smell of dichloromethane, and concentrate to obtain a yellow transparent liquid which is the volatile oil of agarwood leaves .

As an optimized embodiment, in step 101, the time for soaking the powder of Agarwood leaves in water is 8-10 hours.

As an optimized implementation, in step 101, the sieve used is a 20-mesh sieve.

As an optimized implementation, in step 101, the solid-liquid ratio of the agarwood leaf powder to water is 1g:7mL˜1g:8mL.

As an optimized implementation, in step 102, the material bottle 28 is heated by an electric heating mantle, and the solvent bottle 29 is heated by a water bath.

As an optimized implementation, in step 103, the time for distillation and extraction is 6-7 hours.

As an optimized implementation, in step 102, it also includes putting zeolite into the material bottle 28 before heating to prevent bumping of the aqueous solution of Agarwood leaves.

Compared with prior art, the beneficial effect of the present invention is:

1. In this case, the simultaneous distillation and extraction technology is used to extract the volatile oil in the leaves of Agarwood, which combines the two steps of aqueous distillation and solvent extraction of Agarwood leaves into one. Most of the steps of the method are carried out in a simultaneous distillation and extraction device, which is simple and convenient to operate Practical and easy for industrialized production, and the method is used to make the water vapor containing the volatile oil of the agarwood leaf and the dichloromethane vapor meet at the top of the simultaneous distillation extraction device, and fully contact, which is beneficial for the volatile oil of the agarwood leaf to be extracted from the water vapor to the methylene chloride vapor Among them, it is beneficial to reduce the amount of solvent used, prevent the destruction and volatilization of the active ingredients in the volatile oil, thereby ensuring the value of the extract; in addition, the density of dichloromethane is greater than that of water and is incompatible with water, which is beneficial to dichloromethane and water. Stratification is formed in the U-shaped condensate collection pipe; and when heating is started, the heating sequence is controlled so that the dichloromethane in the solvent bottle evaporates earlier than the aqueous solution of the agarwood leaves in the material bottle, so that the vapor of the dichloromethane first evaporates under the action of the condenser The lower condensate fills the U-shaped condensate collection pipe to a certain height to prevent the water after evaporation and condensation of the agarwood leaf aqueous solution from entering the other side of the U-shaped condensate collection pipe, and as the condensate increases, it finally enters the solvent through the second return pipe In the bottle; the heating temperature of the material bottle in this case is 90°C-100°C, which can not affect the active ingredients of the volatile oil of the agarwood leaves under the condition of continuous generation of water vapor in the material bottle, and the heating temperature of the solvent bottle is 60°C-65°C, It can continuously generate dichloromethane vapor in the solvent bottle to realize the distillation and extraction of the volatile oil in the agarwood leaves.

2. The higher the degree of fragmentation of agarwood leaves, that is, the smaller the particles, the easier it is to evaporate the volatile oil. Because the smaller the particles, the larger the specific surface area, the larger the contact area, and the shorter the distance for the oil to diffuse from the inside of the agarwood leaf to the surface, so it is easier to separate out from the agarwood leaf.

3. For the aqueous solution of agarwood leaves, increasing the proportion of water will make the water dispersion of agarwood leaves more sufficient, which can improve the extraction rate, but with the further increase of water, the heating time will be relatively prolonged, resulting in an increase in the amount of oil volatilization and hydrolysis, thus The extraction rate is reduced. Therefore, the test in this case shows that the extraction rate is the best when the solid-liquid ratio of agarwood leaf powder to water is 1g:7mL～1g:8mL.

4. Putting zeolite into the material bottle before heating is beneficial to prevent bumping of the agarwood leaf aqueous solution.

[Description of drawings]

Fig. 1 is a flow chart of the method of the present invention.

Fig. 2 is a schematic diagram of a simultaneous distillation extraction device, wherein, 20 is an extraction/condensation chamber, 21 is a material bottle connecting pipe, 22 is a solution bottle connecting pipe, 23 is a condenser, 231 is a condenser cooling water inlet, and 232 is a Cooling water outlet of the condenser, 24 is a U-shaped condensate collecting pipe, 25 is a discharge valve, 26 is a first return pipe, 27 is a second return pipe, 28 is a material bottle, and 29 is a solvent bottle.

[detailed description]

The features of the present invention and other related features will be further described in detail below in conjunction with the accompanying drawings through embodiments, so as to facilitate the understanding of those skilled in the art:

As shown in Figure 1-2, a method for extracting volatile oil in Agarwood leaves by simultaneous distillation and extraction technology includes the following steps:

Step 101, pulverize agarwood leaves, pass through a sieve, put the agarwood leaf powder that has passed the sieve into the material bottle 28, and soak in water for a period of time to form an aqueous solution of agarwood leaves, and add dichloromethane into the solvent bottle 29;

Step 102, the material bottle 28 and the solvent bottle 29 are connected to the simultaneous distillation extraction device, and the simultaneous distillation extraction device is provided with an extraction/condensation chamber 20, a material bottle connecting pipe 21, a solution bottle connecting pipe 22, a condenser 23, a U-shaped condensate collecting pipe 24 and discharge valve 25, the condensate entering side of the U-shaped condensate collecting pipe 24 is communicated with the first return pipe 26 between the material bottle connecting pipe 21, and the U-shaped condensate collecting pipe 24 There is a second return pipe 27 connected between the non-condensate inlet side and the solution bottle connecting pipe 22. During work, first close the discharge valve 26 of the U-shaped condensate collecting pipe 24, and heat the material bottle 28 and the solvent bottle 29 respectively. , wherein, the heating temperature of the material bottle 28 is 90°C to 100°C, the heating temperature of the solvent bottle 29 is 60°C to 65°C, and the heating sequence is controlled so that the dichloromethane in the solvent bottle 29 is higher than that in the material bottle 28. Agarwood leaf aqueous solution evaporates earlier so that the steam of dichloromethane condenses and fills U-shaped condensate collecting pipe 24 to a certain height under the effect of condenser 23;

Step 103, during the distillation and extraction process, the condensate is continuously condensed to fill the U-shaped condensate collection pipe 24, and a layered water phase and methylene chloride phase are formed in the U-shaped condensate collection pipe 24, and the excess water phase passes through the first reflux Pipe 26 is refluxed in material bottle 28, and too much dichloromethane phase is refluxed in solvent bottle 29 by the second reflux pipe 27, stops the heating to material bottle 28 and solvent bottle 29 after continuous circulation distillation extraction for a period of time, then opens Discharge valve 25 also collects the dichloromethane phase liquid in lower floor in U-shaped condensate collection pipe 24 with solvent bottle 29;

Step 104, add excess anhydrous sodium sulfate to the collected dichloromethane phase liquid to dry, then centrifuge to take the upper layer liquid, and finally distill and concentrate until there is no smell of dichloromethane, and concentrate to obtain a yellow transparent liquid which is the volatile oil of agarwood leaves .

As mentioned above, the working principle of this case is: the water vapor containing the volatile oil of Agarwood leaves and the dichloromethane vapor meet in the extraction/condensation chamber 20 of the simultaneous distillation extraction device, and they are fully contacted, and the volatile oil of Agarwood leaves is extracted from the water vapor to two In the methyl chloride vapor, then under the effect of the condenser 23, condense and fill the U-shaped condensate collection pipe 24, and because the density of dichloromethane is greater than the water density and is not compatible, the dichloromethane and water are in the U-shaped condensate collection pipe 24 to form layers. In step 102, when heating is started, the heating sequence is controlled so that the dichloromethane in the solvent bottle 29 is evaporated earlier than the aqueous solution of agarwood leaves in the material bottle 28, so that the steam of the dichloromethane is first condensed under the action of the condenser 23 to fill the U-shaped The condensate collection pipe 24 has a certain height, so as to prevent the water after evaporation and condensation of the agarwood leaf aqueous solution from entering the other side of the U-shaped condensate collection pipe 24, and as the condensate increases, it finally enters the solvent bottle 29 through the second return pipe 27 middle. The heating temperature of the material bottle 28 is 90°C to 100°C, which can not affect the active ingredients of the volatile oil of Agarwood leaves under the condition of continuously generating water vapor in the material bottle 28, and the heating temperature of the solvent bottle 29 is 60°C to 65°C. It is possible to continuously generate methylene chloride vapor in the solvent bottle 29. By controlling the heating temperature of the material bottle 28 and the solvent bottle 29, the speeds of condensation and reflux are balanced to realize continuous distillation and extraction.

In step 101, during specific implementation, the soaking time of the agarwood leaf powder is 8-10 hours, the purpose is that the increase of the soaking time can make the water dispersion effect more fully, but the extraction rate does not change much if the soaking time exceeds 10 hours , from the perspective of saving time, choose the soaking time to be 8-10 hours.

In step 101, during specific implementation, the sieve used is a 20-mesh sieve, the purpose of which is that the higher the crushing degree of agarwood leaves, that is, the smaller the particles, the easier the volatile oil is to be evaporated, because the smaller the particles, the larger the specific surface area , the larger the contact area, the shorter the distance that oil diffuses from the inside of the agarwood leaf to the surface, so the easier it is to separate out from the agarwood leaf.

In step 101, during specific implementation, the solid-liquid ratio of agarwood leaf powder to water is 1g:7mL～1g:8mL, the purpose is to increase the proportion of water to make the water dispersion of agarwood leaf more fully, so as to improve the extraction rate, but As the amount of water further increases, the heating time is relatively extended, resulting in an increase in the amount of oil volatilization and hydrolysis, which in turn reduces the extraction rate.

In step 102, during specific implementation, an electric heating mantle is used to heat the material bottle 28, and a water bath is used to heat the solvent bottle 29, and the heating temperature is easy to adjust. In addition, put zeolite into the material bottle 28 before heating to prevent bumping of the Agarwood leaf aqueous solution.

In step 103, during specific implementation, the distillation extraction time is 6-7 hours. The purpose is to increase the extraction rate with the extension of the distillation time, but the extraction for too long will cause the amount of oil volatilization and hydrolysis to increase. , but to reduce the extraction rate.

Specific example 1:

The agarwood leaves are crushed and passed through a 20-mesh sieve, sealed for later use. Accurately weigh 50.00 g of the sieved Agarwood leaf powder, place it in the 3L material bottle 28, add 400 mL of water, soak for 8 hours, add a little zeolite, as shown in Figure 2, connect to the left side of the simultaneous distillation extraction device, and Get 25mL dichloromethane and place in 100mL solvent bottle 29, be connected to the right side of simultaneous distillation extraction device, open condenser 23, close discharge valve 25, then heat solvent bottle 29, make the dichloromethane liquid after the condensation fill U Shape the condensate collecting pipe 24 to a certain height, and then heat the material bottle 28. The material bottle 28 is heated with an electric heating mantle, the temperature is controlled between 90-100°C, and the water is kept boiling to generate steam. The solvent bottle 29 is heated with a constant temperature water bath, and the temperature is controlled between 60-65°C, and continuous distillation and extraction are carried out for 6 hours. After the distillation extraction is finished, cool for 30 minutes, take off the solvent bottle 29, slowly open the discharge valve 25, and collect the methylene chloride phase liquid in the lower layer of the U-shaped condensate collection pipe 24. Add 5g of anhydrous sodium sulfate to the collected dichloromethane phase liquid to dry, leave it to stand for 3 hours and get the supernatant by centrifugation, finally distill and concentrate to no smell of dichloromethane to obtain 0.46g of yellow transparent liquid, namely It is the volatile oil of agarwood leaves, and the calculated yield of the volatile oil of agarwood leaves is 0.92%.

Specific example 2:

The agarwood leaves are crushed and passed through a 20-mesh sieve, sealed for later use. Accurately weigh 75.00 g of the sieved Agarwood leaf powder, place it in the 3L material bottle 28, add 550 mL of water, soak for 10 hours, add a little zeolite, as shown in Figure 2, connect to the left side of the simultaneous distillation and extraction device, and take another 25mL of dichloromethane is placed in a 100mL solvent bottle 29, connected to the right side of the simultaneous distillation extraction device, the condenser 23 is opened, the discharge valve 25 is closed, and the solvent bottle 29 is started to be heated, so that the condensed dichloromethane liquid fills a U-shaped The condensate collecting pipe 24 has a certain height, and then the material bottle 28 is heated. The material bottle 28 is heated with an electric heating mantle, the temperature is controlled between 90-100°C, and the water is kept boiling to generate steam. The solvent bottle 29 is heated with a constant temperature water bath, and the temperature is controlled between 60-65°C, and continuous distillation and extraction are carried out for 7 hours. After the distillation extraction was finished, cool for 30 minutes, take off the solvent bottle 29, slowly open the discharge valve 25, and use the solvent bottle 29 to collect the methylene chloride phase liquid in the lower floor of the U-shaped condensate collection pipe 24. Add 5g of anhydrous sodium sulfate to the collected dichloromethane phase liquid and dry it, leave it to stand for 3 hours and get the supernatant by centrifugation, finally distill and concentrate to no smell of dichloromethane to obtain 0.80g of yellow transparent liquid, namely It is the volatile oil of agarwood leaves, and the calculated yield of the volatile oil of agarwood leaves is 1.07%.

Example 3:

The agarwood leaves are crushed and passed through a 20-mesh sieve, sealed for later use. Accurately weigh 100.00g of the sieved Agarwood leaf powder, place it in the 3L material bottle 28, add 700mL of water, soak for 9 hours, add a little zeolite, as shown in Figure 2, connect to the left side of the simultaneous distillation extraction device, and Get 25mL of dichloromethane and place it in the 100mL solvent bottle 29, connect it to the right side of the simultaneous distillation and extraction device, open the condenser 23, close the discharge valve 25, start heating the solvent bottle 29, and make the condensed dichloromethane liquid fill the outlet Feed pipe, then heat material bottle 28. The material bottle 28 is heated with an electric heating mantle, the temperature is controlled between 90-100°C, and the water is kept boiling to generate steam. The solvent bottle 29 is heated with a constant temperature water bath, and the temperature is controlled between 60-65°C, and continuous distillation and extraction are carried out for 6.5 hours. After the distillation extraction was finished, cool for 30 minutes, take off the solvent bottle 29, slowly open the discharge valve 25, and use the solvent bottle 29 to collect the methylene chloride phase liquid in the lower floor of the U-shaped condensate collection pipe 24. Add 5g of anhydrous sodium sulfate to the collected dichloromethane phase liquid and dry it, leave it to stand for 3 hours and get the supernatant by centrifugation, finally distill and concentrate to no smell of dichloromethane to obtain 1.03g of yellow transparent liquid, namely It is the volatile oil of agarwood leaves, and the calculated yield of the volatile oil of agarwood leaves is 1.03%.

Claims (7)

1. a method for extracting volatile oil in Agarwood leaves by simultaneous distillation and extraction technology, is characterized in that comprising the steps: Step 101, pulverize the agarwood leaves, pass through a sieve, put the agarwood leaf powder through the sieve into the material bottle (28), soak in water for a period of time to form an agarwood leaf aqueous solution, and add dichloromethane to the solvent bottle (29) ; Step 102, connect the material bottle (28) and the solvent bottle (29) to the simultaneous distillation extraction device, and the simultaneous distillation extraction device is provided with an extraction/condensation chamber (20), a material bottle connecting pipe (21), and a solution bottle connection Pipe (22), condenser (23), U-shaped condensate collection pipe (24) and discharge valve (25), the condensate inlet side of the U-shaped condensate collection pipe (24) is connected to the material bottle connection pipe ( 21) is communicated with a first return pipe (26), and a second return pipe (27) is communicated between the non-condensate inlet side of the U-shaped condensate collecting pipe (24) and the solution bottle connecting pipe (22). , first close the discharge valve (26) of the U-shaped condensate collecting pipe (24), and heat the material bottle (28) and the solvent bottle (29) respectively, wherein the heating temperature of the material bottle (28) is 90°C ～100 ℃, the heating temperature of solvent bottle (29) is 60 ℃～65 ℃, and control heating sequence so that dichloromethane in solvent bottle (29) evaporates earlier than the Agarwood leaf aqueous solution in material bottle (28) so that Make the steam of dichloromethane condense and fill the U-shaped condensate collecting pipe (24) to a certain height under the effect of condenser (23) earlier; Step 103, during the distillation and extraction process, the condensate is continuously condensed to fill the U-shaped condensate collection pipe (24), and a layered water phase and methylene chloride phase are formed in the U-shaped condensate collection pipe (24), and the excessive water phase Backflow in the material bottle (28) by the first reflux pipe (26), excessive dichloromethane phase is refluxed in the solvent bottle (29) by the second reflux pipe (27), stops after a period of continuous circulation distillation extraction The heating of material bottle (28) and solvent bottle (29), then open discharge valve (25) and use solvent bottle (29) to collect the dichloromethane phase liquid of lower floor in the U-shaped condensate collection pipe (24); Step 104, add excess anhydrous sodium sulfate to the collected dichloromethane phase liquid to dry, then centrifuge to take the upper layer liquid, and finally distill and concentrate until there is no smell of dichloromethane, and concentrate to obtain a yellow transparent liquid which is the volatile oil of agarwood leaves . 2. A method for extracting volatile oil from agarwood leaves by using simultaneous distillation and extraction technology according to claim 1, characterized in that in step 101, the time for soaking the agarwood leaf powder in water is 8-10 hours. 3. A method for extracting volatile oil from Agarwood leaves by simultaneous distillation and extraction technology according to claim 1, characterized in that in step 101, the sieve used is a 20-mesh sieve. 4. A method for extracting volatile oil from agarwood leaves by using simultaneous distillation and extraction technology according to claim 1, characterized in that in step 101, the solid-liquid ratio of the agarwood leaf powder to water is 1g: 7mL～1g : 8mL. 5. a kind of method that adopts simultaneous distillation extraction technology to extract volatile oil in Agarwood leaves according to claim 1, is characterized in that in step 102, adopts electric heating mantle to heat material bottle (28), adopts water bath to solvent bottle ( 29) Apply heat. 6. A method for extracting volatile oil from Agarwood leaves by simultaneous distillation and extraction technology according to claim 1, characterized in that in step 103, the time for distillation and extraction is 6-7 hours. 7. A method of extracting volatile oil in Agarwood leaves using simultaneous distillation and extraction technology according to any one of claims 1-6, characterized in that in step 102, it is also included in the material bottle (28) before heating Put in zeolite to prevent the water solution of Agarwood leaves from bumping.