阅读说明：本技术 一种草蒿脑的分离提纯方法 (Separation and purification method of estragole ) 是由 田沁东 于 2020-07-02 设计创作，主要内容包括：本申请公开了一种草蒿脑的分离提纯方法,包括以下步骤：步骤一、准备原料：收集生产茴脑产生的前馏分；步骤二、制备催化剂：取硅藻土置于30％氢氧化钠溶液中,加热至350℃,该温度条件下搅拌合成人工沸石,取出人工沸石清洗、干燥后得到催化剂；步骤三、催化：按重量份数取前馏分100份于容器中,再加入催化剂5-8份,将容器放在油浴锅中,加热搅拌1h,其中加热温度为150-160℃,搅拌速度为320r/min,然后冷却至常温,过滤除掉人工沸石,得到草蒿脑粗品；步骤四、精馏：取步骤三中的草蒿脑粗品加入塔釜中,进行精馏得到草蒿脑成品。本申请通过催化反应和精馏的结合,得到纯度高于99％的草蒿脑成品,提高了市场经济效率。(The application discloses a separation and purification method of estragole, which comprises the following steps: step one, preparing raw materials: collecting the pre-fraction produced in the production of anethole; step two, catalyst preparation: placing diatomite in 30% sodium hydroxide solution, heating to 350 ℃, stirring and synthesizing artificial zeolite under the temperature condition, taking out the artificial zeolite, cleaning and drying to obtain a catalyst; step three, catalysis: taking 100 parts of the front fraction by weight in a container, adding 5-8 parts of a catalyst, placing the container in an oil bath pot, heating and stirring for 1h, wherein the heating temperature is 150-; step four, rectification: and (4) adding the crude product of the estragole in the step three into a tower kettle, and rectifying to obtain the finished product of the estragole. According to the method, the tarragon finished product with the purity higher than 99% is obtained by combining catalytic reaction and rectification, and the market economic efficiency is improved.)

1. A separation and purification method of estragole is characterized in that: the method comprises the following steps:

step one, preparing raw materials: collecting the pre-fraction produced in the production of anethole;

step two, catalyst preparation: placing diatomite in 30% sodium hydroxide solution, heating to 350 ℃, stirring and synthesizing artificial zeolite under the temperature condition, taking out the artificial zeolite, cleaning and drying to obtain a catalyst;

step three, catalysis: taking 100 parts of the front fraction by weight in a container, adding 5-8 parts of a catalyst, placing the container in an oil bath pot, heating and stirring for 1h, wherein the heating temperature is 150-;

step four, rectification: adding the crude product of estragole in the third step into a tower kettle, and rectifying to obtain the final product of estragole, wherein the rectifying step comprises heating, opening the water on the top of the tower, opening a vacuum pump, collecting water, joint oil, and connecting estragole.

2. The method for separating and purifying estragole according to claim 1, wherein the method comprises: in the second step, the weight ratio of the diatomite to the 30% sodium hydroxide solution is 5: 8.

3. The method for separating and purifying estragole according to claim 2, wherein: the container in the third step is a beaker.

4. The method for separating and purifying estragole according to claim 3, wherein the method comprises: the capacity of the sesame seed cake was 2000 ml.

5. The method for separating and purifying estragole according to claim 4, wherein the method comprises: in the fourth step, the heating is carried out by an electric furnace, and the temperature of the tower material is controlled to be 110-.

6. The method for separating and purifying estragole according to claim 5, wherein the method comprises: the pressure provided by the vacuum pump in the fourth step is 4.5mmHg-5.5 mmHg.

7. The method for separating and purifying estragole according to claim 6, wherein: the linker oil in the fourth step is that the monoterpene is collected after the single paste begins to slip out when the temperature of the materials in the tower bottom is 110 ℃.

8. The method for separating and purifying estragole according to claim 7, wherein: the step four, the inoculation of the estragole refers to the step of collecting the estragole by slipping the estragole out when the temperature of the materials in the tower kettle is 150 ℃.

Technical Field

The invention belongs to the technical field of compound extraction and particularly relates to a separation and purification method of estragole.

Background

Artemisia ordosica L.with molecular formula of C10H12O, molecular weight of 148.22, is colorless to pale yellow liquid, and has anise-like fragrance. The boiling point is 216 ℃. Soluble in ethanol and chloroform and practically insoluble in water. The natural product is contained in apple, bilberry, aniseed, cider, marjoram, tarragon, fennel, etc.

With the technical upgrading and transformation of anise processing enterprises, the quality of products such as anise oil, trans-anethole and the like is improved, the yield is increased, and the front fraction (accounting for about 10 percent of the total amount of the anise oil) generated in the production of the anethole is continuously increased. The front fraction is rich in estragole, while the current front fraction of the star anise oil is mainly sold in a low-price commodity and is not effectively utilized. Therefore, the isolation process research is carried out on the estragole in the front fraction of the anise oil, and the additional value of the front fraction is improved.

Currently, the front cut is generally purified by adopting a rectification mode, wherein the rectification temperature is 120 ℃, the vacuum degree is 5mmHg, and the reflux ratio is 7: 6, the purity of the separated estragole reaches 87% -91%, the alpha-terpineol accounts for 5% -8%, and the recovery rate is 83% -87%, but the purity cannot be improved because the alpha-terpineol is difficult to remove, and the market value of the estragole is seriously influenced.

Disclosure of Invention

The invention aims to provide a separation and purification method of estragole, which aims to solve the problem of low purity of estragole obtained by rectifying the prior front cut.

The separation and purification method of estragole in the scheme comprises the following steps:

step one, preparing raw materials: collecting the pre-fraction produced in the production of anethole;

step two, catalyst preparation: placing diatomite in 30% sodium hydroxide solution, heating to 350 ℃, stirring and synthesizing artificial zeolite under the temperature condition, taking out the artificial zeolite, cleaning and drying to obtain a catalyst;

step three, catalysis: taking 100 parts of the front fraction by weight in a container, adding 5-8 parts of a catalyst, placing the container in an oil bath pot, heating and stirring for 1h, wherein the heating temperature is 150-;

step four, rectification: adding the crude product of estragole in the third step into a tower kettle, and rectifying to obtain the final product of estragole, wherein the rectifying step comprises heating, opening the water on the top of the tower, opening a vacuum pump, collecting water, joint oil, and connecting estragole.

Further, the weight ratio of the diatomite to the 30% sodium hydroxide solution in the second step is 5: 8.

Further, the container in the third step is a beaker.

Further, the capacity of the sesame seed cake was 2000 ml.

Further, the heating in the fourth step is electric furnace heating, and the temperature of the tower material is controlled to be 110-.

Further, the pressure provided by the vacuum pump in the fourth step is 4.5mmHg-5.5 mmHg.

Furthermore, the linker oil in the fourth step is that the monoterpene is collected after the single patch begins to slip out when the temperature of the materials in the tower is 110 ℃.

Further, the step four of receiving the estragole refers to that the estragole is slipped out when the temperature of the tower kettle material is 150 ℃, so as to collect the estragole.

The working principle and the beneficial effects of the scheme are as follows: according to the chromatogram, the front fraction mainly contains 92.27% of estragole and 6.78% of alpha-terpineol, the alpha-terpineol in the front fraction is cracked under high-temperature catalysis to generate monoterpenes mainly comprising dipentene, alpha-terpinene and r-terpinene through catalytic reaction, and then the monoterpene in the crude product of the estragole is separated through a rectification step, so that a finished product of the estragole with higher purity is obtained.

Drawings

FIG. 1 is a chromatogram of the components of a front end cut according to the present invention;

FIG. 2 is a chromatogram of crude component of estragole according to the present invention;

FIG. 3 is a chromatogram of the components of the final product of estragole in the present invention.

Detailed Description

The following is further detailed by way of specific embodiments: