阅读说明：本技术 一种草蒿脑制备方法 (Preparation method of estragole ) 是由 徐国平 李国进 饶治平 于 2019-11-23 设计创作，主要内容包括：本发明公开了一种草蒿脑制备方法,其特征是步骤如下:(1)粉碎,浸出得初始料液：将原料洗净晾干,用球磨机或研磨机磨成粉状,再加入醇类物质,浸泡一定时间,得到初始料液；(2)压滤,得滤液：使用300～400目网布过滤,并施加一定压力,即得滤液；(3)分离醇类物质：将滤液加入蒸馏装置中,加热蒸馏分离出醇类物质,加热温度为70～85℃,收集到中间产物；(4)超临界CO2萃取；(5)减压精馏提纯：将初级草蒿脑放入精馏塔,进行二次减压精馏,第二次减压精馏得到的产物即为草蒿脑成品。本发明工序简单,生产成本低,有利于快速提取优质草蒿脑,适用于香料、食品和饮料等行业,便于推广使用。(The invention discloses a method for preparing estragole, which is characterized by comprising the following steps of (1) crushing, leaching to obtain initial feed liquid: cleaning and airing the raw materials, grinding the raw materials into powder by using a ball mill or a grinding machine, adding alcohol substances, and soaking for a certain time to obtain initial feed liquid; (2) and (3) performing filter pressing to obtain filtrate: filtering with 300-400 mesh gauze, and applying certain pressure to obtain filtrate; (3) separating alcohol substances: adding the filtrate into a distillation device, heating and distilling to separate alcohol substances, wherein the heating temperature is 70-85 ℃, and collecting an intermediate product; (4) supercritical CO2 extraction; (5) and (3) rectification and purification under reduced pressure: and (3) putting the primary estragole into a rectifying tower, carrying out secondary vacuum rectification, and obtaining a product, namely the estragole finished product, by the secondary vacuum rectification. The method has simple process and low production cost, is beneficial to quickly extracting the high-quality estragole, is suitable for industries of spices, foods, beverages and the like, and is convenient to popularize and use.)

1. A preparation method of estragole is characterized by comprising the following steps of (1) crushing and leaching to obtain initial feed liquid: cleaning and airing the raw materials, grinding the raw materials into powder by using a ball mill or a grinding machine, adding alcohol substances, and soaking for a certain time to obtain initial feed liquid; (2) and (3) performing filter pressing to obtain filtrate: filtering with 300-400 mesh gauze, and applying certain pressure to obtain filtrate; (3) separating alcohol substances: adding the filtrate into a distillation device, heating and distilling to separate alcohol substances, wherein the heating temperature is 70-85 ℃, and collecting an intermediate product; (4) supercritical CO2 extraction: putting the collected intermediate product into an extraction kettle, preheating the extraction kettle and a separation kettle, opening a CO2 gas cylinder to supply gas when the preset temperature is reached, opening a high-pressure pump to boost the pressure, adjusting the pressure and the temperature, controlling the flow of CO2, starting cyclic extraction, extracting at constant temperature and constant pressure for 1-2 hours, and then discharging to obtain primary estragole; (5) and (3) rectification and purification under reduced pressure: and (3) putting the primary estragole into a rectifying tower, carrying out secondary vacuum rectification, and obtaining a product, namely the estragole finished product, by the secondary vacuum rectification.

2. The method for preparing estragole according to claim 1, wherein: the raw material is green pricklyash peel or star anise.

3. The method for preparing estragole according to claim 1, wherein: the alcohol substance is ethanol and/or isopropanol.

4. The method for preparing estragole according to claim 1, wherein: the pressure applied in the step (2) is 0.3-0.5 Mpa.

5. The method for preparing estragole according to claim 1, wherein: and (4) adjusting the pressure to 10-20 Mpa, the temperature to 40-55 ℃, and controlling the CO2 flow to 50-80L/H.

6. The method for preparing estragole according to claim 1, wherein: the vacuum rectification purification process comprises the following steps: carrying out first vacuum rectification, controlling the temperature of the kettle to be 50-120 ℃ under the pressure of less than 100Pa, and collecting a transitional intermediate product; and (3) carrying out second vacuum rectification, rectifying the intermediate product obtained in the first time again, regulating the kettle temperature to be 85-105 ℃ under the pressure of less than 300Pa, controlling the top temperature to be 62-75 ℃, and collecting the artemisia apiacea product.

Technical Field

The invention belongs to the technical field of spices and fine chemical engineering, and particularly relates to a preparation method of estragole.

Background

Artemisia apiacea Hance is named as common Chinese name, namely p-allyl anisole and p-methoxy phenyl propylene. Colorless to light yellow liquid, has anise-like fragrance, boiling point of 216 ℃, is soluble in ethanol and chloroform and is hardly soluble in water. The natural product is contained in apple, bilberry, aniseed, cider, marjoram, tarragon, fennel, etc. and is mainly used for preparing spices, beer essence and flavoring agent. For bakery products, alcoholic and non-alcoholic beverages, gums, candies, sweetmeats, ice creams, fish, salads, sauces, vinegar and the like, are extremely important flavours, active intermediates.

The estragole is widely present in parts of inflorescences, branches, leaves, stems, fruits, seeds and the like of plants, and particularly has high content in some Chinese herbal medicines and spice plants. Fennel grass, Chinese wampee, anemone leaf, green pepper, violet basil, hairy basil, wrinkled gianthyssop herb, common goldenrod herb and the like are important resources with better development and utilization prospects.

The estragole is one of the important activities of Chinese herbal medicine plants, is one of the main perfume components in essential oil of some important perfume plants, has been applied to the aspects of medicine, pesticide, food additive, fine chemical engineering and the like which need the biological activity, and has better prospect. At present, the method is widely applied to the industries of spices, foods and beverages.

At present, the technology for extracting the estragole from various plants is still immature, the extraction steps are complicated, a large amount of catalyst is consumed, and only a small amount of high-quality estragole can be extracted.

The main preparation methods in the industry at present comprise: 1. is obtained by fractionating turpentine or tarragon oil; 2. obtained by reacting allyl bromide with magnesium p-methoxyphenol. The two methods for preparing the estragole have the defects of harsh preparation conditions, difficult operation, high production cost, serious environmental pollution, low purity of prepared products and the like, and are difficult to be applied on a large scale in production.

Disclosure of Invention

The invention aims to solve the technical problems and provide a preparation method of the estragole which is beneficial to improving the extraction efficiency and high purity.

In order to achieve the purpose, the invention adopts the following technical scheme.

A preparation method of estragole is characterized by comprising the following steps of (1) crushing and leaching to obtain initial feed liquid: cleaning and airing the raw materials, grinding the raw materials into powder by using a ball mill or a grinding machine, adding alcohol substances, and soaking for a certain time to obtain initial feed liquid; (2) and (3) performing filter pressing to obtain filtrate: filtering with 300-400 mesh gauze, and applying certain pressure to obtain filtrate; (3) separating alcohol substances: adding the filtrate into a distillation device, heating and distilling to separate alcohol substances, wherein the heating temperature is 70-85 ℃, and collecting an intermediate product; (4) supercritical CO2 extraction: putting the collected intermediate product into an extraction kettle, preheating the extraction kettle and a separation kettle, opening a CO2 gas cylinder to supply gas when the preset temperature is reached, opening a high-pressure pump to boost the pressure, adjusting the pressure and the temperature, controlling the flow of CO2, starting cyclic extraction, extracting at constant temperature and constant pressure for 1-2 hours, and then discharging to obtain primary estragole; (5) and (3) rectification and purification under reduced pressure: and (3) putting the primary estragole into a rectifying tower, carrying out secondary vacuum rectification, and obtaining a product, namely the estragole finished product, by the secondary vacuum rectification.

Further preferably, the raw material is green pepper or star anise.

Further preferably, the alcohol is ethanol and/or isopropanol.

Further preferably, in the step (2), the pressure applied is 0.3 to 0.5 MPa.

Further preferably, in the step (4), the pressure is adjusted to be 10-20 Mpa, the temperature is adjusted to be 40-55 ℃, and the CO2 flow is controlled to be 50-80L/H.

Further preferably, in the step (5), the vacuum distillation purification process is as follows: carrying out first vacuum rectification, controlling the temperature of the kettle to be 50-120 ℃ under the pressure of less than 100Pa, and collecting a transitional intermediate product; and (3) carrying out second vacuum rectification, rectifying the intermediate product obtained in the first time again, regulating the kettle temperature to be 85-105 ℃ under the pressure of less than 300Pa, controlling the top temperature to be 62-75 ℃, and collecting the artemisia apiacea product.

The invention has the advantages that: 1. firstly, the intermediate product is obtained by adopting the methods of crushing, filter pressing, distillation and the like, and the operation is simple and convenient; 2. by using supercritical CO2 extraction, the extraction efficiency of the product can be improved to the maximum extent, and the yield is greatly improved; 3. purifying by secondary decompression rectification, ensuring the purity of the estragole and obtaining the high-quality estragole finished product.

Detailed Description

The present invention will be explained in further detail below with reference to examples for the purpose of facilitating understanding.