阅读说明：本技术 一种用于提纯大麻二酚的结晶工艺 (Crystallization process for purifying cannabidiol ) 是由 周宇平 蒋忠秋 于 2020-04-14 设计创作，主要内容包括：本发明涉及一种用于提纯大麻二酚的结晶工艺,属于化学提取技术领域。将待处理的大麻二酚原料放置于乙醇溶液中混合并形成第一混合物,向第一混合物中加入纯化水并搅拌均匀形成第二混合物,再将第二混合物过滤并得到第一大麻二酚晶体；将干燥后的第一大麻二酚晶体放置到正己烷溶液中进行搅拌形成第三混合物,过滤后经真空干燥得到第二大麻二酚晶体；将淋洗后的第二大麻二酚晶体放置于真空干燥箱中干燥。本发明的有益之处是：将大麻二酚原料通过结晶工艺进行多次结晶提取,通过提纯实现了大麻二酚晶体中大麻二酚的含量大于等于99.5%且大麻贴酚的含量小于等于0.1%的目的,从而实现了高纯度提取的目的,本发明工艺新颖,操作方便,提纯效果较好。(The invention relates to a crystallization process for purifying cannabidiol, belonging to the technical field of chemical extraction. Placing cannabidiol raw materials to be treated in an ethanol solution, mixing to form a first mixture, adding purified water into the first mixture, uniformly stirring to form a second mixture, and filtering the second mixture to obtain first cannabidiol crystals; placing the dried first cannabidiol crystal into a normal hexane solution, stirring to form a third mixture, filtering, and performing vacuum drying to obtain a second cannabidiol crystal; and (4) placing the washed second cannabidiol crystals in a vacuum drying oven for drying. The invention has the advantages that: the cannabidiol raw material is crystallized and extracted for multiple times through a crystallization process, and the purposes that the content of cannabidiol in cannabidiol crystals is more than or equal to 99.5 percent and the content of cannabilabrin is less than or equal to 0.1 percent are achieved through purification, so that the purpose of high-purity extraction is achieved.)

1. A crystallization process for purifying cannabidiol, characterized in that the crystallization process comprises the steps of:

A. placing cannabidiol raw material (1) to be treated in ethanol solution to be mixed to form a first mixture (2), and placing the first mixture (2) in an environment of 15-30 ℃ to be stirred for 10 minutes;

B. after the cannabidiol raw material (1) in the first mixture (2) is completely dissolved into the ethanol solution, adding purified water (3) into the first mixture (2) and uniformly stirring to form a second mixture (4), standing the second mixture (4) in an environment at-20 ℃ and crystallizing for 12 hours, and filtering the second mixture (4) to obtain a first cannabidiol crystal (5);

C. placing the first cannabidiol crystal (5) in a suction filter funnel which is opened to vacuum, leaching the first cannabidiol crystal (5) by using a 50% -60% acetonitrile water solution, placing the leached first cannabidiol crystal (5) in a vacuum drying oven for drying, wherein the temperature of the vacuum drying oven is more than or equal to 45 ℃;

D. placing the dried first cannabidiol crystal (5) into a normal hexane solution, stirring to form a third mixture (6), placing the third mixture (6) in an environment of-20 ℃ for crystallization for 12 hours after the first cannabidiol crystal (5) in the third mixture (6) is completely dissolved, filtering, and performing vacuum drying to obtain a second cannabidiol crystal (7);

E. placing the second cannabidiol crystal (7) in a vacuum filtration funnel, leaching the second cannabidiol crystal (7) by using a 50% -60% acetonitrile water solution, placing the leached second cannabidiol crystal (7) in a vacuum drying oven for drying, and thus obtaining a high-purity cannabidiol crystal (8) with the purity of more than or equal to 99.5%, wherein the temperature of the vacuum drying oven is more than or equal to 45 ℃.

2. A crystallization process for purifying cannabidiol as claimed in claim 1, wherein: the content of the cannabidiol in the cannabidiol raw material (1) is more than or equal to 80%.

3. A crystallization process for purifying cannabidiol as claimed in claim 1, wherein: the cannabidiol raw material (1) and the ethanol solution are mixed according to a ratio of 1 g: mixing at a ratio of 5ml to 10 ml.

4. A crystallization process for purifying cannabidiol as claimed in claim 1, wherein: the volume of the purified water (3) corresponds to 40-50% of the volume of the ethanol solution used.

5. A crystallization process for purifying cannabidiol as claimed in claim 1, wherein: the ratio of the first cannabidiol crystals (5) to the aqueous acetonitrile solution is 1 g: 5ml to 10 ml.

6. A crystallization process for purifying cannabidiol as claimed in claim 1, wherein: the ratio of the first cannabidiol crystal (5) to the n-hexane solution is 1 g: 4 ml.

7. A crystallization process for purifying cannabidiol as claimed in claim 1, wherein: the ratio of the second cannabidiol crystals (7) to the aqueous acetonitrile solution is 1 g: 5ml to 10 ml.

The technical field is as follows:

the invention relates to a crystallization process for purifying cannabidiol, belonging to the technical field of chemical extraction.

Background art:

cannabidiol, CBD, english: cannabidial is a pure natural ingredient extracted from the cannabis plant. The cannabidiol has a molecular formula of C21H30O2, is white to light yellow resin or crystal in character, has a melting point of 66-67 ℃, is hardly dissolved in water, and is dissolved in organic solvents such as ethanol, methanol, ether, benzene, chloroform and the like. Cannabidiol has the functions of blocking the adverse effect of certain polyphenol on the nervous system of a human body, blocking breast cancer metastasis, treating epilepsy, resisting rheumatoid arthritis, resisting insomnia and other physiological activities, and has a good effect of treating multiple sclerosis.

The impurities in the prior cannabidiol are mainly cannabilabrin, namely CBG, in order to obtain high-purity cannabidiol, the cannabidiol needs to be crystallized for multiple times, but the prior cannabidiol product process cannot reduce the content of the cannabilabrin in the crystallization process, and if the cannabidiol is crystallized for multiple times, the content of the cannabilabrin is increased, so that the purity of the cannabidiol is reduced, and the efficacy of the cannabidiol is reduced.

The invention content is as follows:

the technical problem to be solved by the invention is as follows: provides a crystallization process for purifying cannabidiol, which aims to solve the problems in the industry at present.

In order to solve the technical problems, the invention is realized by the following technical scheme: a crystallization process for purifying cannabidiol, the crystallization process comprises the following steps:

A. placing cannabidiol raw material to be treated in an ethanol solution to mix and form a first mixture, and placing the first mixture in an environment of 15-30 ℃ to stir for 10 minutes.

B. And after the cannabidiol raw material in the first mixture is completely dissolved into the ethanol solution, adding purified water into the first mixture, uniformly stirring to form a second mixture, standing the second mixture in an environment at-20 ℃, crystallizing for 12 hours, and filtering the second mixture to obtain the first cannabidiol crystals.

C. Placing the first cannabidiol crystal into a suction filter funnel which is opened to vacuum, leaching the first cannabidiol crystal by using a 50-60% acetonitrile water solution, placing the leached first cannabidiol crystal into a vacuum drying oven for drying, wherein the temperature of the vacuum drying oven is more than or equal to 45 ℃.

D. And placing the dried first cannabidiol crystals into a normal hexane solution, stirring to form a third mixture, placing the third mixture in an environment of-20 ℃ for crystallization for 12 hours after the first cannabidiol crystals in the third mixture are completely dissolved, filtering, and performing vacuum drying to obtain second cannabidiol crystals.

E. Placing the second cannabidiol crystal into a vacuum filtration funnel, leaching the second cannabidiol crystal by using a 50-60% acetonitrile water solution, placing the leached second cannabidiol crystal into a vacuum drying oven for drying, and obtaining the high-purity cannabidiol crystal with the purity of more than or equal to 99.5%, wherein the temperature of the vacuum drying oven is more than or equal to 45 ℃.

Preferably, the content of cannabidiol in the cannabidiol raw material is greater than or equal to 80%.

Preferably, the cannabidiol feedstock and the ethanol solution are mixed in a 1 g: mixing at a ratio of 5ml to 10 ml.

Preferably, the volume of said purified water corresponds to 40% to 50% of the volume of the ethanol solution used.

Preferably, the ratio of the first cannabidiol crystals to the aqueous acetonitrile solution is 1 g: 5ml to 10 ml.

Preferably, the ratio of the first cannabidiol crystals to the n-hexane solution is 1 g: 4 ml.

Preferably, the ratio of the second cannabidiol crystals to the aqueous acetonitrile solution is 1 g: 5ml to 10 ml.

Compared with the prior art, the invention has the advantages that: the cannabidiol raw material is crystallized and extracted for multiple times through a crystallization process, and the purposes that the content of cannabidiol in cannabidiol crystals is more than or equal to 99.5 percent and the content of cannabilabrin is less than or equal to 0.1 percent are achieved through purification, so that the purpose of high-purity extraction is achieved.

Description of the drawings:

the invention is further described below with reference to the accompanying drawings.

FIG. 1 is a process flow diagram of the present invention.

In the figure: cannabidiol raw material 1; a first mixture 2; purifying the water 3; a second mixture 4; a first cannabidiol crystal 5; a third mixture 6; second cannabidiol crystals 7; high purity cannabidiol crystals 8.

The specific implementation mode is as follows:

the invention is described in detail below with reference to the following figures and embodiments: