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Preparation method of cannabidiol crystals

A technology of cannabidiol and crystals, which is applied in the field of preparation of high-purity cannabidiol crystals, can solve the problems of complex operation, waste of resources, and low extraction rate, and achieve low organic solvent consumption, short production cycle, and simple operation Effect

Active Publication Date: 2019-09-27
云南翰谷生物科技有限公司
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Problems solved by technology

[0005] However, the traditional column chromatography process is extremely complex, high production cost, low extraction rate, easy to cause waste of resources, greater environmental pollution, and the macroporous adsorption resin and polyamide chromatography column used have a short service life
More importantly, the effect of column chromatography depends heavily on the conditions of each operation and the proficiency of the operator, so that the quality of the obtained product (purity, impurity type and content, color, crystal morphology, etc.) fluctuates greatly and cannot be obtained. Meet the requirements of industrial production
[0006] Supercritical fluid or subcritical fluid extraction technology has problems such as high equipment requirements, high production cost, and complicated operation. Moreover, the purity of cannabidiol obtained is still low, and it is not suitable for use in the medical field
Existing solvent extraction usually requires enzymatic hydrolysis pretreatment of raw materials, the solvent consumption is huge, the extraction rate is very low, and the subsequent separation process is complicated and cumbersome
[0007] Both biosynthesis and chemical synthesis currently have low production efficiencies
Moreover, since CBD has multiple chiral centers and cis-trans isomeric double bonds, the separation and purification steps are complicated and the cost is high
Therefore, biosynthesis and chemical synthesis are only suitable for synthesizing a small amount of samples, and are currently not suitable for large-scale industrial applications.
[0008] In addition, the existing methods are difficult to effectively and stably control the THC content <0.3%, which is difficult to meet the requirements of the safety supervision department, and is not conducive to the transportation, storage and use of cannabidiol products

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  • Preparation method of cannabidiol crystals
  • Preparation method of cannabidiol crystals
  • Preparation method of cannabidiol crystals

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preparation example Construction

[0029] Specifically, the present invention provides a method for preparing cannabidiol crystals, characterized in that the method comprises the following steps:

[0030] (1) Decarboxylation and extraction are carried out to the floral and leaf powder of industrial hemp to obtain a decarboxylated extract;

[0031] (2) Mixing the decarboxylated extract with the first solvent, standing for precipitation at a temperature lower than 20°C, separating and removing the precipitate, and concentrating the solvent containing cannabidiol to obtain a concentrated extract;

[0032] (3) The concentrated extract is mixed with a second solvent and filtered, and the filtrate is subjected to high-pressure preparative liquid chromatography to collect fractions containing cannabidiol, and then remove the solvent in the fractions to obtain crude cannabidiol;

[0033] (4) The cannabidiol crude product is mixed with a crystallization solvent, and crystallized at a temperature lower than room temperat...

Embodiment 1

[0086] Weigh 10 kg of industrial hemp leaf powder with a particle size of 60 meshes and a CBD content of 0.94%, and decarboxylate it at 100° C. for 2 hours at high temperature.

[0087] Then, under heating to keep the temperature at 60°C, mix the decarboxylated powder and n-hexane at a weight ratio of 1:6, extract for 2 hours under stirring, and recover CBD-containing n-hexane. Repeat the extraction step 2 more times. The recovered n-hexanes were combined, evaporated and concentrated to obtain 690 g of extract extract with a CBD content of 13.4%.

[0088] The extract was mixed with absolute ethanol at a weight ratio of 1:10, and left to settle at 4°C for 4 hours, and then DL-6000B low-speed refrigerated centrifuge was centrifuged at 1000rpm to remove the sediment. Concentrate the absolute ethanol containing CBD to obtain 580 g of treated extract with a CBD content of 15.3%.

[0089] Weigh 200g of the treated extract and mix it with a mixed solvent of petroleum ether and acet...

Embodiment 2

[0093] Weigh 10 kg of industrial hemp leaf powder with a particle size of 60 meshes and a CBD content of 0.94%, and decarboxylate it at 100° C. for 2 hours at high temperature.

[0094] Then, under heating to keep the temperature at 60°C, mix the decarboxylated powder with 95% ethanol at a weight ratio of 1:6, extract for 2 hours under stirring, and recover CBD-containing ethanol. Repeat the extraction step 2 more times. The recovered ethanol was combined, evaporated and concentrated to obtain 1780 g of extract extract with a CBD content of 5.12%.

[0095] The extract was mixed with absolute ethanol at a weight ratio of 1:10, and left to settle at 4°C for 4 hours, and then centrifuged at 1000rpm in a low-speed refrigerated centrifuge to remove the sediment. Concentrate the absolute ethanol containing CBD to obtain 760 g of treated extract with a CBD content of 11.6%.

[0096] Weigh 200g of the treated extract and mix it with a mixed solvent of petroleum ether and acetone (th...

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Abstract

The invention relates to a preparation method of cannabidiol crystals. The preparation method comprises following steps: 1, industrial hemp flower and leaf powder is subjected to decarboxylation and extraction so as to obtain a decarboxylation extracted product; 2, the decarboxylation extracted product is mixed with a first solvent, an obtained mixture is allowed to stand at a low temperature for precipitation, a precipitate is removed, the obtained solvent containing cannabidiol is subjected to concentration so as to obtain a concentrated extracted product; 3, the concentrated extracted product is mixed with a second solvent, filtering is carried out, an obtained filtrate is subjected to high pressure preparation liquid chromatogram treatment, a fraction containing cannabidiol is collected, and the solvent in the fraction is removed so as to obtain a cannabidiol crude product; and 4, the cannabidiol crude product is mixed with a crystallization solvent, and crystallization is carried out at a low temperature so as to obtain the cannabidiol crystasl. The preparation method is capable of obtaining the high purity cannabidiol crystals at a high total extraction rate, is low in energy consumption and organic solvent consumption amount, is capable of saving more energy, is more friendly to the environment, and is more specifically to be used in industrial applications.

Description

technical field [0001] The invention relates to the field of industrial preparation of cannabinoid crystals, in particular to a preparation method of high-purity cannabidiol crystals. Background technique [0002] Cannabis (Cannabis sativa L.) is an annual herb with important economic value and medicinal value, also known as hemp, hemp, hemp, mountain silk hemp, jute and industrial hemp. The main active substances in cannabis are cannabinoids, which mainly include tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN) and its carboxyl compounds. [0003] Among cannabinoid compounds, CBD is a non-addictive component in cannabis, which can inhibit the adverse effects of certain polyphenols on the human nervous system, and has a series of functions such as blocking breast cancer metastasis, treating epilepsy, and anti-rheumatoid arthritis. Physiologically active function. In recent years, cannabidiol has attracted widespread attention in the fields of medicine, food,...

Claims

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Application Information

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IPC IPC(8): C07C37/68C07C37/84C07C39/23
CPCC07C37/004C07C37/84C07C2601/16C07C39/23
Inventor 李琳婧肖丰坤雷鹏陈黎飞施豪
Owner 云南翰谷生物科技有限公司
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