阅读说明：本技术 一种用乙醇从工业大麻中提取cbd的工艺 (Process for extracting CBD from industrial hemp by using ethanol ) 是由 刘慧颖 刘冰 于 2021-01-19 设计创作，主要内容包括：本发明公开了一种用乙醇从工业大麻中提取CBD的工艺,该工艺通过以下步骤实现：第1步,将工业大麻花叶清洗晾干切碎处理；第2步,将工业大麻花叶烘干；第3步,烘干后的花叶用无水乙醇进行浸泡制得提取液；第4步,浸泡后花叶由滤网过滤出并加热,剩余的固体或半固体膏状物即为富含CBD的浸膏；第5步,将CBD浸膏进行硅胶柱层析分离,再采用溶剂将其洗脱收集CBD组分,在减压条件下浓缩CBD组分,即可得到CBD粗晶体；第6步,将CBD粗晶体用结晶溶剂进行溶解过滤,减压浓缩至饱和溶液,再在低温条件下放置析出晶体,随后经过过滤、干燥,即可得到CBD成品。本发明中在使用工业大麻提取CBD时的提取效率较高,同时提取出的CBD纯度较高,适合工厂大规模生产使用。(The invention discloses a process for extracting CBD from industrial hemp by using ethanol, which is realized by the following steps: step 1, cleaning, airing and chopping industrial hemp flowers and leaves; step 2, drying the industrial hemp flowers and leaves; step 3, soaking the dried flower leaves in absolute ethyl alcohol to prepare an extracting solution; step 4, filtering the soaked flower leaves by using a filter screen and heating, wherein the remaining solid or semisolid paste is an extract rich in CBD; step 5, carrying out silica gel column chromatography separation on the CBD extract, eluting the CBD extract by adopting a solvent, collecting CBD components, and concentrating the CBD components under a reduced pressure condition to obtain CBD coarse crystals; and 6, dissolving and filtering the CBD coarse crystal by using a crystallization solvent, concentrating under reduced pressure to obtain a saturated solution, standing at a low temperature to separate out a crystal, and filtering and drying to obtain a CBD finished product. The extraction efficiency is high when the industrial hemp is used for extracting the CBD, and the purity of the extracted CBD is high, so that the method is suitable for large-scale production in factories.)

1. A process for extracting CBD from industrial hemp with ethanol, characterized in that it is carried out by the following steps:

step 1, cleaning and airing picked industrial hemp flowers and leaves, and then carrying out chopping treatment;

step 2, drying the industrial hemp flowers and leaves until the water content is 2-4%;

step 3, soaking the dried flower leaves in absolute ethyl alcohol to prepare an extracting solution;

step 4, filtering out flowers and leaves by using a filter screen after soaking, heating the filtrate at 90-120 ℃, evaporating the solvent in the filtrate after the solvent becomes gas, and obtaining the residual solid or semisolid paste which is the extract rich in the CBD, wherein the content of the CBD is 40-65%;

step 5, filling the prepared CBD extract into a silica gel wet method with the column diameter ratio of 1: 7-10 for silica gel column chromatography separation, eluting the column by using a solvent, collecting CBD components, and concentrating the CBD components under a reduced pressure condition to obtain CBD coarse crystals with the content of the CBD coarse crystals being more than 95%;

and 6, dissolving the prepared CBD coarse crystal by using a crystallization solvent, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, standing the saturated solution at a low temperature to precipitate crystals, and filtering and drying in a low-temperature reduced-pressure environment to obtain a CBD finished product.

2. The process for extracting CBD from industrial hemp by using ethanol as claimed in claim 1, wherein the size of the crushed industrial hemp flower and leaf pieces in step 1 is 3-6 mm.

3. The process for extracting CBD from industrial hemp by using ethanol as claimed in claim 1, wherein the soaking time required in the step 3 is 60-90 minutes, the soaking temperature is less than 50 ℃, and the ethanol concentration is 85-100%.

4. The process for extracting CBD from industrial hemp by using ethanol as claimed in claim 1, wherein the solvent in the step 5 is one of n-hexane, dichloromethane, petroleum ether, ethyl acetate, ethanol, methanol, or a mixture of any several thereof.

5. The process for extracting CBD from industrial hemp using ethanol as claimed in claim 1, wherein the crystallization solvent in the step 6 is n-heptane.

6. The process for extracting CBD from industrial hemp by using ethanol as claimed in claim 1, wherein the CBD content of the CBD finished product obtained in the step 6 is 97-99.9%.

Technical Field

The invention relates to the technical field of extraction and separation of natural phytochemicals, in particular to a process for extracting CBD from industrial hemp by using ethanol.

Background

Industrial hemp refers to a hemp that has been legally planted and contains less than 0.3% Tetrahydrocannabinol (THC). At present, industrial hemp is planted in Yunnan province and Heilongjiang province in large scale, and the planting scale is enlarged year by year. The industrial HEMP (HEMP) has extremely high medicinal value and wide application, and relates to the fields of textile, paper making, food, medicine, sanitation, daily chemicals, leather, automobiles, buildings, decoration, packaging and the like. Is a classic production material and is also one of the traditional raw materials of medicinal materials and health care products in China. The main cannabinol compounds in the hemp plant include Tetrahydrocannabinol (THC), Cannabinol (CBN), Cannabidiol (CBD), Cannabigerol (CBG), cannabichromene (CBC), etc., wherein the former three compounds account for more than 90% of the cannabinol compounds. Cannabidiol, CBD for short, is the main chemical component in medicinal plant cannabis sativa, and modern medical research shows that CBD has significant curative effect in aspects of anti-epilepsy, anti-stress, anti-inflammation and the like, and CBD is approved by the United states food and drug administration, is used for epilepsy treatment, and can also be used as a dietary supplement for improving mood and resisting anxiety.

The existing CBD extraction process has low extraction efficiency when extracting CBD, and the extracted CBD has low purity, thus being not beneficial to large-scale production and use.

An effective solution to the problems in the related art has not been proposed yet.

Disclosure of Invention

The invention aims to provide a process for extracting CBD from industrial hemp by using ethanol, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a process for extracting CBD from industrial hemp with ethanol, which is carried out by the following steps:

step 1, cleaning and airing picked industrial hemp flowers and leaves, and then carrying out chopping treatment;

step 2, drying the industrial hemp flowers and leaves until the water content is 2-4%;

step 3, soaking the dried flower leaves in absolute ethyl alcohol to prepare an extracting solution;

step 4, filtering out flowers and leaves by using a filter screen after soaking, heating the filtrate at 90-120 ℃, evaporating the solvent in the filtrate after the solvent becomes gas, and obtaining the residual solid or semisolid paste which is the extract rich in the CBD, wherein the content of the CBD is 40-65%;

step 5, filling the prepared CBD extract into a silica gel wet method with the column diameter ratio of 1: 7-10 for silica gel column chromatography separation, eluting the column by using a solvent, collecting CBD components, and concentrating the CBD components under a reduced pressure condition to obtain CBD coarse crystals with the content of the CBD coarse crystals being more than 95%;

and 6, dissolving the prepared CBD coarse crystal by using a crystallization solvent, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, standing the saturated solution at a low temperature to precipitate crystals, and filtering and drying in a low-temperature reduced-pressure environment to obtain a CBD finished product.

Further, the size of the industrial hemp flower and leaf fragments subjected to the shredding treatment in the step 1 is 3-6 mm.

Further, the soaking time required in the step 3 is 60-90 minutes, the soaking temperature is less than 50 ℃, and the ethanol concentration is 85-100%.

Further, the solvent in the step 5 is one of n-hexane, dichloromethane, petroleum ether, ethyl acetate, ethanol and methanol, or a mixture of any of the above.

Further, the crystallization solvent in the step 6 is n-heptane.

Further, the content of the CBD finished product in the CBD finished product prepared in the step 6 is 97-99.9%.

Compared with the prior art, the invention has the following beneficial effects: the process for extracting the CBD from the industrial hemp by using the ethanol has the advantages of low investment, high benefit, low pollution, high extraction efficiency and high purity of the extracted CBD, and is suitable for large-scale production and use in factories.

Detailed Description

Technical solutions in embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.

In the description of the present invention, it should be noted that the terms "top", "bottom", "one side", "the other side", "front", "back", "middle", "inside", "top", "bottom", etc. indicate orientations or positional relationships only for the convenience of describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, as they may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

According to the embodiment of the invention, the process for extracting CBD from industrial hemp by using ethanol is realized by the following steps:

step 1, cleaning and airing picked industrial hemp flowers and leaves, and then carrying out chopping treatment;

step 2, drying the industrial hemp flowers and leaves until the water content is 2-4%;

step 3, soaking the dried flower leaves in absolute ethyl alcohol to prepare an extracting solution;

step 4, filtering out flowers and leaves by using a filter screen after soaking, heating the filtrate at 90-120 ℃, evaporating the solvent in the filtrate after the solvent becomes gas, and obtaining the residual solid or semisolid paste which is the extract rich in the CBD, wherein the content of the CBD is 40-65%;

step 5, filling the prepared CBD extract into a silica gel wet method with the column diameter ratio of 1: 7-10 for silica gel column chromatography separation, eluting the column by using a solvent, collecting CBD components, and concentrating the CBD components under a reduced pressure condition to obtain CBD coarse crystals with the content of the CBD coarse crystals being more than 95%;

and 6, dissolving the prepared CBD coarse crystal by using a crystallization solvent, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, standing the saturated solution at a low temperature to precipitate crystals, and filtering and drying in a low-temperature reduced-pressure environment to obtain a CBD finished product.

Wherein the size of the industrial hemp flower and leaf fragments subjected to the shredding treatment in the step 1 is 3-6 mm.

Wherein the soaking time required in the step 3 is 60-90 minutes, the soaking temperature is less than 50 ℃, and the ethanol concentration is 85-100%.

Wherein, the solvent in the step 5 adopts one of n-hexane, dichloromethane, petroleum ether, ethyl acetate, ethanol and methanol, or a mixture of any of the above.

Wherein the crystallization solvent in the step 6 is n-heptane.

Wherein the content of the CBD finished product in the CBD finished product prepared in the step 6 is 97-99.9%,

in summary, the following steps: the process for extracting the CBD from the industrial hemp by using the ethanol has the advantages of low investment, high benefit, low pollution, high extraction efficiency and high purity of the extracted CBD, and is suitable for large-scale production and use in factories.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.