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Method for extracting and separating 24-dehydrocholesterol and cholesterol by ionic liquid

A dehydrocholesterol and ionic liquid technology, applied in the production of steroids, bulk chemicals, organic chemistry, etc., can solve problems such as low separation selectivity and extraction capacity, environmental pollution caused by volatile organic solvents, and environmental pollution , to achieve the effect of reducing the theoretical plate number of fractionation and solvent consumption, reducing equipment investment and production cycle, and reducing pollution

Active Publication Date: 2014-08-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A kind of AgNO is disclosed in US patent US3803184 3 Complexation chromatography, this method has good selectivity, but the production cost is relatively large, the process is cumbersome, and the production cycle is long
A synthetic conversion method is disclosed in U.S. Patent US3846455. This method has a high yield, but the production cycle is long, and more acid-base solvents are used, which is easy to pollute the environment.
In addition, there is a method for separating 24-dehydrocholesterol and cholesterol disclosed in Chinese patent CN101270141A, which is mainly an organic solvent fractionation extraction method. into a raw material liquid, the raw material liquid is fractionated and extracted, the extract is collected and concentrated to obtain 24-dehydrocholesterol, and the extraction residue is collected and concentrated to obtain cholesterol; the extractant of the fractional distillation and extraction is one of methanol, octanol, sulfolane or Its mixture; the solvent is the same as the detergent extracted by fractional distillation, which is one of petroleum ether, hexane, and octane; this method has fast phase separation speed, simple process, stable operation, low cost, large production capacity, and high product quality , low energy consumption, but this method uses volatile organic solvents as the extraction agent, there is a problem of volatile organic solvents polluting the environment, and the separation selectivity and extraction capacity are not high at the same time
[0005] It can be seen that there is still a lot of room for improvement in the existing methods for separating 24-dehydrocholesterol and cholesterol.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The mixture of raw material 24-dehydrocholesterol and cholesterol (24-dehydrocholesterol / cholesterol = 13.64%, mass ratio) is dissolved in petroleum ether with a boiling range of 60-90°C to prepare the total concentration of 24-dehydrocholesterol and cholesterol It is 0.9 g / L raw material solution. Using 1-butylcyano-3-methylimidazole-tetrafluoroborate ionic liquid as extractant, petroleum ether with a boiling range of 60-90°C as detergent, extraction agent, detergent and raw material solution The flow ratio is 6:4.5:1.5 (that is, 4:3:1), and the fractional extraction is carried out at 50°C. There are 3 stages in the extraction section and 6 stages in the washing section, and the extract and raffinate are collected.

[0036] The raffinate was concentrated in vacuo, washed with water and dried to obtain cholesterol; the extract was back-extracted with n-hexane, and the extracted phase of n-hexane was concentrated in vacuo, washed with water and dried to obtain 24-dehydro...

Embodiment 2

[0038] The mixture of raw materials 24-dehydrocholesterol and cholesterol (24-dehydrocholesterol / cholesterol=13.64%, mass ratio) is dissolved in n-hexane to prepare a raw material solution with a total concentration of 24-dehydrocholesterol and cholesterol of 1.8 g / L . 1-sulfonepropyl-quinoline-bistrifluoromethanesulfonimide salt ionic liquid is used as the extractant, n-hexane is used as the detergent, and the flow ratio of the extractant, detergent, and raw material solution is 4:3: 1. Fractional extraction is carried out at 60°C. There are 2 stages in the extraction section and 6 stages in the washing section, and the extract and raffinate are collected.

[0039] The raffinate was concentrated in vacuo, washed with water and dried to obtain cholesterol; the extract was back-extracted with n-hexane, and the extracted phase of n-hexane was concentrated in vacuo, washed with water and dried to obtain 24-dehydrocholesterol. Among them, the purity of 24-dehydrocholesterol was 9...

Embodiment 3

[0041] The mixture of raw material 24-dehydrocholesterol and cholesterol (24-dehydrocholesterol / cholesterol = 11.26%, mass ratio) is dissolved in octane to prepare a raw material solution with a total concentration of 24-dehydrocholesterol and cholesterol of 0.5 g / L . The benzimidazole-tetracyanoboric acid ionic liquid-methanol binary mixed solvent is used as the extractant (the molar fraction of benzimidazole-tetracyanoboric acid in the mixed solvent is 90%), and octane is used as the detergent. The extractant, detergent, The flow ratio of the three raw materials is 2:1:1, and the fractional extraction is carried out at 40°C. There are 3 stages in the extraction section and 7 stages in the washing section, and the extract and raffinate are collected.

[0042] The raffinate was concentrated in vacuo, washed with water and dried to obtain cholesterol; the extract was back-extracted with n-hexane, and the extracted phase of n-hexane was concentrated in vacuo, washed with water a...

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Abstract

The invention discloses a method for extracting and separating 24-dehydrocholesterol and cholesterol by ionic liquid. According to the invention, ionic liquid or binary mixed solvent made of ionic liquid and polar solvent is used as extractant; extract and raffinate are obtained through fractional extraction; and high-purity 24-dehydrocholesterol and cholesterol can be obtained from the extract and the raffinate respectively. The ionic liquid extractant adopted by the method has better thermal stability, noninflammability and higher selectivity than traditional organic solvent, and has the characteristics of simple and safe technology, environmental friendliness and the like, so that the ionic liquid extractant is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating 24-dehydrocholesterol and cholesterol, belongs to the technical field of chemical separation, and in particular relates to a method for extracting and separating 24-dehydrocholesterol and cholesterol by using ionic liquid. Background technique [0002] Cholesterol, also known as cholesterol, is a derivative of cyclopentane polyhydrophenanthrene. Cholesterol is widely present in animals, especially in brain and nerve tissue, and is also high in kidney, spleen, skin, liver and bile. Cholesterol is an indispensable and important substance in animal tissue cells. It not only participates in the formation of cell membranes, but also is a raw material for the synthesis of bile acids, vitamin D and steroid hormones. 24-Dehydrocholesterol (Desmosterol) is a sterol substance extracted from mixed phytosterols, animal serum, liver and some other animal tissues, and is the direct precursor of cholesterol biosynthes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
CPCY02P20/54
Inventor 邢华斌刘献献杨启炜苏宝根鲍宗必杨亦文任其龙苏云梁瑞斯
Owner ZHEJIANG UNIV
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