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A method for separating cholesterol and 24-dehydrocholesterol by complex crystallization

A technology for separation of dehydrocholesterol and crystallization, which is applied in the fields of steroids and organic chemistry, can solve the problems of long production cycle, cumbersome process, low selectivity and extraction capacity, and achieve low production equipment requirements, simple operation process, good separation selectivity

Active Publication Date: 2022-06-14
浙江花园营养科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product purity and yield obtained by column chromatography are not high, and the separation efficiency is low; AgNO 3 Although chromatography has better selectivity, the production cost is high, the process is cumbersome, and the production cycle is long; the synthetic conversion 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; fractional distillation extraction The amount of volatile organic solvent used in the method is large, and the selectivity and extraction capacity are not high; and for the ionic liquid extraction method, the high cost of the ionic liquid is still a major obstacle hindering its industrialization

Method used

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  • A method for separating cholesterol and 24-dehydrocholesterol by complex crystallization
  • A method for separating cholesterol and 24-dehydrocholesterol by complex crystallization

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Experimental program
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Effect test

Embodiment 1

[0037] 1) Complex crystallization: cholesterol and 24-dehydrogen cholesterol mixed raw materials (cholesterol: 24-dehydrogen cholesterol = 8: 9), methanol, CuCl, concentrated hydrochloric acid (36%) according to the mass ratio of 1: 17: 0.5: 1.6 prepared as a mixed solution, with nitrogen to replace the air in the reactor after stirring at 30 °C protected from light for 1h. After the end of the reaction, the cooling crystallization is carried out, the cooling speed is 5 °C / h, the crystallization temperature is -10 °C, and the crystallization time is 5h.

[0038] 2) Filtration washing: the reaction liquid is filtered to obtain the filtrate and the filter cake, and the filter cake is washed and filtered 3 times using -10 °C methanol, and the methanol quality used for each wash is 2 times the quality of the filter cake.

[0039] 3) Filter cake decombination: Remove the filter cake from step 2) and dissolve it at 30 °C with methanol 17 times the mass of the filter cake. The complexing...

Embodiment 2

[0044] The experimental apparatus and the operating process are the same as Example 1, only step 1), the complexing agent CuCl is replaced by copper tetrafluoroborate, and the analysis results are shown in Table 1.

Embodiment 3

[0046] The experimental apparatus and the operating process are the same as Example 1, only step 1), the solvent methanol is replaced by isopropanol, the mass ratio of raw materials to solvents is changed to 1:11, the crystallization temperature is -20 ° C, and the crystallization time is 10h; Step 2) in which the detergent is replaced by isopropanol at -20 °C; Step 3) In step 3), the solvent is replaced with isopropanol 11 times the mass of the filter cake, and the analysis results are shown in Table 1.

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Abstract

The invention discloses a method for separating cholesterol and 24-dehydrocholesterol by complex crystallization. First, soluble cuprous salt is used as a complexing agent to obtain high-purity cholesterol through complex crystallization, and then cholesterol and 24-dehydrocholesterol in the mother liquor are separated by toluene. The dehydrocholesterol was extracted, and the mixture obtained after evaporating to dryness was dissolved in acetic acid for recrystallization to obtain high-purity 24-dehydrocholesterol. Simultaneously, after the mother liquor of acetic acid is evaporated, its dried matter can be used as raw material continuously, thereby improving the whole process yield. The present invention can be separated by using a crystallization reactor commonly used in the field, has low requirements on equipment, and the complexing agent used can greatly improve the separation efficiency, and has the characteristics of simple operation, less solvent consumption, and environmental protection.

Description

Technical field [0001] The present invention belongs to the field of chemical separation technology, specifically relates to a method of separating cholesterol and 24- dehydrogen cholesterol by complex crystallization method. Background [0002] Cholesterol is an indispensable and important substance in animal tissue cells, which is not only involved in the formation process of cell membranes, but also the raw material for the synthesis of bile acids, vitamin D and steroid hormones, and is widely used in medicine, food, feed, cosmetics and other fields. At present, the production process of cholesterol is mainly to extract free cholesterol from the lanolin derivative lanool, but the product is often mixed with a large amount of 24-dehydrocholesterol. At the same time, 24-dehydrocholesterol is also an important life active substance, which is a direct precursor to cholesterol synthesis, has some physiological role of cholesterol, and also plays an important role in mammalian sexua...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 郭阳单伟达刘建刚钱国平邵振宝王丽虹
Owner 浙江花园营养科技有限公司
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