Method for producing dehydroepiandros-sterone

A technology of dehydroepiandrosterone and production steps, which is applied in the field of production of dehydroepiandrosterone, can solve the problems of long production cycle, polluted environment by waste liquid, and high cost of dehydroepiandrosterone, and achieves the effect of reducing the usage amount

Inactive Publication Date: 2010-06-02
湖北省丹江口开泰激素有限责任公司
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Problems solved by technology

[0003] In order to solve the problems of high cost of dehydroepiandrosterone, long production cycle and environmental pollution by waste liquid, the present invention proposes a method for producing dehydroepiandrosterone

Method used

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  • Method for producing dehydroepiandros-sterone
  • Method for producing dehydroepiandros-sterone

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Embodiment Construction

[0017] like figure 1 as shown,

[0018] First, in the reaction tank, 120kg of ketoximes obtained by the oximation reaction of dienes, dried with a water content of ≤0.5%, were added to 780kg of benzene dehydrated by edible salt, and heated and dissolved. After the ketoximes were completely dissolved, the temperature was lowered to 38 ℃±2℃, then add 57.6kg of pyridine, the content of pyridine is ≥98%, and the water content is less than 0.2%;

[0019] Next, in the jacket of the reaction tank, pass salt water to lower the temperature by 5-8°C, add dropwise a mixed solution of 58kg phosphorus oxychloride and 98kg benzene, the content of phosphorus oxychloride is ≥ 98%, and the dropwise temperature is controlled within 15°C. After adding the mixed solution of phosphorus oxychloride and benzene dropwise, keep the reaction at 16°C-18°C;

[0020] Next, quickly add 227kg of dilute hydrogen chloride acid water to the solution after reacting for 3 hours, the content of hydrogen chlorid...

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Abstract

The invention provides a method for producing dehydroepiandros-sterone, comprising the following steps of: drying ketoxime substance obtained after the oximation reaction of diene till water content is not more than 0.5 percent; adding into benzene dehydrated with edible salt for raising the temperature and dissolving; after complete dissolving, reducing the temperature by 38+ / -2 DEG C and adding pyridine; reducing the temperature by 5-8 DEG C with saline water; dropwise adding mixed solution of phosphorus oxychloride and benzene and controlling the temperature within 15 DEG C during dropping; keeping the temperature of the mixed solution within 16-18 DEG C for three hours; rapidly adding dilute acid liquid and then raising the temperature to 58+ / -1 DEG C; keeping the temperature and reacting for 2 hours within 58+ / -1 DEG C; and feeding wastewater into a storage tank, washing three times till the wastewater is neutral, filtering materials, adding water, steaming and distilling for hydrolysis reaction. The invention effectively reduces the consumption of phosphorus oxychloride and hydrochloric acid, simultaneously recovers the wastewater, carries out displacement reaction by using caustic soda to displace pyridinium in the wastewater into pyridine, purifies and recycles the pyridine, greatly reduces the cost of products while ensuring the quality of the product and improves the market competitiveness.

Description

technical field [0001] The invention relates to a method for producing dehydroepiandrosterone. Background technique [0002] DHEA is a steroid hormone API, widely used. At present, the process ratio of DHEA production is ketoxime: benzene: phosphorus oxychloride: pyridine: hydrochloric acid = 1: 6.5: 0.88: 0.48: 1.8, and the process method of acid hydrolysis in the hydrolysis process is to control the temperature within 12°C Slowly add dropwise, it takes a long time, and the waste liquid generated is drained. Among the above production processes, the ratio of chemical raw materials such as phosphorus oxychloride with high market price is high, the waste liquid containing pyridinium salt is not recycled, the production cycle is long, the waste liquid is acidic and discharged into the environment, and the treatment cost is high, resulting in The production cost of DHEA products is relatively high, and the market competitiveness is not high. Contents of the invention [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J1/00C07D213/16
Inventor 闻开学曹雪山李勇
Owner 湖北省丹江口开泰激素有限责任公司
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