Method for producing oxygen bridge material

A production method and oxygen bridge technology, applied in the direction of steroids, organic chemistry, etc., can solve the problems of easy explosion and low product quality, and achieve the effects of improving safety, increasing efficiency, saving costs and man-hours

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

Since the solvent used in the production process of oxygen bridges is methanol, oxygen and by-product sodium peroxide are generated during the epoxy reaction process, which is prone to the danger of explosion; currently, nitrogen protection is commonly used in the production process, and the produced oxygen bridges are highly efficient. Liquid phase analysis shows that the content of oxygen bridges is about 95%, and the melting point is ≤184°C. The quality of the product in the process is not high, which has a great impact on the subsequent reaction - the Woshi oxidation reaction, which has become a constraint to improve the yield and quality of Woshi oxide. One of the key processes to reduce production costs

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  • Method for producing oxygen bridge material
  • Method for producing oxygen bridge material

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Embodiment Construction

[0016] Such as figure 1 shown.

[0017] First, 1000L industrial methanol is pumped into the reaction tank, the content of methanol is ≥98%, and then 100kg of dienolketone with a content of ≥98.5% is put into the methanol solution, and the dienolketone is stirred and heated in the methanol solution to Dienolone is completely dissolved at 55±2°C, then the solution is cooled to 26°C±2°C, and an industrial sodium hydroxide aqueous solution is prepared during the cooling process, wherein the sodium hydroxide aqueous solution is 30kg of water and 15kg of solid sodium hydroxide Prepared, the content of sodium hydroxide is ≥ 95%, and 500g of industrial sodium silicate complexing agent with a content of ≥ 98% is added to the above alkaline water solution;

[0018] Next, add 21kg of hydrogen peroxide dropwise in the above solution in 30-35 minutes, after stirring for 10 minutes, then add 11.3kg of alkaline water dropwise in 30-35 minutes, the dropping rate is 0.38L / min, wherein alkalin...

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Abstract

The invention provides a method for producing oxygen bridge material, which comprises the following steps of pumping methanol in a retort, adding dehydropregnenolone, stirring and heating to completely dissolve the materials, and preparing and adding aqueous sodium hydroxide solution into a sodium silicate complexing agent during lowering temperature; 30-35 min later, dropwise adding hydrogen peroxide and stirring; 30-35 min later, dropwise adding water containing soda and controlling temperature and reacting for 30 min; about 60 min later, dropwise adding hydrogen peroxide and reacting for 30 min; 60-90 min later, dropwise adding water containing soda and controlling the temperature to be 28-30 DEG C during dropwise adding; raising the temperature to be 36-40 DEG C naturally after the dropwise adding, and reacting for 6 hours within the temperature range of 36-40 DEG C; and confirming the material is qualified if the content of hydrogen peroxide is detected to be within the range of 0.5-0.8 percent after the reaction. The temperature can be controlled during the processing of dropwise adding just by using an explosion-proof mat and a headspace exhaust plant without the need of the protection of nitrogen, thereby achieving safer reaction.

Description

technical field [0001] The invention relates to a production method of an oxygen bridge. Background technique [0002] The oxygen bridge is a steroid hormone intermediate obtained by hydrolysis of dienol ketone at the 3-position, and two-step chemical reactions of the 16 and 17-position epoxy. It is an important process raw material for the production of Woshi oxide, and Woshi oxide It is an important and irreplaceable main raw material for the production of dexamethasone. Since the solvent used in the production process of oxygen bridges is methanol, oxygen and by-product sodium peroxide are produced during the epoxy reaction process, which is prone to the danger of explosion; currently, nitrogen protection is commonly used in the production process, and the produced oxygen bridges are highly efficient. Liquid phase analysis shows that the content of oxygen bridges is about 95%, and the melting point is ≤184°C. The quality of the product in the process is not high, which h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J21/00
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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