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Method for treating spirolactone intermediate production wastewater

A technology for the production of waste water and intermediates, which is applied in the fields of filtration treatment, chemical instruments and methods, multi-stage water/sewage treatment, etc., can solve the problems of difficult waste water treatment and long time, and achieve environmental friendly treatment process, improve efficiency, The effect of high yield

Active Publication Date: 2021-10-29
佳尔科生物科技南通有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of method for processing spironolactone intermediate production waste water, to solve the present stage spironolactone intermediate waste water treatment difficulty that proposes in the above-mentioned background technology, the problem of long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 2500kg of waste water from the synthesis of 17b, 20b-epoxy-3-ethoxy-17a-pregna-3,5-diene into the reactor, and add 40% HBr aqueous solution to the reactor dropwise. And react until pH=7, at this time, 126kg of HBr aqueous solution will be consumed, and then 1326kg of water will be distilled under the condition of pressure of -0.095Mpa and temperature controlled at 70°C. At this time, 1326kg of water can be directly recycled as process water, and then The feed liquid flowing out without water was cooled to 30°C, then 1950kg of dichloromethane was added, continued to cool to -15°C, and after heat preservation and crystallization for 5 hours, pressure filtration was carried out to form a filtrate, and then washed with 130kg of dichloromethane to produce a washing liquid. At the same time, 400kg of solids will be generated after washing, and the generated solids will be vacuum-dried at 40°C for 4 hours to obtain 340kg of sodium bromide (after analysis, the content is 98....

Embodiment 2

[0020] 2500kg of synthetic 17b, 20b-epoxy-3-ethoxyl-17a-pregna-3,5-diene waste water is added to the reactor, and 40% aqueous HBr solution is added dropwise in the reactor to carry out Neutralization reaction until pH = 7, at this time, 126kg of HBr aqueous solution will be consumed, and then 1350kg of water will be distilled under the conditions of pressure -0.095Mpa and temperature control at 50°C. At this time, 1350kg of water can be directly recycled as process water, and then Cool the anhydrous feed liquid to 30°C, then add 2552kg of chloroform, continue to cool to -15°C, carry out heat preservation and crystallization for 5 hours, then carry out pressure filtration to form a filtrate, and then wash with 130kg of chloroform to produce a washing liquid, and at the same time after washing 410kg of solids will also be generated, and the generated solids will be vacuum-dried at 40°C for 4 hours to obtain 350kg of sodium bromide (after analysis, the content is 98.7%, meeting th...

Embodiment 3

[0022] Add 2500kg of waste water from the synthesis of 17b, 20b-epoxy-3-ethoxy-17a-pregna-3,5-diene into the reactor, and add 40% HBr aqueous solution to the reactor dropwise. And react until pH=7, at this time, 126kg of HBr aqueous solution will be consumed, and then 1326kg of water will be distilled under the condition of pressure of -0.095Mpa and temperature controlled at 60°C. At this time, 1326kg of water can be directly recycled as process water, and then Cool the feed liquid flowing out without water to 30°C, then add 1300kg chloroform, continue to cool to -15°C, carry out heat preservation and crystallization for 5 hours, then carry out pressure filtration to form a filtrate, and then wash with 130kg chloroform to produce a washing liquid, and also after washing 380kg of solids will be generated, and the generated solids will be vacuum-dried at 40°C for 4 hours to obtain 330kg of sodium bromide (after analysis, the content is 98.3%, which meets the requirements of indus...

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PUM

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Abstract

The invention discloses a method for treating spirolactone intermediate production wastewater, which is characterized by comprising the following four steps: 1) performing neutralization reaction; 2) separating filtrate, solid and washing liquid through pressure reduction, cooling, solvent addition, cooling, filter pressing and washing; 3) performing vacuum drying on the solid to obtain sodium bromide; and 4) merging the filtrate and the washing liquid, recovering the solvent, directly applying the solvent, and evaporating out dimethyl sulfoxide from the residual liquid. According to the method, the HBr aqueous solution is adopted to carry out neutralization reaction on the wastewater generated by the spirolactone intermediate, then the filtrate, the solid and the washing solution are separated through pressure reduction, cooling, solvent adding, cooling, filter pressing and washing, and the solvent is recycled by utilizing pressure, so that the solvent can be turned into wealth, the wastewater treatment difficulty is reduced, the wastewater treatment time is shortened, and the wastewater treatment efficiency is improved; meanwhile, environmental pollution is avoided, and the pressure of environmental protection treatment is relieved.

Description

technical field [0001] The invention belongs to the technical field of wastewater recovery and treatment, and relates to a method for treating wastewater produced by spironolactone intermediates. Background technique [0002] Spironolactone (spironolactone, 1), the chemical name is (7 0c, 170c)-7. (acetylthio)-17. Hydroxy-3. Oxygen surrogate steroid. 4-ene-21. Carboxylate 1L Lactone, a mineralocorticoid antagonist developed by Pfizer, has been marketed in many countries and is clinically used as a diuretic. However, 17b, 20b-epoxy-3-ethoxy-17a-pregna-3,5-diene is an important intermediate for the synthesis of spironolactone, and its main preparation method is to use 4-AD as raw material, using triethyl orthoformate After the ester protects the 3-position carbonyl group, dimethyl sulfoxide is used as a solvent, under the catalysis of sodium ethoxide, and trimethyl sulfide bromide are epoxidized, after the reaction is completed, the ethanol is evaporated under reduced pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10
CPCC02F9/00C02F1/001C02F1/04C02F1/66
Inventor 王彩霞周革
Owner 佳尔科生物科技南通有限公司
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