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Method of recycling acid wastewater generated during production of dehydropregnenolone acetate

A technology of dienolone acetate and diene waste acid water, which can be applied in chemical instruments and methods, carboxylate preparation, chromium oxide/hydrate and other directions, and can solve the waste of resources, increase the treatment cost, waste of water resources, etc. problem, to achieve the effect of convenient operation and simple method

Active Publication Date: 2015-11-18
湖北竹溪人福药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic manufacturers generally use diosgenin as raw material to synthesize dienes through ring-opening acylation and oxidative hydrolysis. For every 1 ton of dienes produced, 20 tons of waste acid water will be produced, causing a major waste of water resources and polluting surroundings
The water washing to neutral link of cyclohexane extraction of diene will produce a large amount of chromium-containing waste acid water. The traditional process collects the high-concentration acid water produced by the first washing of the cyclohexane layer, and the second and third low Concentrated chromium-containing waste acid water is discharged into sewage. Even if it reaches the standard after treatment, it still contains heavy metal chromium, which pollutes the environment and wastes water resources.
[0003] Patent No. 200910063423.7, a method for preparing chromium oxide green by using chromium slag after dienolone production discloses that chromium oxide green is prepared by using diene waste liquid, but sodium acetate is not separated from the waste liquid; resulting in waste of resources , increasing the difficulty of subsequent use of wastewater
[0004] Patent CN103274923B is a method for recycling dienolone acetate waste liquid. Although sodium acetate is produced, solvent ethanol is used for alcohol analysis, which increases the processing cost, and the method does not use the low-concentration acid water from the previous batch. It is used for the next batch of water-washed cyclohexane layer, so the waste acid water in the system is not fully utilized
[0005] There is no report on the literature on the recycling of dienolone acetate waste acid water

Method used

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  • Method of recycling acid wastewater generated during production of dehydropregnenolone acetate

Examples

Experimental program
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Effect test

example 1

[0025] 1) Take 100g of saponin through ring-opening, oxidative hydrolysis to synthesize dienolone acetate, extract with 2L of cyclohexane, wash the cyclohexane layer with 2L of drinking water three times until neutral, and collect three times respectively The acidic aqueous layer was separated.

[0026] 2) Add 125g of sodium carbonate to the first high-concentration waste acid water to adjust pH=8, add 2.5g of water and hydrazine, stir for 1 hour, filter to obtain Cr(OH)3, content: 98.1%; concentrate the filtrate until When 2 / 5 of the filtrate is concentrated, cool down to 10°C and crystallize for 4 hours, and filter to obtain sodium acetate trihydrate, content: 60%; 1L of concentrated waste water and 1L of fresh drinking water will be used for the third batch of the next batch of production. wash.

[0027] 3) Add 4g of sodium carbonate to the second and third waste acid water to adjust pH=8, add 1g of water and hydrazine, stir for 1 hour, filter to obtain Cr(OH)3, content: 9...

example 2

[0029] 1) Take 100g of saponin through ring-opening, oxidative hydrolysis to synthesize dienolone acetate, extract with 2L of cyclohexane, and wash with the waste acid water from the previous batch until neutral.

[0030] 2) Use the 2L filtrate from the second water wash of the previous batch for the first wash. After washing and stratification, high-concentration waste acid water is obtained. Add 200g of sodium carbonate to the high-concentration waste acid water to adjust pH = 9, and add 3.75g Water and hydrazine, stirred for 1 hour, filtered to obtain Cr(OH)3, content: 98%; the filtrate was concentrated until 3 / 5 of the filtrate was concentrated, cooled to 15°C for crystallization for 6 hours, filtered to obtain sodium acetate trihydrate, content: 61%, a total of 2L of concentrated wastewater and 1L of fresh drinking water are used for the third washing in the next batch of production.

[0031] 3) Add 10g of sodium carbonate to the second and third waste acid water to adjus...

example 3

[0033] 1) Take 100g of saponin through ring-opening, oxidative hydrolysis to synthesize dienolone acetate, extract with 2L of cyclohexane, and wash with the waste acid water from the previous batch until neutral.

[0034] 2) Use 2L of the filtrate from the second water wash of the previous batch for the first wash, and after washing and stratification to obtain high-concentration waste acid water, add 125g of sodium carbonate to the high-concentration waste acid water to adjust pH = 8, and add 2.5g Water and hydrazine, stirred for 1 hour, filtered to obtain Cr(OH)3, content: 98.3%; the filtrate was concentrated until 2 / 5 of the filtrate was concentrated, cooled to 10°C for crystallization for 4 hours, filtered to obtain sodium acetate trihydrate, content: 60%; the concentrated wastewater is used for the third washing in the next batch of production.

[0035] 3) Add 4g of sodium carbonate to the second and third waste acid water to adjust pH=8, add 1g of water and hydrazine, st...

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Abstract

The invention relates to a method of recycling acid wastewater generated during the production of dehydropregnenolone acetate. The method starts with the diene production process and recycles the acid wastewater which can be recycled and reused in all the processes. The obtained by-product contains high-purity chromic hydroxide and sodium acetate, both of which can be sold. Compared with the conventional acid wastewater treatment method, the method provided by the invention is simple and easy to operate and low in energy consumption, improves the utilization rate of the acid wastewater, reduces the production water using amount, lowers the cost and burden of the wastewater treatment, and reduces the pollution caused by the acid wastewater to the environment.

Description

technical field [0001] The invention relates to a recycling method of waste water, in particular to a recycling method of dienolone acetate waste acid water. Background technique [0002] Diene, English name: 16-pregnadien-20-oneacetate, chemical name: 3β-hydroxy-pregnadien-5,16-diene-20-one-3-acetate, molecular formula C23H32O3. Diene is an important starting material for the production of steroid hormone drugs, and can be used to synthesize adrenal hormone drugs, steroidal anti-inflammatory drugs, glucocorticoid drugs, sex hormone drugs and other drugs. Domestic manufacturers generally use diosgenin as raw material to synthesize dienes through ring-opening acylation and oxidative hydrolysis. For every 1 ton of dienes produced, 20 tons of waste acid water will be produced, causing a major waste of water resources and polluting environment. The water washing to neutral link of cyclohexane extraction of diene will produce a large amount of chromium-containing waste acid wat...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41C01G37/033C02F9/04
CPCC01G37/033C02F1/001C02F1/66C02F9/00C07C51/41C07C53/10
Inventor 周建生郑承刚杨艳青郑建雄张阳洋龚青侯海波
Owner 湖北竹溪人福药业有限责任公司
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