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A kind of method of dienolone acetate waste acid water recycling

A technology of dienolone acetate and diene waste acid water, which is applied in chemical instruments and methods, carboxylate preparation, chromium oxide/hydrate, etc., and can solve problems such as increased processing costs, waste of resources, and environmental pollution , to achieve the effect of simple method and convenient operation

Active Publication Date: 2016-08-24
湖北竹溪人福药业有限责任公司
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  • 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 CN 103274923 B is a method for recycling dienolone acetate waste liquid. Although sodium acetate is produced, the solvent ethanol is used for alcohol analysis, which increases the processing cost, and the method does not use the low concentration of the previous batch. The acid water 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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  • A kind of method of dienolone acetate waste acid water recycling

Examples

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Effect test

example 1

[0025] 1) Take 100g of saponin through ring opening, oxidative hydrolysis to synthesize dienolone acetate, after extraction with 2L of cyclohexane, wash the cyclohexane layer three times with 2L of drinking water until it is neutral, and collect three times respectively The separated acid water layer.

[0026] 2) Add 125g of sodium carbonate to the first high-concentration waste acid water to adjust the pH=8, add 2.5g of hydrazine hydrate, stir for 1h, filter to obtain Cr(OH)3, content: 98.1%; the filtrate is concentrated until it is concentrated When the filtrate is 2 / 5, the temperature is lowered to 10℃ to crystallize for 4h, and the sodium acetate trihydrate is obtained by filtration, content: 60%; the concentrated 1L wastewater and 1L fresh drinking water total 2L for the third production of the next batch Washed.

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

example 2

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

[0030] 2) Perform the first washing with the 2L filtrate of the second washing from the previous batch. 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 Hydrazine hydrate, stirred for 1h, filtered to obtain Cr(OH)3, content: 98%. The filtrate was concentrated until 3 / 5 of the filtrate was concentrated, and the temperature was lowered to 15°C to crystallize for 6 hours, and sodium acetate trihydrate was obtained by filtration, content: 61%. A total of 2L of concentrated wastewater and 1L of fresh drinking water are used for the third washing of the next batch of production.

[0031] 3). Add 10g of sodium carbonate to the second and third was...

example 3

[0033] 1) Take 100g of saponin through ring opening, oxidative hydrolysis to synthesize dienolone acetate, after extraction with 2L of cyclohexane, wash with the previous batch of waste acid water to neutrality.

[0034] 2) Perform the first washing with the 2L filtrate of the second washing from the previous batch. After washing and stratification, high-concentration waste acid water is obtained. Add 125g sodium carbonate to the high-concentration waste acid water to adjust pH=8, and add 2.5g Hydrazine hydrate, stirred for 1h, filtered to obtain Cr(OH)3, content: 98.3%. The filtrate was concentrated until 2 / 5 of the filtrate was concentrated, and the temperature was lowered to 10°C for 4 hours to crystallize, and then filtered to obtain sodium acetate trihydrate, content: 60%. The concentrated wastewater is used for the third washing of 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 hydrazin...

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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 method for recycling waste water, in particular to a method for recycling waste acid water of dienol ketone acetate. Background technique [0002] Diene, English name: 16-pregnadien-20-one acetate, chemical name: 3β-hydroxy-pregnadien-5,16-diene-20-one-3-acetate, molecular formula is C23H32O3. Diene is an important starting material for the production of steroid hormones, and can be used to synthesize adrenal hormones, steroidal anti-inflammatory drugs, glucocorticoids, sex hormones and other drugs. Domestic manufacturers generally use diosgenin as raw materials to synthesize diene through ring-opening acylation and oxidative hydrolysis. For every ton of diene produced, 20 tons of waste acid water will be produced, causing a major waste of water resources and pollution. surroundings. The process of washing the diene with cyclohexane to neutrality will produce a large amount of chromium-containing waste acid water. The traditiona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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