Method for recycling dehydropregnenolone acetate waste liquor

A technology of dienolone acetate and waste liquid, which is applied in the direction of carboxylate preparation, chromium trioxide, chromium oxide/hydrate, etc., can solve the problems of waste of resources, increase the difficulty of subsequent use of wastewater, and achieve water conservation , Significant economic benefits, easy operation

Inactive Publication Date: 2015-01-07
CHINA THREE GORGES UNIV +1
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  • Description
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Problems solved by technology

[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 this waste liquid, but sodium acetate is not separated from the waste liquid; resulting in waste of resources , which increases the difficulty of subsequent use of wastewater, and there is no report on the separation of sodium acetate from dienolone acetate production waste liquid

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  • Method for recycling dehydropregnenolone acetate waste liquor

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example 1

[0026] Take 50g of dienolone acetate production waste liquid, adjust the pH to 8 with 20% NaOH solution under stirring, produce a large amount of precipitation, add 0.2g of activated carbon, boil for 10 minutes, filter while hot, wash four times with 20mL boiling water each time , Obtain filter residue A and filtrate A. Filtrate A was concentrated to 50mL under reduced pressure, and the evaporated hot water could be recycled, then 50mL of ethanol was added, crystallized by cooling, filtered, and washed twice with 30mL of ethanol each time to obtain filter residue B and filtrate B. Filter residue B was dried to obtain 54.1 g of white sodium acetate trihydrate crystals, and its content and other indicators were determined by the national standard GB / T 693-1996 method, and the results met the chemical purity grade standard.

[0027] Filter residue A was calcined to obtain 11.9 g of powdered chromium oxide green.

[0028] Filtrate B recovered ethanol and added 18.0g NaOH to the r...

example 2

[0030] Take 100g of dienolone acetate production waste liquid, adjust the pH to 7 with 30% NaOH solution under stirring, a large amount of precipitation occurs, add 0.5g of activated carbon, boil for 5 minutes, filter while hot, and wash four times with 30mL boiling water each time , Obtain filter residue A and filtrate A. Filtrate A was concentrated to 80mL under reduced pressure, and the evaporated hot water could be recycled. Add 70mL of methanol, cool and crystallize, filter, and wash twice with 40mL of methanol each time to obtain filter residue B and filtrate B. The filter residue B was dried to obtain 108.3 g of white sodium acetate trihydrate crystals, and its content and other indicators were determined by the national standard GB / T 693-1996 method, and the results met the chemical purity grade standard.

[0031] Filter residue A was calcined to obtain 23.8 g of powdered chromium oxide green.

[0032] Add 36.0g NaOH to the residual liquid after recovering methanol fr...

example 3

[0034] Take 10kg of dienolone acetate production waste liquid, adjust pH=7.5 with 40% NaOH solution under stirring, produce a large amount of precipitation, add 0.05kg of activated carbon, boil for 8 minutes, filter while hot, wash four times with 3kg of boiling water each time , Obtain filter residue A and filtrate A. Filtrate A was concentrated to about 8L under reduced pressure, and the evaporated hot water could be recycled. Add 7L of ethyl acetate, cool and crystallize, filter, and wash twice with 3L of ethyl acetate each time to obtain filter residue B and filtrate B. The filter residue B was dried to obtain 10.84 kg of white sodium acetate trihydrate crystals, and its content and other indicators were determined by the national standard GB / T 693-1996 method, and the results met the chemical purity grade standard.

[0035] Filter residue A was calcined to obtain 2.39kg of powdered chromium oxide green.

[0036] After recovering ethyl acetate from filtrate B, add 3.6kg N...

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Abstract

The invention provides a method for recycling dehydropregnenolone acetate waste liquor. The method comprises the following steps of: separating and recycling sodium acetate from the treated waste liquor through NaOH sedimentation, decoloration, filtration, solvent washing, concentration, crystallization, drying and the like, and completely recovering sodium acetate by utilizing the hot water generated by concentration and the mother liquor generated by crystallization. Product inspection proves that the content of the active ingredient in a product is more than 98.5%, various indexes meet chemical purity grades specified by national standard GB / T693-1996, and therefore the product can be directly applied to the production of the dehydropregnenolone acetate or sold as a commodity; and at the same time, the filter residue obtained from the filtration process is calcined to obtain the chromium oxide green which has a plurality of uses and high added value. The waste liquor treatment method provided by the invention is simple in process, capable of achieving energy conservation and emission reduction, and conductive to environment protection to generate social benefit; and by adopting the method, sodium acetate can be completely recovered, and the chromium oxide green with high added value can be obtained to generate great economic efficiency.

Description

technical field [0001] The invention relates to a method for recycling chemical waste water, in particular to a method for recycling dienolone acetate waste liquid. Background technique [0002] Utilizing saponin to produce dienolone acetate through chromic acid oxidative decomposition is the most mature and most commonly used production process at present. The waste liquid generated in the production process contains a large amount of chromium acetate, sodium acetate, acetic acid and organic oxide impurities. Appears as a thick paste. Generally, manufacturers sell it to steel mills at low prices for smelting steel. This is not only a big loss for dienolone acetate manufacturers, but also does not conform to green chemistry under the background of vigorously advocating global green economic integration. Chemical industry "reduce material consumption, realize waste reduction, recycling and harmless" requirements. [0003] Patent No. 200910063423.7, a method for preparing ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/10C07C51/41C01G37/033
Inventor 廖全斌代忠旭刘明国刘丹
Owner CHINA THREE GORGES UNIV
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