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A method for treating 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor

A technology of methylandrostene and diene, which is applied to the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as waste of resources and environmental pollution

Active Publication Date: 2022-04-15
SHANDONG SITO BIO TECHNOLOGY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the embodiments of the present invention is to provide a method for processing 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor, to solve the prior art problem of 16α- The treatment method of methylandrost-4, 9(11)-diene-3, 17-dione mother liquor is likely to cause technical problems of environmental pollution and waste of resources

Method used

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  • A method for treating 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor
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  • A method for treating 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor

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Embodiment 1

[0060] (1), 800Kg 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor produced in the workshop was pumped into the kettle, heated to 30~35°C, and added dropwise for 30~ 112Kg of 20% sodium carbonate solution at 35°C, precipitated lithium carbonate solid, stirred for one hour after dripping, filtered to obtain filter residue, washed twice with water, removed and dried at 90°C to obtain lithium carbonate.

[0061] (2), pump the filtrate and lotion in (1) into the multi-effect evaporator, distill under reduced pressure to a thick state, and recover the distilled water in the distillation process at the same time, the water recovered in the distillation process is used as process water in production Use; then filter the thick liquid to obtain the filtrate and 99Kg of white crystalline salt.

[0062] (3), re-throw the white crystalline salt in the reaction kettle, add 104Kg of 30% sodium hydroxide aqueous solution by mass percentage, stir for 1 hour, static layering, diisoprop...

Embodiment 2

[0065] (1), 850Kg 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor produced in the workshop was pumped into the kettle, heated to 30~35°C, and added dropwise for 30~ 133.3Kg of 15% sodium carbonate solution at 35°C with a mass percentage of 133.3Kg precipitated lithium carbonate solid, stirred for one hour after dripping, filtered to obtain a filter residue, washed twice with water, removed and dried at 90°C to obtain lithium carbonate.

[0066] (2), pump the filtrate and lotion in (1) into the multi-effect evaporator, distill under reduced pressure to a thick state, and recover the distilled water in the distillation process at the same time, the water recovered in the distillation process is used as process water in production use; then filter the thick liquid to obtain the filtrate and 110Kg of white crystalline salt.

[0067] (3), re-throw the white crystalline salt in the reaction kettle, add 116Kg of 30% sodium hydroxide aqueous solution by mass percentage, stir ...

Embodiment 3

[0070] (1), 800Kg 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor produced in the workshop was pumped into the kettle, heated to 30~35°C, and added dropwise for 30~ 100Kg of potassium carbonate solution with a mass percentage of 20% at 35°C, lithium carbonate solid was precipitated, stirred for one hour after dripping, and filtered to obtain a filter residue, which was washed twice with water, removed and dried at 90°C to obtain lithium carbonate.

[0071] (2), pump the filtrate and lotion in (1) into the multi-effect evaporator, distill under reduced pressure to a thick state, and recover the distilled water in the distillation process at the same time, the water recovered in the distillation process is used as process water in production Use; then filter the thick liquid to obtain the filtrate and 100Kg of white crystalline salt.

[0072] (3) Throw the white crystalline salt back into the reaction kettle, add 80Kg of water to dissolve it, add 30Kg of sodium hydroxid...

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Abstract

The embodiment of the present invention provides a method for processing 16α-methylandrosta-4,9(11)-diene-3,17-dione mother liquor, the method comprising: adding a sufficient amount of carbonic acid to the mother liquor The salt is subjected to a precipitation reaction, and the precipitate is taken out after the reaction is complete to obtain crude lithium carbonate; the solution after the precipitation is taken out is distilled to a thick state, and then the thick liquid is filtered to obtain a filter residue and a filtrate; the filter residue is put into a strong alkali solution After mixing, leave it still to obtain a layered solution; take the upper layer of the layered solution to distill to obtain diisopropylamine; take the lower layer of the layered solution to pass through chlorine gas and add an organic solvent for extraction reaction to obtain bromine; The aqueous solution obtained after the extraction reaction is distilled together with the filtrate to obtain solid waste containing organic phosphorus. The embodiment of the present invention can effectively recover diisopropylamine, lithium, bromine and water in the 16α-methylandroster-4,9(11)-diene-3,17-dione mother liquor, and can efficiently remove the mother liquor organophosphorus in.

Description

technical field [0001] The invention relates to the technical field of environmental protection, in particular to a method for treating 16α-methylandrost-4,9(11)-diene-3,17-dione mother liquor. Background technique [0002] 16α-methylandrost-4,9(11)-diene-3,17-dione is an important intermediate in the synthesis of betamethasone and dexamethasone. [0003] In the prior art, the synthetic route of 16α-methylandrost-4,9(11)-diene-3,17-dione is as follows: [0004] [0005] In the above synthetic route, it is necessary to use diisopropylamine to react with lithium metal or butyllithium to obtain lithium diisopropylamide, and at the same time, use polyethylene to absorb the hydrogen generated by the reaction, and then put And pass through methyl bromide and use hexamethylphosphoric triamide (HMPA) as a catalyst for reaction, and then add hydrochloric acid and water after the reaction to obtain 16α-methylandrost-4,9(11)-diene- 3,17-diketone will generate methanol, diisopropy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D15/08C01B7/09C07C209/86C07C209/00C07C211/06
CPCC01D15/08C01B7/096C07C209/86C07C209/00C07C211/06
Inventor 米奇杨明军孙福锁崔玉国王玉帅
Owner SHANDONG SITO BIO TECHNOLOGY CO LTD
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