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Recycling method of divalproex sodium crystallization mother liquor

A divalproex sodium and crystallization mother liquor technology, which is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problems of low purity, difficult quality control, low recovery rate, etc., and achieve reduction The production cost, the reaction process is easy to control, and the effect of the method is simple and easy

Active Publication Date: 2014-03-26
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is: the local concentration of valproic acid and sodium valproate is uneven, so there may be several mixing ratios in the obtained product, the purity of the product is reduced, and the quality is not easy to control
The disadvantages of this method are: the process has high requirements for equipment, which is difficult to meet in general production, and it is easy to cause product agglomeration during the drying process, affecting the use of the product, and the quality is not easy to control
However, the method is cumbersome to operate, the recovery rate is low, and the quality of recovered divalproex sodium is not up to standard or the purity is not high, which can neither effectively utilize it, but also increase the actual production cost

Method used

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  • Recycling method of divalproex sodium crystallization mother liquor

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Embodiment approach

[0052] A preferred embodiment of the present invention is:

[0053] A kind of recycling method of divalproex sodium crystallization mother liquor, it comprises:

[0054] 1) Concentrating divalproex sodium crystallization mother liquor to obtain a solid mixture containing divalproex sodium;

[0055] 2) adding the solid mixture obtained in step 1) to the sodium hydroxide solution to obtain a mixed solution;

[0056] 3) adding inorganic salts to the mixed solution obtained in step 2), and filtering to obtain metal salt precipitation of valproic acid; and

[0057] 4) Add the precipitated valproic acid salt obtained in step 3) into the hydrochloric acid solution, and fractionally distill the organic layer obtained after the reaction to obtain valproic acid.

[0058] Another preferred embodiment of the present invention is:

[0059] 1) Concentrate the divalproex sodium reaction mother liquor to dryness;

[0060] 2) Add 10-30% (w / v) concentration of sodium hydroxide until the mot...

Embodiment 1

[0071] In the three-necked flask, add divalproex sodium acetone reaction mother liquor 1700ml, recover acetone by normal pressure distillation, the distillation is complete at 60°C, and the concentrated residue weighs about 75 grams. Add about 39ml of 25% (w / v) sodium hydroxide solution, stir to adjust the pH to 8.0, the residue in the bottle is completely dissolved, add 20 grams of activated carbon, stir for 10 minutes and filter, add 27 grams of calcium chloride to the filtrate 54ml of aqueous solution was stirred to precipitate a large amount of white solids, cooled, suction filtered, washed with water, and dried to obtain 74.9 grams of white calcium valproate solids, with a yield of about 95% and a content of more than 99.1%.

[0072] Add the obtained calcium valproate into 200ml of 2mol / L hydrochloric acid, stir and separate the layers, distill the upper organic layer under reduced pressure, collect the distillate at 112-114℃ / 7~8mmHg, and obtain valproic acid transparent l...

Embodiment 2

[0074] In a three-neck flask, add divalproex sodium acetone reaction mother liquid 1700ml, recover acetone by atmospheric distillation, and the distillation is completed at 60°C, the concentrated residue weighs about 75 grams, and 25% (w / v) sodium hydroxide is added The solution is about 39ml, stir to adjust the pH to 9.5, all the residue in the bottle is dissolved, add 20 grams of activated carbon, stir for 10 minutes and filter, add 34ml of an aqueous solution made of 23 grams of magnesium chloride to the filtrate, stir to precipitate a large amount of white solid, cool, and suction filter, Washing with water and drying gave 71.6 grams of white magnesium valproate solid, with a yield of about 95.2% and a content greater than 99.1%.

[0075] Add the obtained magnesium valproate into 200ml of 2mol / L hydrochloric acid, stir and separate layers, distill the upper organic layer under reduced pressure, collect the distillate at 112-114°C / 7~8mm Hg, and obtain valproic acid transpare...

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Abstract

The invention provides a recycling method of divalproex sodium crystallization mother liquor. The method comprises the following steps: 1) concentrating the divalproex sodium crystallization mother liquor to obtain a solid-state mixture containing divalproex sodium; 2) mixing the solid-state mixture obtained in the step 1) with an alkaline solution to dissolve the solid-state mixture to further obtain a mixed solution; 3) mixing the mixed solution obtained in the step 2) with an inorganic salt to produce a valproate precipitate, and separating to obtain the valproate precipitate; 4) mixing the valproate precipitate obtained in the step 3) with an acid solution to obtain an organic layer, and performing fractionation on the organic layer to obtain valproic acid. Through the method provided by the invention, the yield of obtained valproic acid can be as high as 93%, the purity is not lower than 99.6%, and valproic acid can meet medicinal requirements; the method provided by the invention has the advantages of simplicity, easiness in operation, easiness in control of reaction process and effect of reducing actual production cost, and is in line with requirements of industrial mass production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for recycling divalproex sodium crystallization mother liquor. Background technique [0002] Divalproex sodium is an anticonvulsant and mood stabilizing drug mainly used in the treatment of epilepsy and bipolar disorder, and can also be used in the treatment of migraine and schizophrenia. Divalproex sodium is used to control absence seizures, tonic-clonic seizures (grand mal), complex partial seizures, and seizures associated with Lennox-Gastaut syndrome in patients with epilepsy. Divalproex binds and inhibits GABA transaminase. It acts by dissociation into valproate ions in the gastrointestinal tract. Divalproex sodium has less gastrointestinal side effects and fewer drug interactions, so it has physiological properties equal to or better than valproic acid or sodium valproate, and is widely used clinically. [0003] The report about the synthetic techniq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/487C07C53/128
CPCC07C51/02C07C53/128
Inventor 张小均马德银赵德李明川
Owner NEW FOUNDER HLDG DEV LLC
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