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A kind of method of reclaiming potassium chloride from valproic acid high-salt waste water

A high-salt wastewater and valproic acid technology, applied in the separation/purification of carboxylic acid compounds, alkali metal chlorides, organic chemistry, etc., can solve the problems of bacterial death, reduce the total yield, and increase manufacturing costs. Reach the effect of reducing chemical oxygen consumption, reducing processing difficulty and saving cost

Active Publication Date: 2022-01-28
HUNAN XIANGZHONG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, not only the total yield is reduced, but the manufacturing cost is increased, and the existence of these organic acids also increases the oxygen consumption value of the wastewater and increases the difficulty of wastewater treatment.
And if the concentration of potassium chloride is too high, it is easy to cause equipment corrosion, bacteria death, sewage treatment capacity decline, and discharge not up to standard in the process of sewage treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Pump 3000kg of acid water after centrifuging dipropylmalonic acid into a 5000L reactor, add 500kg of tert-butyl methyl ether under stirring, continue stirring for 1 hour, and let stand to separate layers. The organic layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate was put into a clean and dry esterification kettle, concentrated to dryness, and propylmalonic acid and dipropylmalonic acid were recovered. The acid water is pumped into another 5000L reaction kettle, and potassium hydroxide solution is added dropwise under stirring to adjust the pH to 5-6. When the water is distilled to about 1000L, transfer to the crystallization kettle, continue to distill water to about 400L, cool down, centrifuge, and discharge the material into a drying oven to dry to constant weight (moisture ≤ 0.5%). Obtain potassium chloride 380kg of white crystalline powder, purity is 95.8%, yield 84.4%.

Embodiment 2

[0020] Pump 3000kg of acid water after centrifuging dipropylmalonic acid into a 5000L reactor, add 500kg of tert-butyl methyl ether under stirring, continue stirring for 1 hour, and let stand to separate layers. The organic layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate was put into a clean and dry esterification kettle, concentrated to dryness, and propylmalonic acid and dipropylmalonic acid were recovered. The acid water is pumped into another 5000L reaction kettle, and potassium hydroxide solution is added dropwise under stirring to adjust the pH to 7-7.5. When the water is distilled to about 1000L, transfer to the crystallization kettle, continue to distill water to about 400L, cool down, centrifuge, and discharge the material into a drying oven to dry to constant weight (moisture ≤ 0.5%). Obtain potassium chloride 400kg of white crystalline powder, purity is 96.5%, yield 88.9%.

Embodiment 3

[0022] Pump 3000kg of acid water after centrifuging dipropylmalonic acid into a 5000L reactor, add 500kg of tert-butyl methyl ether under stirring, continue stirring for 1 hour, and let stand to separate layers. The organic layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate was put into a clean and dry esterification kettle, concentrated to dryness, and propylmalonic acid and dipropylmalonic acid were recovered. The acid water is pumped into another 5000L reaction kettle, and potassium hydroxide solution is added dropwise under stirring to adjust the pH to 8-9. When the water is distilled to about 1000L, transfer to the crystallization kettle, continue to distill water to about 400L, cool down, centrifuge, and discharge the material into a drying oven to dry to constant weight (moisture ≤ 0.5%). Obtain potassium chloride 390kg of off-white crystalline powder, purity is 93.8%, yield 84.4%.

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Abstract

The invention proposes a method for recovering potassium chloride from valproic acid high-salt wastewater. The steps include: (1) collecting the acid water after centrifuging dipropylmalonic acid, adding ether, ester, chlorinated hydrocarbon, alcohol (immiscible with water) solvent, stirring and extracting, layering, drying to obtain 2-propane Dipropylmalonic acid and dipropylmalonic acid, the recovery rate reaches more than 90%, and can be used to prepare valproic acid. (2) Collect the waste acid water after recovering 2-propylmalonic acid and dipropylmalonic acid, adjust the pH to 7-7.5 with potassium hydroxide, distill water to an appropriate amount, add activated carbon and diatomaceous earth for decolorization, filter, Vacuum belt drying to obtain white crystalline powder with high purity and high recovery rate. Prepare valproic acid by reclaiming 2-propylmalonic acid and dipropylmalonic acid, and reclaim high-purity potassium chloride from waste water, which not only reduces the production cost of valproic acid, but also greatly eases the subsequent Environmental pressures.

Description

technical field [0001] The invention relates to a method for recovering potassium chloride from valproic acid high-salt wastewater. Background technique [0002] Valproic acid and its derivatives belong to the first-line antiepileptic drugs, which act in the form of valproic acid after being absorbed by the body. Partial motor seizures, absence seizures, and infantile spasms. Today, the therapeutic field of valproic acid and its derivatives is still expanding. In addition to anti-epilepsy, the FDA-approved indications also include bipolar disorder and migraine. [0003] Propylation, hydrolysis, acidification and decarboxylation of diethyl malonate to obtain valproic acid has become the first choice for large-scale industrial production of valproic acid and its derivatives. However, according to analysis and statistics, after acidification and separation of 2,2-dipropylmalonic acid, the acid water contains more organic acids, including the main by-product propylmalonic acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F1/66C01D3/04C01D3/16C01D3/14C07C51/48C07C55/02
CPCC01D3/04C01D3/16C01D3/14C07C51/48C01P2006/80C07C55/02
Inventor 唐汉华段世辉杨贞皓
Owner HUNAN XIANGZHONG PHARM CO LTD
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