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Method for recovering and recycling L-tartaric acid

A technology of tartaric acid and ammonium hydrogen tartrate, applied in chemical instruments and methods, preparation of carboxylates, preparation of organic compounds, etc., can solve the problems of high cost and large energy consumption, and achieves reduced energy consumption, simple process operation, and reaction mild conditions

Active Publication Date: 2012-06-20
京山瑞生制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In summary, there are various defects in the existing recovery and utilization methods of tartaric acid, or a large amount of calcium sulfate by-products are generated, and because the tartaric acid aqueous solution is evaporated, concentrated and crystallized, the energy consumption is very large and the cost is relatively high ; Or need to form D-sodium hydrogen tartrate or D-potassium hydrogen tartrate precipitation, thereby realize the separation of tartaric acid, the defects such as higher cost

Method used

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  • Method for recovering and recycling L-tartaric acid
  • Method for recovering and recycling L-tartaric acid

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) acidification precipitation: get the waste water 1000g (7wt% L-tartaric acid) containing diammonium tartrate that the p-thymphenyl phenylserine ethyl ester resolution process of racemization produces, be 45-50 ℃ at reaction temperature, with concentrated Hydrochloric acid was acidified to pH 3, and the reaction time was 0.5h. The reaction solution formed a precipitate of ammonium hydrogen tartrate and was filtered. The obtained precipitate was dried and dehydrated to obtain 66.5 g of ammonium hydrogen tartrate (85.3% recovery rate). L-ammonium hydrogen tartrate is an off-white solid with a purity greater than 99% and an optical purity of 100% as determined by HPLC.

[0024] (2) Acidification desalination: get the product ammonium hydrogen tartrate 33.4g obtained in the step (1), add 135g methyl alcohol, add the concentrated sulfuric acid of 10g, carry out acidification reaction. The reaction temperature is 42-45°C, and the reaction time is 2h. After the reaction,...

Embodiment 2

[0026] (1) Acidification precipitation: get the waste water 1000g (8wt% L-tartaric acid) containing the diammonium tartrate that the racemized p-thymphenylphenylserine ethyl ester resolution process produces, be 0 ℃ at reaction temperature, acidify with concentrated sulfuric acid To pH 2.5, the reaction time is 2h. The reaction solution formed a precipitate of ammonium hydrogen tartrate and was filtered. The obtained precipitate was dried and dehydrated to obtain 81.9 g of ammonium hydrogen tartrate (92.0% recovery). L-ammonium hydrogen tartrate is an off-white solid with a purity greater than 99% and an optical purity of 100% as determined by HPLC.

[0027] (2) acidification desalination: get the product ammonium hydrogen tartrate 33.4g of gained in the step (1), add 135g methyl alcohol, add 23.1g hydrochloric acid methanol solution (30%), carry out acidification reaction. The reaction temperature is 20-25°C, and the reaction time is 6h. After the reaction, the inorganic s...

Embodiment 3

[0029] (1) Acidification precipitation: get the waste water 1000g (10wt% L-tartaric acid) containing the diammonium tartrate that the racemized p-thymphenylphenylserine ethyl ester resolution process produces, be 25-30 ℃ at reaction temperature, with phosphoric acid Acidification to pH 4.0-4.5, the reaction time is 4h. The reaction solution formed a precipitate of ammonium hydrogen tartrate and was filtered. The obtained precipitate was dried and dehydrated to obtain 92.4 g of ammonium hydrogen tartrate (recovery rate: 83.0%). L-ammonium hydrogen tartrate is an off-white solid with a purity greater than 99% and an optical purity of 100% as determined by HPLC.

[0030] (2) acidification desalination: get the product ammonium hydrogen tartrate 33.4g obtained in the step (1), add 135g methyl alcohol, add 12g acetic acid, carry out acidification reaction. The reaction temperature is 0°C, and the reaction time is 10 h. After the reaction, the inorganic salts are removed by filtr...

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Abstract

The invention provides a method for recovering and recycling L-tartaric acid. The method comprises the following steps of: performing acidification and precipitation specific to waste water containing tartaric acid diammonium generated in a process for splitting racemic 4-methylsulfonylphenyl serine ethyl ester to form and separate a tartaric acid hydrogen ammonium salt; and acidizing and desalting to obtain a methanol solution of the L-tartaric acid. The method can be directly applied to the splitting process of racemic 4-methylsulfonylphenyl serine ethyl ester, and the recovery and recycling of the L-tartaric acid are realized. The method provided by the invention has mild reaction conditions and simple process operation, and the production cost of the splitting process can be greatly lowered.

Description

Technical field [0001] The present invention relates to a method for recovering and recycling L-tartaric acid. Background technology [0002] L-tartaric acid (L-tartaric acid), molecular formula: C4H606, molecular weight: 150.09, CAS number: 87-69-4. This product is colorless translucent crystals or white fine to coarse crystalline powder with a sour smell. [0003] L-tartaric acid (L-tartaric acid) is widely used as a sour agent in beverages and other foods, and is used in wine, soft drinks, candies, bread, and some gelatinous sweets. Utilizing its optical activity, it can be used as a chemical resolving agent for the production of anti-tuberculosis drug intermediate DL-aminobutanol. It can also be used as a chiral raw material for the synthesis of tartaric acid derivatives. Utilizing its acidity, it can be used as a polyester fabric resin. Catalyst for finishing, PH regulator for oryzanol production; utilizing its complexing properties, used as complexing agent, masking ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/255C07C51/02C07C315/06C07C317/48
Inventor 张治国程云涛
Owner 京山瑞生制药有限公司
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