Synthesis and post-treatment method of high-purity N-carbamylglutamic acid

A technology of carbamoyl glutamic acid and sodium glutamate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfate/bisulfate, etc., can solve the problems of high cost, complex process, low product purity, etc. problems, to achieve the effect of reducing production costs

Active Publication Date: 2017-08-11
内蒙古天翊生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] As can be seen from the above, the existing methods are complicated in technology and high in cost. After hydrochloric acid is acidified, it needs to be heated to more than 80° C. to dissolve, and then the product is cooled and crystallized to obtain the product. Sodium chloride is easily wrapped in the process, which makes the product less pure and produces a large amount of saline wastewater

Method used

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  • Synthesis and post-treatment method of high-purity N-carbamylglutamic acid
  • Synthesis and post-treatment method of high-purity N-carbamylglutamic acid
  • Synthesis and post-treatment method of high-purity N-carbamylglutamic acid

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Embodiment 1

[0025] The steps of the synthesis of the high-purity N-carbamylglutamic acid and its post-processing method of the present invention are as follows:

[0026] a, the 1:1 molar ratio of sodium glutamate and sodium cyanate is added to the reaction kettle, and water is used as a solvent, and the reaction is stirred at 50 °C;

[0027] b, the reaction solution was cooled, acidified to PH=3 with 80% sulfuric acid by mass, then heated to 40° C., stirred uniformly, and filtered to obtain the target product; the product purity was 99.2%.

[0028] c, the mother liquor is cooled to 0°C, the hydrated sodium sulfate is precipitated, and filtered to obtain the by-product hydrated sodium sulfate, and the filtrate is adjusted to neutrality with sodium hydroxide solution for recycling.

Embodiment 2

[0030] The steps of the synthesis of the high-purity N-carbamylglutamic acid and its post-processing method of the present invention are as follows:

[0031] a, the 1:1 molar ratio of sodium glutamate and sodium cyanate is added to the reactor, and water is used as a solvent, and the reaction is stirred at 30 °C;

[0032] b, the reaction solution is cooled, acidified to PH=3 with 90% sulfuric acid by mass, then heated to 50° C., stirred evenly, and filtered to obtain the target product; the product has a purity of 99.5%.

[0033] c, the mother liquor is cooled to 5°C, the hydrated sodium sulfate is precipitated, and filtered to obtain the by-product hydrated sodium sulfate, and the filtrate is adjusted to neutrality with sodium hydroxide solution for recycling.

Embodiment 3

[0035] Get embodiment 1 filtrate, liquid chromatography detects the glutamic acid content in the solution, adds sodium hydroxide solution and adjusts the pH value to be 7, adds corresponding sodium glutamate and sodium cyanate, distilled water according to the condition of embodiment 1, stirs down The reaction was heated to 50° C., processed according to the treatment steps of Example 1, and the filtrate was repeated 3 times. The results were as follows, and the purity was all greater than 99.2%.

[0036] repeat times one two three purity(%) 99.5 99.2 99.5

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Abstract

The invention discloses a synthesis and post-treatment method of high-purity N-carbamylglutamic acid and belongs to the field of organic chemistry and fine chemical engineering. According to the method, sodium glutamate and sodium cyanate are adopted as raw materials to prepare N-carbamoyl sodium glutamate, acidification is performed with sulfuric acid after reaction is completed, then heating is performed to 40-50 DEG C, and filtration is performed to obtain a high-purity product after even stirring; a mother solution is cooled to 0-5 DEG C, a byproduct sodium sulfate decahydrate is obtained through filtration, the mother solution is regulated to be neutral with a sodium hydroxide solution for recycled usage. The problems of high cost, low purity, difficult wastewater treatment and the like in the N-carbamylglutamic acid production process are solved, the product purity is up to 99% or above, and a feasible way is provided for industrial production of the N-carbamylglutamic acid.

Description

technical field [0001] The invention belongs to the field of organic chemistry and fine chemical industry, and in particular relates to a method for synthesizing high-purity N-carbamylglutamic acid and its post-processing. Background technique [0002] N-carbamylglutamic acid is an important derivative for the synthesis of different side chain antibacterial agents, and has been used as a drug for the treatment and prevention of hyperammonemia; in addition, it is also an intermediate for the synthesis of heterocyclic and polypeptide compounds. In recent years, it has been found that adding this substance to pig feed can increase the level of arginine required in the growth process of pigs, thereby increasing the growth rate of pigs. [0003] At present, the synthesis and post-processing methods of N-carbamylglutamic acid mainly include the following: [0004] 1. Microwave synthesis [0005] Select glutamic acid and urea as raw materials, add a certain amount of sodium hydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/18C07C275/16C01D5/02
CPCC01D5/02C07C273/1809C07C273/189C07C275/16
Inventor 李中贤刘小培王俊伟殷园园余学军董学亮徐丹
Owner 内蒙古天翊生物科技有限公司
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