Process for preparing glycine using hydroxy-acetonitrile method

A technology of hydroxyacetonitrile and glycine, which is used in the preparation of cyanide reaction, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems such as the problem of separation of inorganic salts that has not been effectively solved, the purity of glycine is not ideal, and the reaction conditions are harsh, etc. Achieve the effect of reducing the generation of hydantoin and peptides, easy to control, and mild reaction conditions

Inactive Publication Date: 2010-09-29
重庆三峡英力化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction yield and the purity of glycine in this method are not ideal
The above method uses ammonia to react, which needs to be carried out under high temperature and high pressure conditions. The reaction conditions are harsh, the equipment investment is large, and the problem of separation of inorganic salts has not been effectively solved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1 Preparation of Glycine

[0051] 400 g of 50% hydroxyacetonitrile solution was added to the reactor at room temperature, 237 g of ammonia water was added, and after 30 minutes of reaction, 526 g of 32% sodium hydroxide solution was added to the ammoniated reaction solution, and the temperature was kept at 40-60 ° C for 4-5 h The ammonia solution of glycine sodium salt is obtained, deaminated to obtain a glycine sodium salt solution, and then 210 g of 98% sulfuric acid is added for neutralization and acidification to obtain a mixed solution of glycine and inorganic salt sodium sulfate. Add 20g of activated carbon to decolorize, cool to 10°C, crystallize, and remove sodium sulfate crystals by centrifugation. The filtrate is crystallized and purified by conventional methods to obtain 235-250g of glycine solid with a purity of more than 98.5% and a percent yield of 90-95%.

Embodiment 2

[0052] The preparation of embodiment 2 glycine

[0053] Add 400 g of 50% hydroxyacetonitrile solution to the reactor at room temperature, add 237 g of ammonia water, and after 30 minutes of reaction, add 299 g of Na to the ammoniated reaction solution 2 SO 4 and 156gCa(OH) 2 The formed mixed solution is incubated at 40-60° C. for 4-5 hours to obtain an ammonia solution of glycinate, and deaminated to obtain a glycinate solution. Subsequently, 210 g of 98% sulfuric acid was added for neutralization and acidification to obtain a mixed solution of glycine, inorganic salts sodium sulfate and calcium sulfate. After filtering to remove the calcium sulfate precipitate, add 20g of activated carbon to decolorize and cool to 10°C, crystallize, and centrifuge to remove sodium sulfate crystals. The filtrate is heated and concentrated and then cooled to room temperature to precipitate glycine crystals. After drying, weigh 220g, with a purity of 98.5% and a yield of 82.35%. .

Embodiment 3

[0054] Example 3 Preparation of Glycine

[0055] 400 g of 50% hydroxyacetonitrile solution was added to the reactor at room temperature, 237 g of ammonia water was added, and after 30 minutes of reaction, 526 g of 32% sodium hydroxide solution was added to the ammoniated reaction solution, and the temperature was kept at 40-60 ° C for 4-5 h The ammonia solution of glycine sodium salt is obtained, deaminated to obtain a glycine sodium salt solution, and then 426.6 g of 36% hydrochloric acid is added for neutralization and acidification to obtain a mixed solution of glycine and inorganic salt sodium chloride. After adding 20g of activated carbon for decolorization, the temperature was raised to 90°C, concentrated under reduced pressure until crystals were precipitated, filtered while hot to remove the inorganic salt sodium chloride, and the filtrate was crystallized and purified by conventional methods to obtain 230-250g of glycine solid with a purity of 98.5-99.5%. The yield is...

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Abstract

The invention discloses a glycine preparing method, which comprises the following steps: 1) blending hydroxy acetonitrile solution or composition to produce hydroxy acetonitrile with ammonia composition to obtain ammonization reacting liquid; 2) blending the ammonization reacting liquid and inorganic alkaline to obtain the alkaline hydrolytic solution; 3) neutralizing the alkaline hydrolytic solution through inorganic acid to obtain the neutralized liquid; 4) disposing the neutralized liquid to obtain the glycine.

Description

technical field [0001] The invention relates to a preparation method for obtaining glycine by direct aminolysis, alkali hydrolysis, neutralization and purification of hydroxyacetonitrile. Methods. Background technique [0002] Glycine is an important raw material for chemical, pharmaceutical, pesticide and other industries, and has a wide range of uses. At present, there are various methods to produce glycine, among which, the α-halogenated acid method is the main industrial production method in China. In the presence of the reaction in the solvent phase. Using the α-halogenated acid method, the solvent phase can be the water phase, but the method for producing glycine by the water phase method has many defects, such as the fact that the catalyst cannot be recovered, the consumption is large, the catalytic efficiency is low, and the unreacted raw materials cannot be returned. Due to the strong alkalinity and water content of the system, it is easy to generate hydrolyzed g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/12C07C229/08
Inventor 查正炯谢增勇顾爱宏黄仁才杨立雯袁可尹应武
Owner 重庆三峡英力化工有限公司
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