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Clean production method of glycine and derivatives thereof

A production method and technology of derivatives, applied in the direction of chemical instruments and methods, preparation of organic compounds, cyanide reaction preparation, etc., can solve the problems of separation of inorganic salts and products, separation of by-products, etc., and achieve purity and yield High, reduce production costs, avoid pollution effects

Inactive Publication Date: 2015-09-09
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The research team of the present inventors found that the aqueous solution containing aminoacetonitrile derivatives is hydrolyzed by one or more inorganic alkalis in calcium hydroxide, barium hydroxide, strontium hydroxide, calcium oxide, barium oxide and strontium oxide to eliminate Ammonia and organic amine compounds are separated to obtain an aqueous solution of glycine derivative salt and a white precipitate. In addition to excess calcium hydroxide, barium hydroxide, and strontium hydroxide, the white precipitate is produced by hydrolysis. Aminodiacetic acid, ethyliminodiacetic acid, nitrilotriacetic acid, etc. will also precipitate in the form of insoluble calcium salt, barium salt and strontium salt, which can be separated by simple filtration, thus solving the problem of difficult separation of by-products The aqueous solution of glycine derivative salt is neutralized by carbon dioxide to obtain inorganic carbonate precipitation and glycine derivative solution. The inorganic carbonate precipitation can be separated by simple filtration, which solves the problem of difficult separation of inorganic salt and product. In addition, the oxides and carbon dioxide obtained by calcination of the separated inorganic carbonate can be recycled. This process produces no waste water and waste residue, and the production process is environmentally friendly and clean.

Method used

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  • Clean production method of glycine and derivatives thereof
  • Clean production method of glycine and derivatives thereof
  • Clean production method of glycine and derivatives thereof

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Effect test

Embodiment 1

[0051] Embodiment 1 N, the preparation of N-dimethylglycine

[0052] Add 614g (4.5mol) of 33% dimethylamine aqueous solution into a 2500ml four-neck flask, start stirring, reflux and cool, heat up and preheat to 35°C-40°C, weigh 408g (3.0mol) of hydroxyacetonitrile aqueous solution, and add constant pressure drops Liquid funnel; control the reaction temperature at 40°C-45°C, control the slow dropwise addition for 1-1.5h, and keep warm for 3h after the dropwise addition; transfer the aqueous solution of the synthesized N,N-dimethylaminoacetonitrile compound to the constant pressure dropping funnel for later use; Add 222.3g-333g (3.0-4.5mol) of calcium hydroxide and 1000g of water into a 3000ml four-neck flask, raise the temperature and preheat to 75°C-80°C, slowly add the above-mentioned N,N-dimethylaminoacetonitrile aqueous solution into hydrogen In the calcium oxide emulsion, stir to remove ammonia at the same time; control the reaction temperature at 75°C-80°C, slowly add dr...

Embodiment 2

[0055] Embodiment 2 N, the preparation of N-dimethylglycine

[0056] Add 614g (4.5mol) of 33% dimethylamine aqueous solution into a 2500ml four-necked flask, start stirring, reflux and cool, heat up and preheat to 35°C-40°C, weigh 408g (3.0mol) of hydroxyacetonitrile aqueous solution, and add constant pressure drops Liquid funnel; control the reaction temperature at 40°C-45°C, control the slow dropwise addition for 1-1.5h, and keep warm for 3h after the dropwise addition; transfer the aqueous solution of the synthesized N,N-dimethylaminoacetonitrile compound to the constant pressure dropping funnel for later use; Add 222.3g-333g (3.0-4.5mol) of calcium hydroxide and 1000g of water into a 3000ml four-neck flask, raise the temperature and preheat to 75°C-80°C, slowly add hydrogen dropwise to the above-mentioned N,N-dimethylaminoacetonitrile aqueous solution In the calcium oxide emulsion, stir to remove ammonia at the same time; control the reaction temperature at 75°C-80°C, slow...

Embodiment 3

[0059] Embodiment 3 N, the preparation of N-dimethylglycine

[0060] Add 614g (4.5mol) of 33% dimethylamine aqueous solution into a 2500ml four-neck flask, start stirring, reflux and cool, heat up and preheat to 35°C-40°C, weigh 408g (3.0mol) of hydroxyacetonitrile aqueous solution, and add constant pressure drops Liquid funnel; control the reaction temperature at 40°C-45°C, control the slow dropwise addition for 1-1.5h, and keep warm for 3h after the dropwise addition; transfer the aqueous solution of the synthesized N,N-dimethylaminoacetonitrile compound to the constant pressure dropping funnel for later use; Add 514g-771g (3.0-4.5mol) of barium hydroxide and 1500g of water into a 5000ml four-neck flask, raise the temperature and preheat to 75°C-80°C, slowly add the above-mentioned N,N-dimethylaminoacetonitrile aqueous solution into hydrogen In the barium oxide emulsion, stir and discharge ammonia at the same time; control the reaction temperature at 75°C-80°C, slowly add dr...

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Abstract

The present invention belongs to the technical field of production, separation and purification of organic compounds, and particularly relates to a clean production method of glycine and derivatives thereof. The method specifically comprises that an aqueous solution of an amino acetonitrile derivative represented by a formula I is subjected to an inorganic alkali hydrolysis reaction, ammonia and organic amine compounds are discharged, separation is performed to obtain an aqueous solution of glycine derivative salts and white precipitate, carbon dioxide is introduced into the aqueous solution of the glycine derivative salts to neutralize, separation is performed to obtain an inorganic carbonate precipitate and a solution of glycine derivatives represented by a formula II, and the glycine derivatives are obtained from the glycine derivative solution. With the method of the present invention, the separation and purification difficulty problems of the glycine derivatives and the byproducts such as iminodiacetic acid, methyl iminodiacetic acid, ethyl iminodiacetic acid, inorganic salts and the like are solved, the purifity and the yield of the glycine derivatives are high, the raw material is completely utilized, the production cost is reduced, the pollution of the three waste on the environment is avoided, and the production is clean and environmental protection. The formulas I and II are defined in the instruction.

Description

technical field [0001] The invention belongs to the technical field of production, separation and purification of organic compounds, and in particular relates to a clean production method of glycine and its derivatives. Background technique [0002] Glycine, also known as aminoacetic acid, is an important fine chemical synthesis intermediate, which has been widely used in medicine, food, chemical industry, pesticide and other fields. The food and pharmaceutical industries have gradually become the largest demand areas for the use of glycine, and its market demand is very large. In 2010, the global demand will be close to 1000kt. [0003] Due to the special structure of glycine, glycine and glycine derivatives have been widely used in industry, agriculture, biomedicine and other fields. Common glycine derivatives include N,N-dimethylglycine, N,N-diethylglycine, N- Methylglycine, N-ethylglycine, etc., can be used as effective chelating agents for metal ions in industry, and a...

Claims

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Application Information

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IPC IPC(8): C07C229/08C07C229/12C07C227/18
Inventor 吴传隆秦岭王用贵李欧杨帆姚如杰郑道敏
Owner CHONGQING UNISPLENDOUR CHEM