High efficiency production method of glycine

A production process, glycine technology, applied in the chemical industry, can solve the problems of difficult recycling of catalysts, limited industrial production value, freezing to -10°C, etc., and achieve the effects of facilitating recycling, increasing yield, and reducing production energy consumption

Inactive Publication Date: 2018-06-01
严世佳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming of chloroacetic acid ammonolysis synthetic method: energy consumption is high, and yield is low (about 85%), also has a large amount of catalysts (hexamethamine) to be difficult to recycle
[0003] Chinese patent application "A kind of clean production process of glycine co-production ammonium chloride" (public number: CN103570568), and Chinese patent application "a kind of clean production process of glycine co-production calcium chloride" (public number: CN103

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a three-necked reaction flask equipped with a thermometer, a magnetic stirrer, a condenser tube and a dropping funnel, add 27.88 grams of 0.2500 mol of ammonium chloroacetate, 85.0 grams of methanol and 7.5 grams of urotropine, stir until completely dissolved, and heat up to At 60°C, 32.31 g (0.2500 mol) of N,N-diisopropylethylamine was slowly added dropwise, and the dropwise addition was completed within 2 hours, and then kept stirring at 67°C for 2.5 hours. Cool down to 50°C, filter the precipitated glycine crystals, and filter the mother liquor for the reaction in Example 2. The obtained glycine crystals were washed with methanol and dried to obtain 18.1 g of glycine crystals with a content of 98.5%, with a yield of 95.0%.

Embodiment 2

[0029] In the three-necked reaction flask that thermometer, magnetic stirrer, condensing tube and dropping funnel are housed, add respectively 27.88 grams (0.2500 moles) of ammonium chloroacetate, the filter mother liquor of embodiment one and add 0.8 grams of urotropine, stir Until it is completely dissolved, heat up to 63°C, start to slowly add 32.31 g (0.2500 mol) of N,N-diisopropylethylamine dropwise, and complete the dropwise addition within 2 hours, then keep stirring at 67°C for 2.5 hours. The temperature was lowered to 45° C., the precipitated glycine crystals were filtered, and the mother liquor was filtered for the third reaction in Example 3. The obtained glycine crystals were washed with methanol and dried to obtain 18.5 g of glycine crystals with a content of 98.2%, with a yield of 96.8%.

Embodiment 3

[0031] In a three-necked reaction flask equipped with a thermometer, a magnetic stirrer, a condenser and a dropping funnel, add 27.88 grams (0.2500 moles) of ammonium chloroacetate and the filtered mother liquor of Example 2 respectively, stir until completely dissolved, and heat up to 65°C , began to slowly add 32.31 g (0.2500 mol) of N,N-diisopropylethylamine dropwise, the dropwise addition was completed within 2 hours, and then kept stirring at 67°C for 2.5 hours. The temperature was lowered to 45° C., and the precipitated glycine crystals were filtered. The obtained glycine crystals were washed with methanol and dried to obtain 18.6 g of glycine crystals with a content of 98.0%, with a yield of 97.1%. Then, the temperature of the filtered mother liquor was lowered to 10° C., and 26.9 g of the precipitated N,N-diisopropylethylamine hydrochloride was filtered, and the filtered mother liquor was used for the reaction in Example 4.

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PUM

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Abstract

The invention discloses a high efficiency production method of glycine. The high efficiency production method comprises following steps: solvent methanol or ethanol, and catalyst urotropine or paraformaldehyde are introduced into a reactor, Ammonium-monochloracetat is added, the temperature is increased to 60 to 70 DEG C, N,N-Diisopropylethylamine or N,N-Diethylbenzylamine or N, N-di-n-propyl benzylamine or N, N-di-n-butyl benzylamine are added dropwise in 2h, thermal insulation reaction is carried out at 65 to 75 DEG C for 2.5h, the temperature is reduced to 40 to 50 DEG C for precipitation of glycine crystal, or the temperature is reduced to 10 to 25 DEG C for precipitation of a mixture of glycine crystal and an ammonium salt; and then filtering, washing, and drying are carried out successively so as to obtain a glycine product, wherein a washing liquid is adopted for recycling of N,N-Diisopropylethylamine or N,N-Diethylbenzylamine or N, N-di-n-propyl benzylamine or N, N-di-n-butyl benzylamine. The glycine yield is increased by 10% of that in the prior art; energy consumption is reduced; catalyst recycling is realized; recycling of N,N-Diisopropylethylamine or N,N-Diethylbenzylamine or N, N-di-n-propyl benzylamine or N, N-di-n-butyl benzylamine is realized; and combined production of ammonium chloride is realized.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a high-efficiency production process of glycine. Background technique [0002] Glycine is the simplest amino acid, and it is widely used in chemical industry, pesticide, medicine, food and farming. At present, the Strecker synthesis method is mainly used to produce glycine in the United States, Japan and other countries, and the ammonolysis synthesis method of chloroacetic acid is used in China. The process of ammonolysis synthesis of chloroacetic acid is: react chloroacetic acid, ammonia, and urotropine in water, add a large amount of methanol to precipitate glycine, produce a ton of glycine to produce methanol mother liquor of more than ten cubic meters, and recover methanol requires a large amount of energy. The main shortcoming of chloroacetic acid ammonolysis synthetic method: energy consumption is high, and yield is low (about 85%), also has a large amount of cat...

Claims

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Application Information

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IPC IPC(8): C07C227/08C07C229/08C01C1/16
CPCC01C1/164C07C227/08C07C229/08Y02P20/584
Inventor 严世佳李增寅
Owner 严世佳
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