Method for synthesizing aminoacetonitrile hydrochloride from hydrocyanic acid

A technology of aminoacetonitrile hydrochloride and aminoacetonitrile, which is applied in the preparation of carboxylic acid nitriles, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of large amount of wastewater, lengthy process, and increased wastewater treatment costs. Achieve the effects of mild reaction conditions, simple process, high appearance and high content

Pending Publication Date: 2020-08-04
营口德瑞化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are three main disadvantages of this method: First, the process is lengthy, requiring three solid-liquid separations and two solid dryings, long production cycle, large energy consumption, and large equipment occupation
Second, the amount of wastewater is large, and high cyanide, high COD, high ammonia nitrogen, and high salt are difficult to treat, which increases the cost of wastewater treatment
Third, the yield is low and the product quality is not stable

Method used

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  • Method for synthesizing aminoacetonitrile hydrochloride from hydrocyanic acid
  • Method for synthesizing aminoacetonitrile hydrochloride from hydrocyanic acid
  • Method for synthesizing aminoacetonitrile hydrochloride from hydrocyanic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Synthesize hydroxyacetonitrile according to the general process;

[0030] 2) Put 102 grams of 25% ammonia water into a 500 mL four-necked reaction flask, start stirring, control the temperature at 20-30°C, slowly add 114 grams of 50% hydroxyacetonitrile dropwise, and keep stirring for 1.5 hours. Deamination yields aminoacetonitrile.

[0031] 3) Control the temperature at 20-30° C., slowly add 183 grams of 30% hydrochloric acid dropwise into the reaction flask. Keep warm and stir for 2 hours. Dehydrochlorination, low-temperature negative pressure concentration to a certain amount of water, cooling crystallization, filtration, vacuum drying to obtain the dry product of aminoacetonitrile hydrochloride, the appearance of which is off-white crystalline powder. The weight is 75.5 grams, and the yield is 81.6% (based on hydroxyacetonitrile). The content is 99.3%.

Embodiment 2

[0033] 1) Synthesize hydroxyacetonitrile according to the general process;

[0034] 2) Put 114 grams of 50% hydroxyacetonitrile into a 500 mL four-necked reaction flask. Stirring was started, the temperature was controlled at 20-30°C, and 25.5 grams of ammonia gas was quickly introduced. Keep stirring for 1.5 hours. Deamination obtains aminoacetonitrile;

[0035] 3) Control the temperature at 20-30°C at 30°C, and slowly inject 55 grams of hydrogen chloride gas into the reaction bottle. Keep warm and stir for 2 hours. Dehydrochlorination, low-temperature negative pressure concentration to a certain amount of water, cooling crystallization, filtration, vacuum drying to obtain the dry product of aminoacetonitrile hydrochloride, the appearance of which is off-white crystalline powder. The weight is 76 grams, and the yield is 82.2% (based on hydroxyacetonitrile). The content is 99.6%.

Embodiment 3

[0037] 1) Synthesize hydroxyacetonitrile according to the general process;

[0038] 2) Put 75 grams of 25% ammonia water into a 500 mL four-necked reaction bottle. Stirring was started, the temperature was controlled at 20-30°C, and 114 grams of 50% hydroxyacetonitrile was slowly added dropwise. Keep stirring for 1.5 hours. Deamination yields aminoacetonitrile.

[0039] 3) Control the temperature at 20-30° C., slowly add 134 grams of 30% hydrochloric acid dropwise into the reaction bottle. Keep warm and stir for 2 hours. Dehydrochlorination, low-temperature negative pressure concentration to a certain amount of water, cooling crystallization, filtration, vacuum drying to obtain the dry product of aminoacetonitrile hydrochloride, the appearance of which is off-white crystalline powder. The weight is 74 grams, and the yield is 80% (calculated as hydroxyacetonitrile). The content is 99.3%.

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Abstract

The invention relates to the technical field of organic chemical synthesis. The method comprises the following steps: reacting hydrocyanic acid with formaldehyde to obtain a hydroxyacetonitrile aqueous solution, reacting hydroxyacetonitrile with ammonia to obtain an aminoacetonitrile aqueous solution, reacting aminoacetonitrile with hydrogen chloride, and concentrating, crystallizing, filtering and drying the obtained feed liquid to obtain aminoacetonitrile hydrochloride. The method provided by the invention is simple in technological process and mild in reaction condition, high-temperature and high-pressure operation is not involved, and used equipment is conventional equipment; except hydrocyanic acid, other raw materials are easy to obtain, and the raw material cost is low; waste waterand waste gas are small in amount and can be used indiscriminately, and only a small amount of ammonium chloride is generated; the product quality is good, and the appearance and content are higher than those of a sodium cyanide process.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing aminoacetonitrile hydrochloride from hydrocyanic acid. Background technique [0002] Aminoacetonitrile hydrochloride is an important pharmaceutical and pesticide intermediate, which can be used in the synthesis of a variety of organic compounds, such as the plant growth regulator Thidiazuron, the brain function improver Oxiracetam, the antirheumatic drug Ilamo Germany, antihypertensive drug timolol and so on. [0003] At present, the commonly used technique is first to use sodium cyanide, formaldehyde, ammonium chloride, etc. as raw materials to synthesize a one-step intermediate methyleneaminoacetonitrile, and then react methyleneaminoacetonitrile in a hydrogen chloride alcohol solution to obtain aminoacetonitrile hydrochloride. There are three main disadvantages of this method: First, the process is lengthy, requiring three solid-li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/25
CPCC07C253/00C07C253/30
Inventor 刘子程麻勇任江胜刘玉宝安东亮吴丹李雪研纪宇侯奕彤
Owner 营口德瑞化工有限公司
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