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Preparation method of aminoacetonitrile hydrochloride

A technology of aminoacetonitrile hydrochloride and aminoacetonitrile is applied in the field of preparation of aminoacetonitrile hydrochloride, can solve the problems of high cost, low yield, complicated operation and the like, and achieves the effects of simple operation and high total yield

Inactive Publication Date: 2012-05-02
太仓市茜泾化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Among the above methods, although the liquid hydrocyanic acid method has a higher yield, the operation is dangerous. In order to obtain liquid hydrocyanic acid, a refrigeration system and equipment investment are required large, high cost, and uneconomical; while the hydroxyacetonitrile method has long reaction steps, cumbersome operation, large equipment investment, and high cost; the sodium cyanide method has the advantage of simple operation, but the yield is low, only about 50%

Method used

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Embodiment 1

[0018] A kind of preparation method of aminoacetonitrile hydrochloride: comprise the steps:

[0019] (1) Ammonium chloride, formaldehyde, acetic acid and sodium cyanide are used as reaction raw materials to generate aminoacetonitrile through condensation reaction: first, 53.5g of ammonium chloride, 162g of 37% formaldehyde and 267.5g of water are put into the reactor, and after stirring evenly , cooled to below 0°C, then dropwise added 153g of 32% sodium cyanide aqueous solution, and added dropwise to half, started to add 42g of acetic acid dropwise at the same time, after the dropwise addition, continued the reaction at below 0°C for 1-2 hours, then filtered, and left Experience aminoacetonitrile 48g, wherein, the weight ratio of ammonium chloride, formaldehyde, acetic acid, sodium cyanide is 1:2:0.7:1.

[0020] (2), make aminoacetonitrile and methanol solution of hydrogen chloride react to generate aminoacetonitrile hydrochloride: 48g of aminoacetonitrile obtained in s...

Embodiment 2

[0022] A kind of preparation method of aminoacetonitrile hydrochloride: comprise the steps:

[0023] (1) Ammonium chloride, formaldehyde, acetic acid and sodium cyanide are used as reaction raw materials to generate aminoacetonitrile through condensation reaction: first, 53.5g of ammonium chloride, 162g of 37% formaldehyde and 267.5g of water are put into the reactor, and after stirring evenly , cooled to below 0°C, then added dropwise 122.5g of 40% sodium cyanide aqueous solution, and added dropwise to half, started to add 42g of acetic acid dropwise at the same time, after the dropwise addition, continued to react at below 0°C for 1-2 hours, and then filtered, Centrifuge to obtain 48g of aminoacetonitrile.

[0024] (2), make aminoacetonitrile and methanol solution of hydrogen chloride react to generate aminoacetonitrile hydrochloride: 48g of aminoacetonitrile obtained in step (1), 90g of methanol solution of hydrogen chloride (the content of hydrochloric acid in the so...

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Abstract

The invention relates to a preparation method of aminoacetonitrile hydrochloride, which comprises the following steps: (1) carrying out condensation reaction by using ammonium chloride, formaldehyde, acetic acid and sodium cyanide as reaction raw materials to generate aminoacetonitrile: adding the ammonium chloride, formaldehyde and water into a reactor, uniformly stirring, cooling to below 0 DEG C, dropwisely adding 30-40 wt% sodium cyanide aqueous solution, starting to dropwisely add the acetic acid when 40-60% sodium cyanide aqueous solution is dropwisely added in the reactor, continuing the reaction at below 0 DEG C for 1-2 hours, filtering, and centrifugalizing to obtain the aminoacetonitrile; and (2) mixing the aminoacetonitrile with hydrogen chloride methanol solution, reacting at 45-50 DEG C for 1-2 hours, cooling to below 5 DEG C, filtering, and centrifugalizing to obtain the aminoacetonitrile hydrochloride, wherein in the hydrogen chloride methanol solution, the content of hydrogen chloride is 30-50 wt%, and the water content is less than or equal to 1%. According to the method provided by the invention, the total yield of the target product is high, and the operation is simple.

Description

technical field [0001] The invention relates to a preparation method of aminoacetonitrile hydrochloride. Background technique [0002] In the prior art, aminoacetonitrile hydrochloride is usually obtained by reacting aminoacetonitrile with hydrochloric acid, and the salt-forming yield of aminoacetonitrile hydrochloride is not high. [0003] In addition, the existing method of synthesizing aminoacetonitrile mainly contains following several kinds: [0004] Sodium cyanide method: use amine, sodium cyanide, formaldehyde, react and synthesize in the presence of magnesium salts such as magnesium chloride or magnesium hydrochloride; [0005] Liquid hydrocyanic acid method: use amine, formaldehyde, and liquid hydrocyanic acid as raw materials, add formaldehyde and hydrocyanic acid dropwise at the same time, react, extract and crystallize to obtain aminoacetonitrile, with a yield of 80-95% and a content of 92-98%; [0006] Hydroxyacetonitrile method: Use hydrocyanic acid and forma...

Claims

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Application Information

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IPC IPC(8): C07C255/25C07C253/30C07C253/00
Inventor 吴健明
Owner 太仓市茜泾化工有限公司
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