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Method for preparing aminoacetonitrile sulfate

A technology of aminoacetonitrile sulfate and nitrile sulfate, which is applied in the field of preparation of aminoacetonitrile sulfate, can solve the problems of low yield, high cost, cumbersome operation, etc., and achieve the effect of high total yield and easy operation

Active Publication Date: 2014-09-10
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 The hydroxyacetonitrile method has long reaction steps, complicated 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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of preparation method of aminoacetonitrile sulfate: 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 140g of 35% sodium cyanide aqueous solution, and added dropwise to half, began to dropwise add 42g of acetic acid 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.

[0020] (2), make aminoacetonitrile and sulfuric acid methanol solution to react to generate aminoacetonitrile sulfate: 48g of aminoacetonitrile obtained in step (1), 726g of sulfuric acid methanol solution (the sulfuric acid content in the solution is 10%, and the moisture conte...

Embodiment 2

[0022] A kind of preparation method of aminoacetonitrile sulfate: 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), making aminoacetonitrile and sulfuric acid methanol solution react to generate aminoacetonitrile sulfate: 48g of aminoacetonitrile obtained in step (1) and 484g of sulfuric acid methanol solution (the sulfuric acid content in the solution is 15%, and the mois...

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Abstract

The invention relates to a preparation method of aminoacetonitrile sulfate, which comprises: (1) using ammonium chloride, formaldehyde, acetic acid and sodium cyanide as reaction raw materials to generate aminoacetonitrile through condensation reaction, the specific process is: Put ammonium chloride, formaldehyde and water into the mixture, stir evenly, cool to below 0°C, then add 30wt%~40wt% sodium cyanide aqueous solution dropwise, when the dropwise addition reaches 40%~60%, start to drop acetic acid at the same time, After the dropwise addition, continue the reaction below 0°C for 1-2 hours, filter, and centrifuge to obtain aminoacetonitrile; (2) react aminoacetonitrile and sulfuric acid methanol solution at a temperature of 30-35°C for 1-2 hours, and cool to 5 Below ℃, filter and centrifuge to obtain the aminoacetonitrile sulfate, wherein, in the methanol solution of sulfuric acid, the content of sulfuric acid is less than or equal to 15wt%, and the water content is less than or equal to 1%. According to the method of the invention, the total yield of the target product is high, and the operation is simple and convenient.

Description

technical field [0001] The invention relates to a preparation method of aminoacetonitrile sulfate. Background technique [0002] In the prior art, aminoacetonitrile sulfate is usually obtained by reacting aminoacetonitrile with sulfuric acid aqueous solution. Because aminoacetonitrile has a more active reaction property and sulfuric acid has oxidizing properties, the salt-forming rate of aminoacetonitrile sulfate 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 sulfate; [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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/25C07C253/30
Inventor 吴健明
Owner 太仓市茜泾化工有限公司