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Preparation method of mandelonitrile

A technology of mandelonitrile and sodium cyanide, which is applied in the chemical industry, can solve the problems of difficult storage and poor transportation of raw materials, and achieve the effects of less impurities, recyclable solvents, and easy availability of raw materials

Inactive Publication Date: 2021-02-09
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If liquid hydrocyanic acid is used, the raw materials are not easy to transport and store

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The present embodiment provides a kind of preparation method of mandelonitrile, comprising the following steps:

[0022] Mix 426g of benzaldehyde and 500ml of ethyl acetate evenly, control the temperature of 640g of 30% sodium cyanide aqueous solution at 5°C-10°C, and add hydrochloric acid to adjust the pH to 6.88. Slowly add the prepared benzaldehyde ethyl acetate solution to the stirred sodium cyanide aqueous solution at a temperature of 10°C-20°C. After the addition is completed, control the 16°C heat preservation reaction for two hours, stop stirring, and let stand to separate. layer, after the upper layer was concentrated and recovered the solvent, 538g of product was obtained, and the mandelonitrile of content 98.2%. Based on the added benzaldehyde, the reaction yield was 99.8%.

Embodiment 2

[0024] The present embodiment provides a kind of preparation method of mandelonitrile, comprising the following steps:

[0025] Mix 426.5g of benzaldehyde and 500ml of ethyl acetate evenly, control the temperature of 640g of 30% sodium cyanide aqueous solution at 5°C-10°C and add hydrochloric acid to adjust the pH to 6.92. Slowly add the prepared benzaldehyde ethyl acetate solution to the stirred sodium cyanide aqueous solution at a temperature of 10°C-20°C. After the addition is completed, control the 18°C ​​heat preservation reaction for two hours, stop stirring, and let stand to separate. layer, after the upper layer was concentrated and recovered the solvent, 541g of product was obtained, and the mandelonitrile with a content of 98.0% was obtained. Based on the added benzaldehyde, the reaction yield was 99.9%.

Embodiment 3

[0027] The present embodiment provides a kind of preparation method of mandelonitrile, comprising the following steps:

[0028] Mix 426g of benzaldehyde and 400ml of ethyl acetate evenly, control the temperature of 640g of 30% sodium cyanide aqueous solution at 5°C-10°C, and add hydrochloric acid to adjust the pH to 6.96. Slowly add the prepared benzaldehyde ethyl acetate solution to the stirred sodium cyanide aqueous solution at a temperature of 10°C-20°C. After the addition is completed, control the 16°C heat preservation reaction for three hours, stop stirring, and let stand to separate. layer, after the upper layer was concentrated and recovered the solvent, 536g of product was obtained, and the mandelonitrile with a content of 98.0% was obtained. Based on the added benzaldehyde, the reaction yield was 99.7%.

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PUM

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Abstract

The invention discloses a preparation method of mandelonitrile, which comprises the following steps: dissolving benzaldehyde in ethyl acetate, stirring with a sodium cyanide water solution with the pHvalue regulated by hydrochloric acid to react, standing for layering after the reaction is finished, and recovering ethyl acetate from the upper layer to obtain mandelonitrile. The method provided bythe invention has the characteristics and advantages of easily available raw materials, environment-friendly and safe reaction conditions, short reaction time, recyclable solvent, simple steps, highproduct yield, high purity and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of mandelonitrile. Background technique [0002] Mandelonitrile, also known as almond nitrile and mandelonitrile, is a light yellow transparent oily liquid; soluble in ethanol, ether, and chloroform, but almost insoluble in water; it decomposes into hydrocyanic acid and benzaldehyde when heated. Mainly used in medicine, pesticide, dyestuff and other industries. [0003] The demand for mandelonitrile in domestic and foreign markets is very large, and the production capacity is also increasing year by year. Mandelonitrile can be obtained by direct addition of benzaldehyde and sodium cyanide, but this method is carried out under alkaline conditions, so there are many side reactions, the product is impure, and the yield is low. There are also patent literature reports that benzaldehyde and hydrocyanic acid are used as raw materials, and al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/36C07C253/00C07C253/34
CPCC07C253/00C07C253/34C07C255/36
Inventor 蔡奇峰徐帝邹德友段小瑞汪洪湖
Owner 安徽泰格生物科技有限公司
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