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Preparation method of 4-chlorine-3-hydroxybutyronitrile

A technology of hydroxybutyronitrile and epichlorohydrin, applied in the preparation of cyanide reaction, organic chemistry, etc., can solve the problems of three wastes treatment difficulties, low yield of cyanide-containing wastewater, etc., and achieve favorable environmental protection, low cost, high conversion rate effect

Inactive Publication Date: 2008-08-06
四川省天然气化工研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] These methods all have the disadvantages of low yield and a large amount of cyanide-containing wastewater, and a large amount of sodium sulfate needs to be treated at the same time, and the treatment of the three wastes is relatively difficult.

Method used

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  • Preparation method of 4-chlorine-3-hydroxybutyronitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 500ml three-flask with a thermometer, a condenser, and an agitator, add 153.5 grams of epichlorohydrin (99% by mass), 120 grams of methanol, and 4.0 grams of trimethylamine. At a temperature of 60°C, slowly add The mass percentage is 47.2 grams of 98% hydrocyanic acid, and the time of dropping is 80 minutes, and the insulation reaction finishes in 400 minutes, and the pH value of the reaction solution adjusted with formic acid is weakly acidic (the pH value is between 5.5~6.5, the same below), and then The reaction solution was distilled under reduced pressure to remove 110 grams of light components (including solvent, unreacted epichlorohydrin, etc., the same below), wherein the mass percentage content of epichlorohydrin was 3%, to obtain 4-chloro-3- Hydroxybutyronitrile crude product 194 grams, analysis mass percent content is 94.7% (HPLC), it is transferred to rectifying column rectification, obtains target fraction 4-chloro-3-hydroxybutyronitrile 179.4 grams, ma...

Embodiment 2

[0027] Carry out the feeding operation according to Example 1, the difference is that 4.0 grams of trimethylamine is replaced by 3.0 grams of diisopropylamine, after the reaction is over, the pH value of the reaction solution is adjusted to be weakly acidic with formic acid, and the reaction solution is decompressed to distill out light components Divide 108 grams, wherein, the mass percent content of epichlorohydrin is 2%. Obtain 195.3 grams of 4-chloro-3-hydroxybutyronitrile crude product, and analysis mass percentage content is 95.2% (HPLC), transfers to rectifying column rectification and purification, obtains target cut 4-chloro-3-hydroxybutyronitrile 183.4 grams, The mass percentage content is 98.2% (HPLC), and the product yield is 93.06% based on epichlorohydrin. The residual liquid was incinerated.

Embodiment 3

[0029] Carry out the feeding operation according to Example 1, the difference is that 4.0 grams of trimethylamine are replaced by 4.0 grams of sodium acetate, after the reaction is over, the pH value of the reaction solution is adjusted to be weakly acidic with formic acid, and the light components are distilled out of the reaction solution under reduced pressure 98 grams, wherein the mass percentage content of epichlorohydrin is 3.3%. Obtain 192.8 grams of 4-chloro-3-hydroxybutyronitrile crude product, and analysis mass percentage content is 94.2% (HPLC), transfers to rectifying column rectification and purification, obtains target cut 4-chloro-3-hydroxybutyronitrile 177.7 grams, The mass percent content is 98.7% (HPLC), and the product yield is 91.28% based on epichlorohydrin. The residual liquid was incinerated.

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Abstract

The invention discloses a preparing method of 4-chloride-3-hydroxyl butyronitrile, which comprises the following steps: 1) blending epichlorohydrin and alkaline catalyst with molar rate at 1:1.0-1.5; adding 50-100% formonitrile to synthesize the product; 2) adjusting the reacting liquid to weak acid; distilling in the vacuum to obtain the product; recycling non-reacting epichlorohydrin.

Description

Technical field: [0001] The present invention relates to the preparation method of 4-chloro-3-hydroxybutyronitrile. Background technique: [0002] The existing methods for preparing 4-chloro-3-hydroxybutyronitrile mainly contain the following two methods, and these methods all have deficiencies. [0003] 1. Sodium cyanide method: [0004] In this method, epichlorohydrin is mixed with water, and then sodium cyanide aqueous solution is slowly added, and the pH value is constantly adjusted with sulfuric acid, so that the range of the pH value is accurately kept within the range of 8-10. Distillation and other post-processing processes to obtain the target product. [0005] 2. Hydrocyanic acid-sodium sulfate method: [0006] In this method, epichlorohydrin is mixed with saturated sodium sulfate aqueous solution, and the pH value is maintained in the range of 8-10, and reacted with hydrocyanic acid to obtain 4-chloro-3-hydroxybutyronitrile, and the reaction solution is heat-pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/12C07C253/16
Inventor 黄印马毅罗克俊王锋傅雪琴
Owner 四川省天然气化工研究院