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Separation and purification method of hydroxyacetonitrile

A technology of hydroxyacetonitrile and purification method, which is applied in the direction of carboxylic acid nitrile purification/separation, organic chemistry, etc. It can solve the problems of low content of hydroxyacetonitrile, inability to remove hydroxyacetonitrile impurities, and large degree of decomposition and deterioration of hydroxyacetonitrile, so as to prevent and decompose Effect

Active Publication Date: 2017-05-10
HUAYANG NEW MATERIAL TECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, among the disclosed hydroxyacetonitrile purification methods, the most widely used method is vacuum distillation, but in this method, due to direct contact with air and high distillation temperature (about 100 ° C), hydroxyacetonitrile decomposes and deteriorates The degree is relatively large, so the content of the purified hydroxyacetonitrile is not high
Moreover, vacuum distillation cannot remove impurities in hydroxyacetonitrile

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A commercially available aqueous solution of hydroxyacetonitrile with a hydroxyacetonitrile content of 45% was used as a raw material, extracted three times with n-hexane and combined with the water phase, then contacted with the water phase with ether, combined with the organic phase after three extractions, the organic phase was composed of ether and hydroxyacetonitrile Mixture, use anhydrous magnesium sulfate to dry described organic phase, drying time is 6 hours, then use rotary evaporator to distill under reduced pressure at 30 ℃, pressure is 4.0kpa, remove diethyl ether, remaining liquid is transferred to Schlenk device , the air in the remaining liquid is replaced by a vacuum oil pump and nitrogen, and then the remaining liquid is heated and distilled in an oxygen-free low-pressure environment. At 0.2kpa, hydroxyacetonitrile flows out at 53-54°C. The measured purity of hydroxyacetonitrile is 96%, and the yield 88%, free CN - The content is 0.26%, which shows that...

Embodiment 2

[0038] A commercially available aqueous solution of hydroxyacetonitrile with a hydroxyacetonitrile content of 47% was used as a raw material, extracted three times with n-hexane and combined with the water phase, then contacted with the water phase with ether, combined with the organic phase after three extractions, the organic phase was composed of ether and hydroxyacetonitrile The mixture was dried with anhydrous magnesium sulfate for 5 hours, and then distilled under reduced pressure using a rotary evaporator at 28°C and a pressure of 4.0kpa to remove ether, and the remaining liquid was transferred to a Schlenk device , the air in the remaining liquid is replaced by a vacuum oil pump and nitrogen, and then the remaining liquid is heated and distilled in an oxygen-free low-pressure environment. At 0.2kpa, hydroxyacetonitrile flows out at 53-54°C. The measured purity of hydroxyacetonitrile is 95%, and the yield 86%, free CN - The content is 0.35%, which further shows that hyd...

Embodiment 3

[0040] A commercially available aqueous solution of hydroxyacetonitrile with a hydroxyacetonitrile content of 47% was used as a raw material, extracted three times with n-hexane and combined with the water phase, then contacted with the water phase with ether, combined with the organic phase after three extractions, the organic phase was composed of ether and hydroxyacetonitrile The mixture was dried with anhydrous magnesium sulfate for 6 hours, and then evaporated under reduced pressure using a rotary evaporator at 32°C and a pressure of 4.0kpa to remove ether, and the remaining liquid was transferred to a Schlenk device , the air in the remaining liquid is replaced by a vacuum oil pump and nitrogen, and then the remaining liquid is heated and distilled in an oxygen-free low-pressure environment. At 0.2kpa, hydroxyacetonitrile flows out at 53-54°C. The measured purity of hydroxyacetonitrile is 95%, and the yield 89%, free CN - The content is 0.27%, which further shows that hy...

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Abstract

The invention discloses a separation and purification method of hydroxyacetonitrile. The separation and purification method comprises the following steps: step a), using a first extraction agent to be in contact with a hydroxyacetonitrile water solution for extraction, and separating to obtain a first phase containing hydroxyacetonitrile and water and a second phase containing the first extraction agent and impurities; step b), using a second extraction agent to be in contact with the first phase for extraction, separating to obtain a third phase containing the second extraction agent and the hydroxyacetonitrile and a water phase; step c), using a drying agent to carry out drying treatment on the third phase; step d), separating the hydroxyacetonitrile from the third phase after drying treatment; and step e), carrying out purification treatment on the hydroxyacetonitrile obtained in the step d. Compared with the prior art, the first extraction agent is firstly used for separating the impurities from the hydroxyacetonitrile, then the second extraction agent is used for separating the hydroxyacetonitrile and water, and then drying and purification are carried out, so that the high-purity hydroxyacetonitrile can be obtained.

Description

technical field [0001] The invention relates to the field of separation and purification, in particular to a separation and purification method of hydroxyacetonitrile. Background technique [0002] Hydroxyacetonitrile, also known as glycolonitrile, has the chemical formula HOCH 2 CN, generally a colorless oily liquid, is a derivative of formaldehyde and hydrocyanic acid, and is also the simplest cyanohydrin. As the most important intermediate of cyanohydrin, hydroxyethanol is widely used in organic synthesis, drug synthesis, flotation, etching and many other fields. In the process of organic synthesis or pharmaceutical synthesis using hydroxyacetonitrile as a raw material, industrial hydroxyacetonitrile often contains a small amount of harmful impurities, which will affect the yield of synthetic products. Especially, when the reaction environment is an alkaline condition, the impurity in hydroxyacetonitrile will have a greater impact on the reaction. In mineral flotation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/34C07C255/16
CPCC07C253/34C07C255/16
Inventor 张伟龚文照赵广王向龙贾晨袁秋华冯志武
Owner HUAYANG NEW MATERIAL TECH GRP CO LTD
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