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
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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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