Method for adopting melting crystallization technology to separate and purify succinonitrile
A technology of melting crystallization and purification method, which is applied in the direction of carboxylic acid nitrile purification/separation, organic chemistry, etc., can solve the problems of complex operation, high energy consumption, polymerization coking, etc., and achieves no influence on yield and quality, low operating temperature, The effect of high product purity
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Embodiment 1
[0023] Weigh 100.0 g of succinonitrile raw material, the purity of the crude succinonitrile is 99.81%, the content of light component impurities is 0.08%, and the content of heavy component impurities is 0.11%. Put the crude succinonitrile into a melting crystallizer, heat it to 59.0°C to fully dissolve, start the program to cool down to 52.0°C at a rate of 0.01°C / min, take out the bottom stopper after stabilizing for 180 minutes and release it as the crystallization mother liquor until the liquid is no longer Outflow; then start to heat up and sweat at a rate of 0.01°C / min to 55.0°C, and keep it for 10 minutes, then receive the sweat. Finally, the succinonitrile in the crystallizer is heated and dissolved to obtain the final product, the yield is about 40.1%, and the product purity reaches 99.96%.
Embodiment 2
[0025] Weigh 100.0 g of succinonitrile raw material, the purity of the crude succinonitrile is 99.81%, the content of light component impurities is 0.08%, and the content of heavy component impurities is 0.11%. Put the crude succinonitrile into a melting crystallizer, heat it to 59.0°C to fully dissolve, start the program to cool down to 51.0°C at a rate of 0.005°C / min, take out the bottom plug after stabilization for 120 minutes and release it as a crystallization mother liquor until the liquid is no longer Flow out; then start to heat up and sweat at a rate of 0.05°C / min to 56.0°C, and keep it for 30 minutes, then pick up the sweat. Finally, the succinonitrile in the crystallizer is heated and dissolved to obtain the final product, the yield is about 45.6%, and the product purity reaches 99.97%.
Embodiment 3
[0027] Weigh 100.0 g of succinonitrile raw material, the purity of the crude succinonitrile is 99.81%, the content of light component impurities is 0.08%, and the content of heavy component impurities is 0.11%. Put the crude succinonitrile into a melting crystallizer, heat it to 59.0°C to fully dissolve, start the program to cool down to 50.0°C at a rate of 0.008°C / min, take out the bottom stopper after 60 minutes of stabilization and release it as the crystallization mother liquor until the liquid is no longer Flow out; then start to heat up and sweat at a rate of 0.1°C / min to 57.0°C, and keep it for 60 minutes, then receive the sweat. Finally, the succinonitrile in the crystallizer is heated and dissolved to obtain the final product, the yield is about 45.6%, and the product purity reaches 99.97%.
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