Preparation method of malononitrile and malononitrile prepared by preparation method
A technology of malononitrile and distillation range, applied in the preparation of malononitrile and the field of malononitrile, can solve the problems of difficult phosphorus-containing wastewater treatment, large equipment investment, high cost, etc., and achieves low three waste treatment costs and reduced production. Cost and effect of fewer synthesis reaction steps
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Embodiment 1
[0057] S11, mix 300g cyanoacetamide, 3g pyridine and 900g dichloroethane, and stir evenly;
[0058] S12. When the temperature of the mixed system rises to 75°C, continue to feed phosgene at a rate of 10L / h, reflux for 10h, take out part of the feed liquid, cool to 40°C, and observe that no crystals are precipitated, that is, it is judged that the reaction is over;
[0059] S13. After the reflux reaction is completed, when the temperature of the mixed system is lowered to 60° C., nitrogen gas is continuously introduced at a rate of 10 L / h to evacuate the phosgene to obtain a feed liquid containing malononitrile;
[0060] S14. Distill the feed liquid at atmospheric pressure, remove the distillation gas with a distillation range below 110° C. to obtain a crude malononitrile product with a distillation range greater than 110° C., and distill the crude malononitrile under a vacuum of -0.097 MPa under reduced pressure, Remove fractions with a distillation range below 95°C and collec...
Embodiment 2
[0062] S21. Mix 250g cyanoacetamide, 2g pyridine and 700g dichloroethane, and stir evenly;
[0063] S22. When the temperature of the mixed system is raised to 70°C, continue to feed phosgene at a rate of 15L / h, reflux for 15h, take out part of the feed liquid, cool to 40°C, and observe that no crystals are precipitated, that is, it is judged that the reaction is complete;
[0064] S23. After the reflux reaction is completed, when the temperature of the mixed system is lowered to 60° C., nitrogen gas is continuously introduced at a rate of 15 L / h to evacuate the phosgene to obtain a feed liquid containing malononitrile;
[0065] S24. Distill the feed liquid at atmospheric pressure, remove the distillation gas with a distillation range below 110°C, obtain a crude malononitrile product with a distillation range greater than 110°C, and distill the crude malononitrile under a vacuum of -0.097MPa, Remove fractions with a distillation range below 95°C and collect fractions with a dis...
Embodiment 3
[0067] S31. Mix 350g cyanoacetamide, 4g pyridine and 1000g dichloroethane, and stir evenly;
[0068] S32. When the temperature of the mixed system is raised to 75°C, continue to feed phosgene at a rate of 15L / h, reflux for 15h, take out part of the feed liquid, cool to 40°C, and observe that there is no crystal precipitation, that is, it is judged that the reaction is over;
[0069] S33. After the reflux reaction is completed, when the temperature of the mixed system is lowered to 60° C., nitrogen gas is continuously introduced at a rate of 15 L / h to evacuate the phosgene to obtain a feed liquid containing malononitrile;
[0070] S34. Distill the feed liquid at atmospheric pressure, remove the distillation gas with a distillation range below 110° C. to obtain a crude malononitrile product with a distillation range greater than 110° C., and distill the crude malononitrile under a vacuum of -0.097 MPa, Remove fractions with a distillation range below 95°C and collect fractions w...
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