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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

Inactive Publication Date: 2021-04-30
SHANDONG TIANAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods must use high temperature and high pressure, which requires large equipment investment and high requirements, especially the gas phase reaction, which produces highly toxic cyanide gas, chlorine gas, hydrogen cyanide, etc., and the environmental protection problem is difficult to solve
[0006] Therefore, to develop a new synthesis process of malononitrile to overcome the problems of high cost, large amount of solid waste and difficult treatment of phosphorus-containing wastewater in the prior art is an urgent problem in this area.

Method used

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  • Preparation method of malononitrile and malononitrile prepared by preparation method
  • Preparation method of malononitrile and malononitrile prepared by preparation method
  • Preparation method of malononitrile and malononitrile prepared by preparation method

Examples

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Effect test

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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Abstract

The invention relates to the technical field of chemical synthesis methods, particularly to a malononitrile preparation method and malononitrile prepared thereof. The malononitrile preparation method comprises the following steps: mixing cyanoacetamide, a catalyst and a solvent, heating, refluxing, and introducing phosgene to synthesize malononitrile, wherein the mass ratio of the cyanoacetamide to the catalyst to the solvent is (2.5-3.5):(0.005-0.02):(7.5-10.5), the solvent is any one of dichloromethane, dichloroethane or methylbenzene, and the catalyst is any one or more of diethylamine, N,N-dimethylformamide or pyridine. According to the invention, cyanoacetamide is adopted to synthesize malononitrile in one step under the action of phosgene, wherein the required raw materials are cheap and easy to obtain, the synthetic reaction steps are few, harsh conditions are avoided, the operation is simple, stable and good in controllability, and the yield of the prepared malononitrile can reach 93% or above and is far higher than that of malononitrile obtained through other process schemes; and the preparation method is low in three-waste treatment cost, and has objective economic benefit.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis methods, in particular to a method for preparing malononitrile and the prepared malononitrile. Background technique [0002] Malononitrile is an important raw material for organic synthesis. There are two cyano functional groups in the malononitrile molecule, and the cyano group is a strong polar group with strong electron-withdrawing properties. Due to the action of the two cyano groups, the electron cloud of the malononitrile molecule transfers to the nitrogen atom on the cyano group, so that the two hydrogen atoms on the methylene group in the malononitrile molecule are also quite active. Since both cyano and methylene groups can react, malononitrile is a chemically very active compound that can undergo a series of reactions such as addition, condensation, substitution, cyclization, and polymerization to synthesize a series of important chemical products. The following is the struc...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/04
CPCC07C253/20C07C255/04
Inventor 夏有辉张杰朱巧根崔红建
Owner SHANDONG TIANAN CHEM
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