Method for synthesizing cyanobenzene by recycling and reusing byproducts of benzotripolycyanamide

A technology of benzomelamine and benzonitrile is applied in the field of recycling and reusing benzonitrile by-products to synthesize benzonitrile, which can solve the problems of large amount of benzomelamine sewage and high wastewater treatment costs, and achieve the reduction of types and COD, Realize the effect of recycling and simple reaction process

Active Publication Date: 2021-10-29
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The dissolved organic matter in the wastewater is finally discharged to the sewage treatment station for harmless treatment after the washing process, resulting in a huge amount of benzomelamine sewage and high wastewater treatment costs

Method used

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  • Method for synthesizing cyanobenzene by recycling and reusing byproducts of benzotripolycyanamide
  • Method for synthesizing cyanobenzene by recycling and reusing byproducts of benzotripolycyanamide
  • Method for synthesizing cyanobenzene by recycling and reusing byproducts of benzotripolycyanamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A kind of method that benzomelamine by-product recovery reuses synthetic benzonitrile comprises the steps:

[0040] S1, add 140g benzomelamine by-product (contain about 42g 2,4,6-triphenyl-1,3,5-triazine and 52g benzamide) in reaction container, then add 500mL butanol, 25g hydrochloric acid , 15g of acetic acid and 1.4g of nickel chloride catalyst, heated to 100°C and reacted for 5 hours. After the raw materials were completely acidolyzed, butanol and water were removed under reduced pressure; the reaction materials continued to heat up to 150°C and stirred for 15 hours until the reaction was complete Crude distillation under reduced pressure, collecting the distilled fractions to obtain the crude product of benzonitrile reaction;

[0041] S2, the described benzonitrile reaction crude product that step S1 obtains is transferred in the crude distillation tower, and vacuum distillation collects tower top product and obtains benzonitrile crude product 86.8g (gas phase cont...

Embodiment 2-7

[0048] A kind of benzomelamine by-product recycling method that embodiment 2-7 provides is reused to synthesize benzonitrile, compared with embodiment 1, the difference is that the benzomelamine by-product described in step S1 and hydrochloric acid, acetic acid The quality ratio is shown in Table 1. Except for the above differences, other operations are roughly the same and will not be repeated here. The specific experimental conditions, parameters and measurement results are shown in Table 1.

[0049] As can be seen from the results in Table 1, changing the ratio of 2,4,6-triphenyl-1,3,5-triazine, benzamide to hydrochloric acid and acetic acid in step S1 will affect the obtained benzonitrile The mass yield and purity of the product have a significant impact. When using hydrochloric acid or acetic acid alone, benzonitrile can also be obtained by acid hydrolysis, but the mass yield and purity are low. The present invention uses the mixed acid of hydrochloric acid and acetic a...

Embodiment 8-10

[0054] A kind of method that embodiment 8-10 provides a kind of benzomelamine by-product recovery and reuse synthesis benzonitrile, compared with embodiment 1, the difference is that in step S1, change 2,4,6-triphenyl- The mass ratio of 1,3,5-triazine to nickel chloride, except for the above differences, other operations are roughly the same, and will not be repeated here. The specific experimental conditions, parameters and measurement results are shown in Table 2.

[0055] Preparation conditions and experimental result parameters of table 2 embodiment 1,8-10

[0056]

[0057]

[0058] Comparative example 1 and embodiment 8-10 result can know, along with the increase of transition metal nickel catalyst consumption, the mass yield and the purity of benzonitrile after the reaction present the trend that first increases and then decreases, when the benzomelamine of recovery When the consumption ratio of by-product and nickel chloride is controlled in the scope of 1:(0.005...

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Abstract

The invention provides a method for synthesizing benzonitrile by recycling and reusing byproducts of benzotripolycyanamide, which is characterized in that the byproducts 2, 4, 6 triphenyl-1, 3, 5-triazine, benzamide and the like which are dissolved and recycled in washing water in the production process of the benzotripolycyanamide are used as main raw materials. Firstly, the 2, 4, 6-triphenyl-1, 3, 5-triazine is subjected to acidolysis to obtain benzamidine, benzoic acid and ammonia gas, and the benzoic acid and the ammonia gas generate ammonium benzoate on site; then benzamidine, ammonium benzoate, benzamide and other components are heated and dehydrated under the chelation of nickel chloride to generate benzonitrile; and finally, crude distillation and rectification are performed to obtain the high-purity benzonitrile. A plurality of byproducts and intermediates are converted into benzonitrile and high-boiling residues through ingenious design. According to the method, the treatment difficulty and cost of the wastewater in the production of the benzotripolycyanamide are remarkably reduced, and the economic effect is relatively high; and the whole reaction process is simple, the separation design of recovered effective components is reasonable, the conversion rate of recovered by-products is high, and the purity of synthesized benzonitrile is relatively high.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing benzonitrile by recycling benzomelamine by-products. Background technique [0002] Benzonitrile, also known as benzonitrile, is a colorless oily liquid with an almond-like smell. Slightly soluble in cold water, soluble in hot water, easily soluble in ethanol and ether, can be used as a solvent for nitrile rubber, resin, polymer and paint, etc., and benzonitrile is an important organic synthesis intermediate, mainly used for synthetic pesticides , veterinary drugs, fluorine-containing liquid crystal materials, aliphatic amines, benzoic acid and benzoic melamine and other advanced coating intermediates. With the wide application of advanced coatings such as benzomelamine, the gradual increase in the use of high-efficiency fluorine-containing pesticides, and the expansion of the market for high-end fluorine-containing liquid crystal materials, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C253/06C07C253/22C07C255/50
CPCC07C253/20C07C253/06C07C253/22C07C255/50Y02P20/584
Inventor 舒振操代飞程娟聂少春蔡峰朱明伟孙波黄正望
Owner WUHAN YOUJI IND
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