Green synthesis process of 4,4'-dinitrodiphenyl ether

Abstract

The invention discloses a green synthesis process of a 4,4'-dinitrodiphenyl ether. The sodium para-nitro phenolate and the p-nitrchlorobenzene are taken as raw materials to conduct a condensation reaction, a condensation material liquid obtained after the reaction is cooled, crystalized and centrifugally separated to obtain a crude product and a mother solution, the crude product is washed to obtain the high-purity 4,4'-dinitrodiphenyl ether, the mother solution is directly used in the following condensation reaction without being treated. The condensation product is obtained through a temperature and speed controlled cooling and crystalizing method, a solvent in the mother solution does not need to be distilled and recovered and is directly used, a 4,4'-dinitrodiphenyl ether crystal prepared through cooling and crystalizing is low in impurity content and good in color and luster; the process flow is simplified, the product purity and the yield of the product are increased, the energy is saved, and the emission is reduced.

Description

technical field [0001] The invention relates to the field of fine organic chemical synthesis, in particular to a green synthesis process of 4,4'-dinitrodiphenyl ether. Background technique [0002] 4,4'-dinitrodiphenyl ether is an important fine chemical product, it is a high value-added synthetic intermediate, and its reduction product 4,4'-diaminodiphenyl ether is used in the manufacture of special engineering materials The main monomer of polyimide and heat-resistant plastic polymaleimide resin. Due to the advantages of high temperature resistance, high mechanical strength and radiation resistance, polyimide special engineering materials are widely used in aerospace, microelectronics, nanometer, liquid crystal, separation and filtration membranes and other fields. With the continuous expansion of the application range, the demand for high-temperature resistant polyimide has become increasingly strong. Therefore, the research on the synthesis process of high-quality 4,4′-...

AI Technical Summary

Problems solved by technology

The main problem of the above-mentioned industrialized production process is that the process flow is tedious, especially the post-reaction treatment process is relatively loaded down with trivial details, one, the distillation recovery process of the solvent consumes a lot of energy, and about 10% of the solvent remains in the kettle and is difficult to recover completely. Solvent loss is obvious; Second, the amount of wastewater generated during the stripping and washing process is large, and the organic content in the wastewater is high and the composition is complex, which increases the cost of environmental protection treatment

Especially after the solvent is evaporated, the impurities produced in the reaction process are mixed with the crude diphenyl ether product, resulting in a large amount of water washing, generally requiring about 10 times the amount of water to wash the product, and the washing effect of the trace impurities is not good. , which also causes the impurity content in the diphenyl ether product to be high, which affects the purification of the subsequent hydrogenation product