Preparation method of 4, 4 '-dinitrodiphenyl ether

• Main Authors: MENG TIANHAO, MEI XUE, WANG WENBIN, WANG QI, WANG HE, DU SHUMING
• Format: Patent
• Language: Chinese; English
• Published: 30.04.2021
• Subjects: ACYCLIC OR CARBOCYCLIC COMPOUNDS; CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY; CHEMISTRY; METALLURGY; ORGANIC CHEMISTRY; PERFORMING OPERATIONS; PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL; THEIR RELEVANT APPARATUS; TRANSPORTING

The invention provides a preparation method of 4, 4 '-dinitrodiphenyl ether, which comprises the following steps: carrying out etherification reaction on p-nitrohalobenzene and an organic salt assistant in a solvent under the catalysis of an ionic liquid to obtain a mixture; carrying out liquid separation on the mixture and carrying out regeneration treatment on subnatant obtained by liquid separation; and preparing 4, 4 '-dinitrodiphenyl ether by evaporative crystallization of a supernatant. According to the invention, the yield of the reaction is greatly increased and can reach 98.8% at most, byproducts are few in the reaction process, waste water, gas and solid are less in the reaction process, and pollution to the environment in the production process is effectively reduced. 本发明提供了一种4,4'-二硝基二苯醚的制备方法，包括：在离子液体催化下，将对硝基卤代苯、有机盐助剂置于溶剂中进行醚化反应得混合物；对混合物进行分液并对分液所得下层液进行再生处理；对分液得到的上层液进行蒸发结晶，制得4,4'-二硝基二苯醚，本发明大大提高了反应的产率，产率最高可达到98.8％，而且反应过程中副产物少、三废少，有效减少了生产过程中对环境的污染。