Preparation method of bis(p aminophenoxyl) alkane

Abstract

The invention discloses a preparation method of bis(p aminophenoxyl) alkane. The method comprises the following steps: (1) adding p-chloronitrobenzene, alkyl diol, phase-transfer catalyst and water into a reaction apparatus, stirring and heating to 85-95 DEG C; then dropping sodium hydroxide aqueous solution slowly and reacting for 15-16 h after dropping; (2) carrying out a post-treatment after the reaction to obtain bis(p nitrophenoxyl) alkane; (3) adding Pd / C catalyst, methanol and bis(p nitrophenoxyl) alkane into an autoclave and enclosing; displacing hydrogen for 2-5 times and reacting with stirring for 2-3 h under a pressure of 0.8-2 MPa and a temperature of 0-80 DEG C; (4) carrying out a post-treatment after the reaction to obtain the bis(p aminophenoxyl) alkane. Initial raw material employed by the invention are cheap, easily available and at low cost; a process is simple, with a high final yield and suitable for large scale production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a preparation method of bis(p-aminophenoxy)alkane. Background technique [0002] Bis(p-aminophenoxy)alkane is an important monomer used in the production of heat-resistant insulating polymer materials such as polyamide and polyimide. Its preparation method mainly contains following two kinds at present: [0003] Tetrahedron magazine Tetrahedron (2005 No. 61, page 5351-5362) discloses a kind of starting material with dibromoalkane and p-nitrophenol, in acetonitrile solvent, with anhydrous potassium carbonate as alkali, and potassium iodide as alkali Catalyst, react to prepare intermediate bis(p-nitrophenoxy)alkane; then carry out catalytic hydrogenation reduction on the intermediate to obtain bis(p-aminophenoxy)alkane. The disadvantage of this method is that the starting materials for the two reactions are expensive, and the reaction time is relatively long, resulting i...

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the starting materials for the two reactions are expensive, and the reaction time is long, which leads to relatively large production costs and is not suitable for large-scale production.

The disadvantage of this method is that alkyl glycol needs to undergo sulfonate reaction first, which leads to cumbersome process routes and more waste, and p-nitrophenol is expensive, resulting in high production costs and is not suitable for large-scale production. Production

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