Abstract:

The main method to produce vat red 14，a kind of vat dye，is through the reaction of naphthalenetetracarboxylic acid and o-phenylenediamine with the presence of catalyst. There exist two isomers of vat red 14，the trans-structure is named orange 7 and the cis-structure is named vat red 15. The investigations of microwave heating in the synthesis of vat red 14 were carried out，and the effects of different temperatures（130—160 ℃），reaction times （5—40 min），and heating rates were discussed. It was found that temperature，reaction time and heating rate were the key factors determining the reaction products. Cis-product decreased with increasing temperature，and long reaction time favored trans-product. Trans-product could reach as high as 61% at temperature of 160 ℃ and reaction time of 40 min. It was also found that pre-synthesis at 60—100 ℃ favored the formation of the trans-product.

摘要：

还原红14是一种重要的还原染料，由橙7和还原红15两种互为正反异构体的物质组成，主要由萘四甲酸和邻苯二胺反应生成。本文研究了在微波场存在下萘四甲酸与邻苯二胺的合成反应，分别考察了反应温度（130～160 ℃）、反应时间（5～40 min）、加热方式对产物组成的影响。结果表明：基于微波与极性物质分子的相互作用，反应温度和时间及加热速率对产品组成影响较大，且温度越高，生成的反式产物越高。反应温度160 ℃、反应时间40 min时，反式产物含量达到最大值61%。延长反应时间有利于反式产物的生成。反应温度在60～100 ℃的预缩合反应有利于反式产物的生成。