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商 辉,路冉冉,陈 玉
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SHANG Hui,LU Ranran,CHEN Yu
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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。
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.
商 辉,路冉冉,陈 玉. 微波促进萘四甲酸与邻苯二胺的合成反应 [J]. CIESC Journal.
SHANG Hui,LU Ranran,CHEN Yu. Microwave-assisted synthesis of naphthalenetetracarboxylic acid and o-phenylenediamine[J]. .
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https://hgxb.cip.com.cn/CN/Y2011/V30/I8/1832