颜料红146的连续化合成工艺

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摘要以3-氨基-4-甲氧基苯甲酰苯胺(红色基KD)为重氮组分、N-(4-氯-2,5-二甲氧苯基)-3-羟基-2-萘酰胺(色酚AS-LC)为偶合组分,利用管状微型混合器分别进行重氮化反应及偶合反应,优化了重氮化反应的反应温度与盐酸的用量以及偶合反应的反应温度与反应体系pH值。在反应温度为20℃、n(HCl)∶n(红色基KD)=2.5∶1.0的条件下连续化合成了颜料红146,总收率达到97.0%,色光ΔE<1,粒径明显小于间歇法。与间歇法相比,连续化工艺不仅提高了反应收率,而且降低了能耗与材料成本,提高了综合生产效率,具有广阔的工业化前景。

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	王旭东
	周雪琴
	童立音
	刘东志
	李巍

关键词：颜料红146 微型混合器连续化工艺重氮化反应偶合反应

Abstract： With 3-amino-4-methoxybenzanilide(Red base KD) as diazonium component, N-(4-chloro-2,5-dimethoxyphenyl)-3-hydroxy-2-naphthalene amide(Naphthol AS-LC) as azo-coupling component, the tubular micromixer was applied to carry out diazotization and azo-coupling reaction, respectively, for the continuous-flow synthesis process of Pigment Red 146. The temperature, the amount of hydrochloric acid of diazotization and the temperature, pH of azo-coupling reaction were optimized. As a result, continuous-flow synthesis process was carried out at 20 ℃, n(HCl)∶n(Red base KD)=2.5∶1.0, the yield of pigment reached 97.0%, color property ΔE<1, and particle size was significantly smaller than that of the batch process. Compared with batch process, continuous process not only increases the yield of pigment, but also reduces the energy consumption and material cost, improves production efficiency, so it has broad prospect for industrialization.

Keywords： Pigment Red 146 micromixer continuous-flow process diazotization azo-coupling reaction

Received 2021-04-03;

Fund:国家重点研发计划(2017YFB0307403)。

Corresponding Authors: 李巍,副研究员,E-mail:liwei2008@tju.edu.cn。 Email: liwei2008@tju.edu.cn

About author: 王旭东(1996-),男,硕士研究生,现从事有机颜料连续化合成方面的研究。

引用本文:

王旭东, 周雪琴, 童立音, 刘东志, 李巍.颜料红146的连续化合成工艺[J]. 化学工业与工程, 2022,39(4): 1-8

WANG Xudong, ZHOU Xueqin, TONG Liyin, LIU Dongzhi, LI Wei.Continuous-flow synthesis process of C.I. Pigment Red 146[J]. Chemcial Industry and Engineering, 2022,39(4): 1-8

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