颜料红146的全溶液物料连续偶合工艺研究

摘要偶氮颜料的连续合成工艺契合重点基础材料产品的绿色高效低碳生产战略目标需求,然而堵塞问题却一直限制了偶氮颜料连续合成工艺的工业化生产应用。以颜料红146为研究对象,评估使用全溶液反应物料实现偶氮颜料的连续合成工艺的可行性,期望通过全溶液物料进料来彻底解决堵塞问题。在聚乙二醇的助溶作用下以水为溶剂,原料色酚 AS-LC可以获得澄清的碱性水溶液。以管微碰撞式混合器进行偶合反应,采用强酸性红色基KD重氮盐溶液和强碱性色酚AS-LC溶液进料,利用强酸碱溶液反应快于偶合反应的优势,通过调节AS-LC溶液的碱性调控偶合反应pH值,实现了颜料红146的连续偶合合成。优化了反应出口pH值、聚乙二醇体积分数、进料流量、后处理温度等条件,控制偶合剂溶液中聚乙二醇体积分数=10%、偶合反应出口pH=6、进料流量60 L·h^-1、后处理温度85 ℃的条件下连续化合成的颜料红146样品,偶合反应收率能达到95.04%,所得样品与标准样品色光ΔE<1,粒径明显小于间歇法。全溶液物料的连续偶合反应不仅有效提升了反应收率,而且降低了能耗,同时有效解决了反应器堵塞的问题,实现了高效安全的偶合反应。

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	童立音
	周雪琴
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	刘东志
	李巍
	陈勇

关键词：微反应器微通道合成偶氮颜料连续化工艺偶合反应

Abstract： The continuous synthetic process of azo pigments satisfies the national strategic needs of producing important basic materials in a green, low-carbon and efficient way. However, the blockage in the pipeline and reactor limits industrial production and application of continuous synthetic process. This work investigates the continuous-flow azo-coupling process of C.I. Pigment Red 146 to evaluate the feasibility of azo pigment continuous synthetic process with all inputs dissolved, in an attempt to tackling the blockage issue. Using polyethylene glycol (PEG) as a hydrotrope, the reagent N-(4-chloro-2,5-dimethoxyphenyl)-3-hydroxy-2-naphthalene amide (Naphthol AS-LC) in water exhibits as a clear solution. The continuous coupling reaction is conducted by addition of strongly acidic diazonium salt and strongly basic Naphthol AS-LC solution into a tubular colliding micromixer, which takes the advantage of faster acid-base neutralization than coupling reaction, so that the continuous coupling process of C.I. Pigment Red 146 can be achieved by the regulation of pH of the reaction mixture via the basicity of Naphthol AS-LC solution. The processing conditions, including pH of reactor outlet, volume fraction of PEG, input flow rate and post-treatment temperature were fully optimized. The azo-coupling reaction yield reaches up to 95.04% by setting the aforementioned parameters as pH=6, 10%, 60 L·h^-1 and 85 ℃, respectively. The color property (ΔE) of the products is less than 1 compared with standard sample, and the particle sizes are significantly smaller than those obtained by batch process. The continuous-flow azo-coupling reaction of C.I. Pigment Red 146 with all inputs dissolved promotes the yield of pigment, reduces energy consumption and more importantly, avoids the blockage, realizing efficient and safe azo-coupling reaction.

Keywords： microreactor microchannels synthesis azo pigments continuous-flow process azo-coupling reaction

Received 2023-03-02;

Fund:国家重点研发计划(2017YFB0307403)。

Corresponding Authors: 李巍,副教授,E-mail:liwei2008@tju.edu.cn。 Email: liwei2008@tju.edu.cn

About author: 童立音(1997—),男,硕士研究生,主要研究方向为颜料连续化合成。

引用本文:

童立音, 周雪琴, 徐珍香, 刘东志, 李巍, 陈勇.颜料红146的全溶液物料连续偶合工艺研究[J]. 化学工业与工程, 2024,41(6): 34-41

TONG Liyin, ZHOU Xueqin, XU Zhenxiang, LIU Dongzhi, LI Wei, CHEN Yong.Continuous-flow azo-coupling reaction of C.I. Pigment Red 146 with all inputs are solution[J]. Chemcial Industry and Engineering, 2024,41(6): 34-41

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