Page 31 - 201811

第 35 卷第 11 期 精 细 化 工 Vol.35, No.11
2018 年 11 月 FINE CHEMICALS Nov. 2018

功能材料
溶胶-凝胶法制备二氧化硅包覆水性 C.I.PR31

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曹瑞春 ，魏先福 1,2 ，王 琪 ，张 辉
（1. 南京林业大学 轻工与食品学院，江苏 南京 210037；2. 北京印刷学院 印刷与包装工程学院，北京
102600）

摘要：以 3-氨基-4-甲氧基苯甲酰苯胺（RBKD）和 3-羟基-N-(3-硝基苯基)-2-萘甲酰胺（NASBS）为中间
体，通过重氮化和偶合反应，制备了单偶氮红色系 C.I.PR31。偶合过程中首先选用松香酸对其进行水
性化改性处理，进而通过溶胶-凝胶法在颜料表面包覆了 1~3 层的 SiO 2 颗粒层。经接触角、SEM、TEM、
色光、热重分析测试，结果表明：经过松香酸处理的颜料样品晶体形貌可由长条状转变为圆片状，极
性明显增强。松香酸占总反应物质量的 3%时，颜料与水之间的接触角降至 52.8°，粒径分布峰值和粒径
分布宽度分别降至 78 nm 和 0.01~0.54 μm，具有较佳的亲水性能。包覆 2 层及 2 层以上的 SiO 2 可使颜料接触角
降至 0，完全转为亲水性。松香酸的加入在一定程度上会导致颜料色样偏向红色和蓝色，而 SiO 2 颗粒层则使
颜料偏向绿色和蓝色。包覆 2 层 SiO 2 的 C.I.PR31*-2SiO 2 色差（ ΔE）为 0.96，着色力可达 105.09%，氮气气氛
中加热至 290℃颜料晶体开始分解，达到了耐高温颜料的标准，可以用于水性分散介质。
关键词：C.I.PR31；松香酸；接触角；溶胶-凝胶法；热稳定性；流变性；功能材料
中图分类号：TQ625 文献标识码：A 文章编号：1003-5214 (2018) 11-1817-09

Synthesis of Silica DioxideCoated Waterborne C.I.P R 31 by Sol-gel Method

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CAO Rui-chun , WEI Xian-fu , WANG Qi , ZHANG Hui
（1. Nanjing Forestry University, Industry and Food institute, Nanjing 210037, Jiangsu, China; 2. Printing and
Packaging Engineering Institute, Beijing Institute of Graphic Communication, Beijing 102600, China）
Abstract: Monoazo C.I.PR31 was prepared using 3-amino-4-methoxybenzanilide (RBKD) and 3-hydroxyl
-N-(3-nitrophenyl)-2-naphthyl formamide (NASBS) as intermediates by diazotization and coupling reaction.
Rosin acid was used as surface modification agent of the pigment in the coupling process, then silica
dioxideparticleswith 1~3 layers were coated on the pigment surface by sol-gel method. The samples were
characterized by contact angle measurement, SEM, TEM, color capability and thermogravimetric analysis.
The results showed that after the pigment was treated by rosin acid, its crystal morphology changed from
long strip to disk shapes, and its polarity was obviously enhanced. When the amount of rosin acid was 3%
of the total mass of reactants, the contact angle between the obtained pigment and water was 52.8°, the
mean particle size and the particle size distribution were 78 nm and 0.01~0.54 μm, respectively, and the
pigment sample exhibited good hydrophilic property. The pigments coated with 2 layers and more than 2
layers of silicadioxide with contact angle values of 0° were completely hydrophilic. The introduction of
rosin acid made the pigment hues convert into red and blue, while that of the silicadioxide layer made the
pigment hues convert into green and blue.The color difference (ΔE) and tinting strength of the pigment
sample with 2 layers of silicadioxide, C.I.PR31*-2SiO 2, were 0.96 and 105.09%, respectively. In nitrogen
environment, the pigment crystals began to decompose at 290 ℃. It is obvious that the pigment reached
the standard of high temperature resistant pigment and could be used in aqueous dispersion system.
Key words: C.I.PR31; rosin acid; contact angle; sol-gel method; thermal stability; rheological property;
functional materials
Foundation items: National Natural Science Foundation of China (031105010); Open Fund of Jiangsu
Provincial Key Lab of Pulp and Paper Science and Technology (201534)

收稿日期：2018-01-09; 定用日期：2018-05-09; DOI: 10.13550/j.jxhg.20180026
基金项目：国家自然科学基金项目（031105010）；江苏省制浆造纸科学与技术重点实验室开放基金（201534）
作者简介：曹瑞春（1983—），女，讲师，博士。联系人：张 辉（1962—），男，教授、博士生导师，E-mail：zhnjfu@163.com。