非离子型聚醚改性三硅氧烷表面活性剂的合成表征及性能

doi:10.11949/j.issn.0438-1157.20141831

化工学报 ›› 2015, Vol. 66 ›› Issue (6): 2181-2188.DOI: 10.11949/j.issn.0438-1157.20141831

非离子型聚醚改性三硅氧烷表面活性剂的合成表征及性能

龚红升^1,2, 胡文斌^1,2, 廖列文¹, 张蔚欣¹, 刘其海¹, 胡国栋²

1. 仲恺农业工程学院绿色化工研究所, 广东广州 510225;
2. 中山大学惠州研究院, 广东惠州 516081

收稿日期:2014-12-11 修回日期:2015-02-12 出版日期:2015-06-05 发布日期:2015-03-25
通讯作者: 胡文斌
基金资助:
国家自然科学基金项目(21746272);广州市科技局(2014J4100011);惠州市重大项目(2013B050013014);韶关市重大科技项目(韶财教(2012)111号)。

Synthesis, characterization and properties of non-ionic polyether modified trisiloxanes surfactant

GONG Hongsheng^1,2, HU Wenbin^1,2, LIAO Liewen¹, ZHANG Weixin¹, LIU Qihai¹, HU Guodong²

1. Institute of Green Chemical Engineering, Zhongkai University of Agriculture and Engineering, Guangzhou 510225, Guangdong, China;
2. Huizhou Research Institute of Sun Yat-sen University, Huizhou 516081, Guangdong, China

Received:2014-12-11 Revised:2015-02-12 Online:2015-06-05 Published:2015-03-25
Supported by:
supported by National Natural Science Foundation of China(21746272), Science and Technology of Guangzhou (2014J4100011), Major Scientific and Technological Projects of Huizhou City and Major Scientific and Technological Projects of Shaoguan City(No.(2012)111).

摘要/Abstract

摘要：

选用EO(环氧乙烷ethylene oxide)链长为7~8, 平均相对分子质量为380的烯丙醇聚氧烷羟基醚(PE-38)和1,1,1,3,5,5,5-七甲基三硅氧烷(MD^HM)为原料, 通过无溶剂聚合, 在氮气保护下经Karstedt催化剂催化硅氢加成反应制备了非离子型聚醚改性三硅氧烷表面活性剂(NTS), 并通过傅里叶红外光谱仪和质子核磁共振仪验证了其结构。采用响应面法对合成工艺进行了优化, 确定了NTS的最佳合成条件为:n(C=C):n(Si—H)=0.93, 反应温度为94℃, 催化剂用量为6.4 mg·kg^-1, 在反应时间为2 h下, 经3次重复试验所得产品的平均表面张力为18.417 mN·m^-1, 与理论预测值基本相符。测试了产物NTS 0.1%(质量分数)的水溶液在pH为4、7和10的水溶液中的水解性能, 发现该产物在酸性和碱性条件下可稳定存放30 d左右, 在中性条件下可稳定存放60 d左右。

关键词: 非离子, 表面活性剂, 有机硅, 硅氢加成, 水解性能, 响应面法

Abstract:

Synthesis of non-ionic polyether modified trisiloxanes surfactant (NTS) from MD^HM and polyoxyethylene alkyl allyl ethers (PE-38) with average EO (ethylene oxide) chain length of 7—8 and average molecular weight of 380, was catalyzed by Karstedt catalyst under N₂ with no solvent. Its structure was verified by Fourier transform infrared spectroscopy and proton nuclear magnetic resonance. Synthesis of NTS was optimized by using the response surface methodology (RSM). The optimal conditions at which average surface tension (18.417 mN·m^-1) repeated three times was obtained, being in agreement with the predicted value (18.177 mN·m^-1), were as follows: reaction mass ratio of n(C=C):n(Si—H)=0.93, amount of catalyst 6.4 mg·kg^-1, and reaction temperature and time 94℃ and 2 h, respectively. Hydrolysis of the aqueous solution of NTS at pH 4, 7 and 10 also was studied, and the product under acidic and alkaline conditions was stable for about 30 d, while under neutral condition was stable for about 60 d.

Key words: non-ionic, surfactant, silicone, hydrosilylation, hydrolysis performance, response surface methodology

中图分类号:

TQ423.91

龚红升, 胡文斌, 廖列文, 张蔚欣, 刘其海, 胡国栋. 非离子型聚醚改性三硅氧烷表面活性剂的合成表征及性能[J]. 化工学报, 2015, 66(6): 2181-2188.

GONG Hongsheng, HU Wenbin, LIAO Liewen, ZHANG Weixin, LIU Qihai, HU Guodong. Synthesis, characterization and properties of non-ionic polyether modified trisiloxanes surfactant[J]. CIESC Journal, 2015, 66(6): 2181-2188.

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非离子型聚醚改性三硅氧烷表面活性剂的合成表征及性能

Synthesis, characterization and properties of non-ionic polyether modified trisiloxanes surfactant

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