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作 者:龚红升[1,2] 胡文斌[1,2] 廖列文[1] 张蔚欣 刘其海[1] 胡国栋[2]
机构地区:[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
出 处:《化工学报》2015年第6期2181-2188,共8页CIESC Journal
基 金: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)~~
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(MDHM)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18.417m N·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p H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。Synthesis of non-ionic polyether modified trisiloxanes surfactant(NTS) from MDHM 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 m N·m-1) repeated three times was obtained, being in agreement with the predicted value(18.177 m N·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 p H 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.
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