聚醚改性有机硅表面活性剂的合成

SYNTHESIS OF POLYETHER MODIFIED ORGANIC SILICON SURFACTANT

实验以甲基二氯硅烷(CH_3SiHCl_2)、六甲基二硅氧烷(MM)、烯丙醇聚氧烷基醚(聚醚F6)为原料,氯铂酸-异丙醇为催化剂,经水解、催化平衡反应、硅氢加成反应,合成了聚醚改性有机硅表面活性剂——聚醚改性聚硅氧烷。讨论了原料配比、水解液种类、CH_3SiHCl_2滴加速度、反应时间及反应温度对收率和转化率的影响,实验结果表明,水解反应的适宜条件为:反应温度5℃,以NaHCO_3弱碱饱和溶液作为水解液,CH_3SiHCl_2滴加速率1滴/s;催化平衡反应的条件为:n(MM):n(CH_3SiHCl_2)=1.5:1,催化温度60℃,反应时间6h,低含氢硅油的总收率可达40.9%;硅氢加成反应的条件为:n(C=C):n(Si—H)=1.2:1.0,反应温度90℃,反应时间5h,硅氢转化率95.37%。常温下,0.5%(质量分数)的聚醚改性聚硅氧烷水溶液表面张力降至28.98mN/m。

The polyether modified polysiloxane, as silicone surfactant, was synthesized through hy- drolysis, catalytic equilibrium and hydrosilylation reactions, with methyl dichlorosilane （CH2SiHCl2）, hexamethyldisiloxane （MM） and aliyl alcohol polyoxyethylene alkyl ether （polyether F6） as raw materials. The catalysts were chloroplatinic acid and isopropanol. The influences of the raw materials ratio, hydrolysis species, CH2SiHCl2 addition rate, reaction time and reaction tempera- ture on the yield and the conversion ratio were researched. The structure of the product was charac- terized using infrared spectroscopy. The surface tension was measured. The results showed that the optimal conditions for the hydrolysis reaction were： one drop per second of CH2SiHCl2, reaction tem- perature 5 ℃, with saturated solution of NaHCO3. The catalytic equilibrium reaction conditions ）, 60 ℃ of the temperature and 6 h of the reaction time, and silicone oil was 40.9%. The hydrosilylation conditions were of the reaction temperature and 5 h of the reaction time. The were： 1.5 ： 1 of n（MM） ： n（CH3SiHC12 the total yield of the hydrogen containing 1.2 ： 1.0 of n（C--C） ： n（Si--H）, 90% Cconversion was 95.37%. The surface tension of the aqueous solution reduced to 28.98 mN/m when the mass fraction of the polyether modified polysiloxane was 0.5 %.