磷酸酯型氟硅表面活性剂的合成及表面活性

Synthesis and surface activity of phosphate ester type fluorosilicone surfactants

苯作溶剂,H_2PtCl_6作催化剂,原料含氢氟硅油(FPHMS)和烯丙基端羟基聚氧乙烯醚(FAE-10)经硅氢加成反应先制得中间体端羟基聚醚改性氟硅油(THPEFS),再将THPEFS与磷酸进行酯化反应合成了一种磷酸酯型氟硅表面活性剂(PFSS).PFSS酯化反应条件用正交试验进行了优化,其结构用红外光谱(IR)进行了确认,并对PFSS的临界表面张力(γcmc)、临界胶束浓度(cmc)、硬水中的稳定性、发泡性能、乳化力及耐酸耐碱耐盐性等进行了试验研究.结果表明:PFSS酯化反应的优化条件为:反应温度70℃、反应时间6h、n(THPEFS)∶n(H_3PO_4)=1∶1.1.PFSS水溶液的γcmc为28.4mN·m^(-1),cmc为0.2g·L^(-1).PFSS在硬水中的稳定性达5级,质量分数为0.5%的PFSS水溶液的发泡力为2.20,5 min的稳泡性为0.667,对煤油、环己烷和苯的乳化力分别是40s、113s和1 530s,并具有很好的耐酸耐碱耐盐等化学稳定性.

Benzene as the solvent,Hydroxyl-terminated polyether fluorosilicone oil(THPEFS)was prepared by hydrosilylation of hydrogen-containing fluorine-containing polysiloxane(FPHMS)with Allyl polyoxyethylene ether(FAE-10)in the presence of chloroplatinic acid catalyst.A kind of novel phosphate ester type fluorosilicone surfactants(PFSS)was synthesized by the esterification reaction of THPEFS with phosphoric acid.The esterification reaction conditions of PFSS synthesis were optimized using orthogonal test.The chemical structure of PFSS was characterized by IR.The properties of PFSS,such as critical micelle concentration,surface tension,stability in hard water,foaming property,emulsifying ability and so on resistance to acid,alkali and salt were investigated.Experimental results were showed as follows.Optimum conditions of the esterification reaction for the PFSS are that reaction temperature is 70 ℃,reaction time is 6 h,n(THPEFS)∶n(H_3PO_4)= 1∶1.1.And theγcmc of PFSS solution is 28.4mN/m,cmc of PFSS solution is 0.2g/L.The stability of PFSS in hard water is grade 5.The foaming power of 0.5% PFSS(mass fraction)solution is 2.20 and foam stability after 5 min is 0.667.The emulsifying ability of 0.5% PFSS solution for kerosene,cyclohexane and benzene are 40 s、113 s and 1 530 s,respectively.The PFSS solution has excellent chemical stability of acid-resisting,alkali-resisting and salt-resisting.