以氯铂酸为催化剂,聚甲基氢硅氧烷(PMHS)、N,N-二甲氨基丙烯酰胺(DMAA)单体为反应原料制备了氨基改性聚硅氧烷柔软剂,并且通过正交试验测得最佳方案为反应时间15h,反应温度110℃,催化剂用量50×10-6(相对于反应物的质量),物料比[n(含氢硅油):n(单体)]为1:1.2。且通过红外光谱对合成产物的结构进行了表征,同时,对氨基硅油整理前后的亚麻织物表面形态通过扫描电子显微镜表征。结果表明:氨基基团成功接枝到PMHS侧链上,被氨基硅油整理过的亚麻织物比亚麻原布表面更加光滑。
An amino-modified polysiloxane softener was prepared using chloroplatinic acid as a catalyst,polymethyl hydrogen siloxane (PMHS),and N,N-dimethylaminoacrylamide (DMAA) monomers as reaction raw materials.The best experimental scheme measured by the cross test was that reaction time 15h,reaction temperature 110℃,catalyst dosage 50×10-6(relative to the mass of the reactant),and the material ratio (n(hydrogen-containing silicone oil):n(monomer)) 1:1.2.The structure of the synthesized product was characterized by infrared spectroscopy.At the same time,the surface morphology of the linen fabric before and after amino silicone oil finishing was characterized by scanning electron microscopy (SEM).The results showed that the amino group was successfully grafted onto the PMHS side chain,and the surface of the linen fabric treated with amino silicone oil was smoother than the original linen fabric.
[1] 魏元博.纤维基多功能有机硅柔软剂的合成、表征及应用研究[D].西安:陕西科技大学,2015.
[2] Wei Y,Zheng C,Chen P,et al.Synthesis of multiblock linear polyether functional amino silicone softener and its modification of surface properties on cotton fabrics(article)[J].Polymer Bulletin,2019,76(1):447-467.
[3] 赵欣,孙晓泉,宋秘钊,等.丙烯酸二甲氨基乙酯改性含氢聚硅氧烷的合成与表征[J].印染助剂,2011,28(4):9-10.
[4] 李海楠,赵欣,刘琨.亚麻织物用新型氟硅油的合成及表征[J].上海纺织科技,2019(1):18-20.
[5] Zhou Quankai,Sun Xiaolong,Wang Bingshuai,et al.Synthesis and properties of silicone oil modified by amino polyether[J].Detergent & Cosmetics,2017,40(1):28-30,55.
[6] 王睿.氨基有机硅柔软剂与棉织物的易护理性[D].上海:东华大学,2012.
[7] 张立传,周学山,全凤玉,等.氨基硅油柔软剂的研究进展[J].合成纤维,2010(5):16-20.
[8] 庄宝璐,陆宁宁.水溶性氨基硅油的研制与应用研究[J].印染助剂,2003,20(5):10-12.
[9] 周煜华,杨静,葛利伟,等.有机硅柔软剂氨基硅油的研究进展[J].江西化工,2017(4):28-31.
[10] Winkler H J S,Gilman H.Preparation and reactions of sym-tetraphenyldisilane[J].The Journal of Organic Chemistry,1961,26(4):35-47.
[11] Fritz G,Burdt H.Eine quantitative bestimmung der SiH-und Si-phenyl-gruppe[J].Zeitschrift Fär Anorganische Und Allgemeine Chemie,2010,317(1-2):137-138.
