室温湿气固化硅树脂的制备
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摘要
以甲基苯基二甲氧基硅烷、二甲基二甲氧基硅烷、甲基三甲氧基硅烷、苯基三甲氧基硅烷为原料,在酸性环境中水解共缩合制备了预聚硅树脂,再对硅树脂进行烷氧基封端,合成了可室温湿气固化的甲基苯基硅树脂。研究了烷基与硅原子的量之比(R/Si比)、苯基含量和固化剂用量对硅树脂涂料及固化膜性能的影响。较佳的合成条件为:R/Si比为1.3、苯基摩尔分数为40%、钛酸四丁酯用量为1%,该条件下制得的硅树脂Mn为2 563 g/mol、Mw为6 124 g/mol,室温密闭贮存7 d,能在室温湿气条件下固化,并在冷轧钢板表面形成透明坚硬的耐腐蚀涂层,硅树脂膜的铅笔硬度为4 H,附着力为0级。
Using dimethoxymethylphenylsilane,dimethyldimethoxysilane,methyltrimethoxysilane(MTMOS),and phenyltrimethoxysilane as the raw materials,the presilicone resin was prepared by hydrolysis co-condensation in acidic environment,and then terminated by alkoxy in the presence of the catalyst,the room temperature moisture methyl phenyl silicone resin was synthesized.The influence of molar ratio of R/Si,phenyl content and the amount of curing agent on the coating performance of the silicone resin coating and its film were investigated.The preferred experimental conditions are as follows:the molar ratio of R/Si is 1.3,and the mole fraction of phenyl is 40%,and the amount of tetrabutyltitanate is 1%.Thus the number-average molecular weight of silicone resin is 2 563 g/mol and the weight-average molecular weight of silicone resin is 6 124 g/mol,storage at room temperature for 7 days,and it can be cured at room temperature in humidity.The silicone resin coating on cold-rolled steel plate is transparent and corrosion resistant,the pencil hardness of cured silicone resin coating is 4 H,the adhesion of the films reaches level 0.
Using dimethoxymethylphenylsilane,dimethyldimethoxysilane,methyltrimethoxysilane(MTMOS),and phenyltrimethoxysilane as the raw materials,the presilicone resin was prepared by hydrolysis co-condensation in acidic environment,and then terminated by alkoxy in the presence of the catalyst,the room temperature moisture methyl phenyl silicone resin was synthesized.The influence of molar ratio of R/Si,phenyl content and the amount of curing agent on the coating performance of the silicone resin coating and its film were investigated.The preferred experimental conditions are as follows:the molar ratio of R/Si is 1.3,and the mole fraction of phenyl is 40%,and the amount of tetrabutyltitanate is 1%.Thus the number-average molecular weight of silicone resin is 2 563 g/mol and the weight-average molecular weight of silicone resin is 6 124 g/mol,storage at room temperature for 7 days,and it can be cured at room temperature in humidity.The silicone resin coating on cold-rolled steel plate is transparent and corrosion resistant,the pencil hardness of cured silicone resin coating is 4 H,the adhesion of the films reaches level 0.
引文
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[2]冯圣玉,张洁,李美江,等.有机硅高分子及其应用[M].北京:化学工业出版社,2004:151.
[3]幸松民,王一璐.有机硅合成工艺及产品应用[M].北京:化学工业出版社,2000:717.
[4]彭华龙,尤小姿,徐晓明,等.甲基苯基硅树脂的合成工艺研究[J].绝缘材料,2011,44(4):16-19.
[5]高大海,贾梦秋,吴超波,等.甲基苯基硅树脂合成新工艺[J].热固性树脂,2009,24(1):1-4.
[6]黎春阳,李国军,樊欣,等.耐高温甲基苯基硅树脂的合成[J].有机硅材料,2016,30(1):5-10.
[7]周文君,杨辉.甲基苯基硅树脂的制备工艺优化及阻燃性能[J].化工学报,2006,57(9):2218-2222.
[8]DING L P,SONG R J,LI B.An easy-to-obtain silicone-containing flame retardant and its effects on the combustion of polycarbonate[J].J Appl Polym Sci,2012,126(5):1489-1496.
[9]WEI P,TIAN G H,YU H Z,et al.Synthesis of a novel organic-inorganic hybrid mesoperous silica and its flame retardancy application in PC/ABS[J].Polym Degrad Stab,2013,98(2):1022-1029.
[10]YANG S N,LV G P,LIU Y,et al.Synergism of polysiloxane and zinc borate flame retardant polycarbonate[J].Polym Degrad Stab,2013,98(10):2795-2800.
[11]AKIO N,TOSHITAKA K.Flame retardancy of polycarbonate-polydimethylsiloxane block copolymer/silica nanocomposites[J].J Appl Polym Sci,2006,101(11):3862-3868.