摘要
硼酸参与有机硅单体共缩聚,制备硼改性有机硅耐高温树脂。以聚合反应剩余乙氧基含量评价聚合反应程度,制备的耐热树脂在500℃1h高温下热失重率为评价标准,研究原料配比及制备工艺对产物耐高温性能的影响。结果表明,制备耐高温树脂的优化条件为:反应温度85℃,反应时间4h,水用量为完全水解所需用水量的50%,硼酸用量为树脂质量的13%,苯基与烷基质量比为0.4∶1。500℃高温实验表明,优化条件下制备的硼改性树脂失重率在1h内为12.2%。热重分析TG表明,树脂热解500℃前缓慢,500℃时热失重为8.5%,700℃时树脂热失重为17.0%,制备的树脂具有良好的耐高温性能。
Boric acid participated in the copolymerization of silicone monomer and prepared boron modified silicone high temperature resistant resin.The degree of polymerization was evaluated by the content of residual ethoxy group in the polymerization reaction.The thermogravimetric rate of the heat-resistant resin prepared at 500℃and 1 hour was used as the evaluation standard.The results showed that the optimum conditions for preparing high temperature resistant resin were as follows:reaction temperature was 85℃,reaction time was 4 h,water consumption was 50% of water consumption needed for complete hydrolysis,boric acid consumption was 13% of resin quality,and the mass ratio of phenyl to alkyl was 0.4∶1.The weightlessness rate of boron modified resin prepared under the optimized conditions was 12.16% within 1 hour.TG showed that the resin pyrolyzed slowly before 500℃and lost 8.5% at 500℃.The resin thermal weight loss was 17% at 700℃and the resin had good heat resistance.
引文
[1] Xu L.Organosilicon-mediated organic synthesis/organosi-licon chemistry[J].Current Organic Chemistry,2011,15(16):2742-2742.
[2] K.Indulekha,S.Monisha,R.S.Rajeev,et al.Polycyclic siloxanes:Base resins for novel high temperature resistant platinum curing transparent silicone adhesives[J].International Journal of Adhesion and Adhesives,2018,82:254-262.
[3] Wohl C J,Atkins B M,Belcher M A,et al.Synthesis,characterization,topographical modification,and surface properties of copoly(imide siloxane)s[J].High Performance Polymers,2012,24(1):40-49.
[4] Gupta P,Bajpai M.Development of siliconized epoxy resins and their application as anticorrosive coatings[J].Advances in Chemical Engineering&Science,2011,1:133-139.
[5] Wang C F,Huang F R,Jiang Y,et al.Oxidation behavior of carbon materials derived from a carborane-and silicon-incorporated polymer[J].Ceramics International,2012,38(4):3081-3088.
[6] 中国科学院化学研究所.耐紫外和高温老化的有机硅环氧树脂组合物:ZL200510130312.5[P],2007-06-13.
[7] 吴迪,郭丽.聚氨酯有机硅涂料的研制[J].中国涂料,2004,6(3):31-32.
[8] 鲁照玲.环氧有机硅树脂的合成及耐高温蒸汽防腐涂料的研究[D].湖北:武汉理工大学,2001.