耐撕裂高回弹加成型医用硅橡胶的研制  

Preparation of Additional Curing Medical Silicone Rubber with Tear-Resistant Strength and High Elastic Resilience

作　　者：杨磊 汪翠 张伟成 汪海风 邹磊磊 白玲 杜滨阳[2] YANG Lei;WANG Cui;ZHANG Weicheng;WANG Haifeng;ZOU Leilei;BAI Ling;DU Binyang(Zhejiang Zhongtian Dongfang Fluorosilicone Material Co.,Ltd.,Quzhou 324012,China;Department of Polymer Science and Engineering,Zhejiang University,Hangzhou 310027,China)

机构地区：[1]浙江中天东方氟硅材料股份有限公司,浙江衢州324012 [2]浙江大学高分子科学与工程学系,杭州310027

出　　处：《有机硅材料》2023年第5期14-19,共6页Silicone Material

基　　金：浙江省科技计划项目(2022C01109);衢州市科技计划项目(2022Z03)。

摘　　要：向八甲基环四硅氧烷(D_(4))中加入乙醇及少量冠醚,经凝固抽滤和精馏制得低金属杂质含量的高纯度D_(4),再经碱催化开环聚合及封端反应,分别使用乙烯基双封头和硅油封端剂制得低挥发分的乙烯基和甲基封端的甲基乙烯基硅橡胶。探讨了邵氏A硬度40和70两个硬度级别耐撕裂高回弹硅橡胶的较佳配方。结果表明,制备邵氏A硬度40硅橡胶的较佳配方为:85份乙烯基链节摩尔分数0.03%和15份乙烯基链节摩尔分数0.08%的110生胶作基础聚合物,31份比表面积380 m^(2)/g的气相法白炭黑作补强填料,添加5份羟基硅油、0.1份硬脂酸锌、3份112生胶,此时硅橡胶的邵氏A硬度为42,拉伸强度为11.0 MPa,拉断伸长率为980%,撕裂强度为38 kN/m,回弹率为74.8%,挥发分为0.8%,正己烷溶出物质量分数为1.5%,适用于生产导尿管负压球;制备邵氏A硬度70硅橡胶的较佳配方为:55份乙烯基链节摩尔分数0.08%和42份乙烯基链节摩尔分数0.23%的110生胶、3份112生胶作基础聚合物,42份比表面积380 m^(2)/g的气相法白炭黑作补强填料,添加8份羟基硅油、5份甲氧基硅油、0.1份硬脂酸锌、0.5份活性氢质量分数0.5%的含氢硅油、5份多乙烯基硅油,此时硅橡胶的邵氏A硬度为70,拉伸强度为8.1 MPa,拉断伸长率为540%,撕裂强度为46 kN/m,回弹率为71.5%,挥发分为1.2%,正己烷溶出物质量分数为1.6%,适用于生产导尿管、喉管、引流管等。A high-purity octamethylcyclotetrasiloxane(D_(4))with low metallic impurity was prepared by adding ethanol and a small amount of crown ether by solidification,filtration and distillation.After alkali catalyzed ring opening polymerization and end capping reaction,the low volatile vinyl and methyl terminated methyl vinyl silicone rubber were prepared with tetramethyldivinyldisiloxane and silicone oil as the end capping agents,respectively.The formula of silicone rubber(Shore A hardness 40 and 70)with high tear resistant and elastic resilience were discussed.The results show that the proper formula for silicone rubber with Shore A hardness 40 was that 85 phr of 110 polysiloxane with vinyl mole fraction of 0.03%,15 phr of 110 polysiloxane with vinyl mole of 0.08%,31 phr of fumed silica with 380 m^(2)/g,and 5 phr of hydroxyl silicone oil,0.1 phr of zinc stearate,and 3 phr of 112 polysiloxane with vinyl mole of 3%.The prepared silicone rubber showed Shore A hardness of 42,tensile strength of 11.0 MPa,elongation at break of 980%,tear strength of 38 kN/m,elastic resilience of 74.8%,volatile of 0.8%,and the mass fraction of n-hexane extracts of 1.5%,which was ideal for the production of Foley catheter negative pressure ball.The proper formula for silicone rubber with Shore A hardness 70 was as follows:55 phr of 110 polysiloxane with vinyl mole of 0.08%,42 phr of 110 polysiloxane with vinyl mole of 0.23%,3 phr of 112 with vinyl mole of 3%,42 phr of fumed silica with specific surface area of 380 m^(2)/g,8 phr of hydroxyl silicone oil,5 phr of methoxy silicone oil,0.1 phr of zinc stearate,0.5 phr of hydrogen containing silicone oil with active hydrogen mass of 0.5%,and 5 phr of polyvinyl silicone oil.Thus the silicone rubber has Shore A hardness of 70,tensile strength of 8.1 MPa,telongation at break of 540%,tear strength of 46 kN/m,elastic resilience of 71.5%,volatile of 1.2%,and n-hexane extracts of 1.6%,which can be used on Foley catheter,throat or drainage tube.

关 键 词：医用硅橡胶 撕裂强度 回弹 甲基乙烯基硅橡胶 气相法白炭黑 

分 类 号：TQ333.93[化学工程—橡胶工业]