硅树脂改性桐油醇酸树脂水性绝缘漆的研究
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摘要
根据有机硅树脂和醇酸树脂特性,为适应环保要求,充分利用我国桐油资源,制备出硅树脂改性桐油醇酸树脂水性绝缘漆,并对制备工艺与参数进行优化,利用FTIR,DSC,TG、耐压测试仪等测试手段对相关产物的结构和性能进行表征与测试。
基于溶胶凝胶法,以正硅酸乙酯(TEOS)、甲基三乙氧基硅烷(MTES)为原料,在催化剂作用下水解缩聚合成硅树脂,这种硅树脂以Si-O-Si为主链,含有大量的疏水基团Si-CH3基。实验优化得出硅树脂的最佳合成条件:TEOS、MTES、乙醇和水摩尔比3:4:3:24,催化剂盐酸pH 3-4,反应温度60℃,反应时间4h。在该条件下,硅树脂成膜后,具有很好的耐水性,接触角随着MTES含量的增加而增大, n TEOS / nMTES>5时,接触角稳定在138°漆膜的附着力为1级,硬度为3H。
以马来酸酐(MA)、三羟甲基丙烷(TMP)、桐油为原料,通过酯化反应与Diels– Alder加成反应,合成桐油醇酸树脂,再利用硅树脂通过酯化反应对其进行改性,合成硅树脂改性桐油醇酸树脂水性绝缘漆。实验得出,当体系酸值在55mgKOH/g,硅树脂含量为7.5wt%时,绝缘漆的固含量达到50%以上,而运动黏度在300mm2·s-1以内。漆膜的耐温性能优良,电气强度达到130MV·m-1,水的接触角大于120°,硬度达到5H
In order to meet environmental requirements and take advantage of china tung oil source, tung oil alkyd resin waterborne insulation paint modified by silicon resin was prepared. The parameters of the reaction was optimized, and the structure and properties of relative products were characterized and tested by FTIR, DSC, TG and withstand voltage tester.
Under catalysis, silicon resin was prepared from tetraethoxysilane(TEOS) and methyl triethoxysilane(MTES) in by sol-gel method. Large amounts of hydrophobic groups Si-CH3 were structured on the main chain Si-O-Si of the silicone resin.The best synthesis conditions from optimized experimental were as following: mole ratio of TEOS, MTES, C2H5OH and H2O is 3:4:3:24, reaction temperature and time are 60℃and 4h respectively, catalyst is HCl, whose pH is ranged from 3 to 4. When the above silicone resin was cured, the film has excellent adhesin, hardness and water resistance. With the increase of MTES content, the contact angle is increasing and reaches about 138°for nMTES/nTEOS >5.
Tung oil alkyd resin was prepared from tung oil, maleic anhydride (MA) and trimethylolpropane(TMP) by esterification and Diels-Alder addition reaction.Then, the waterborne insulation paint was prepared from tung oil alkyd resin modified by silicon resin. When acid value of system is 55mgKOH/g, content of silicone resin is 7.5wt%, the solid content of waterborne insulation paint is 55% while kinematic viscosity is wthin 300mm2 ?s-1. The heat resistance of the waterborne insulation paint film is excellent, electrical strength reaches 130MV·m-1, contact angle is above 120°and hardness reaches 5H.
基于溶胶凝胶法,以正硅酸乙酯(TEOS)、甲基三乙氧基硅烷(MTES)为原料,在催化剂作用下水解缩聚合成硅树脂,这种硅树脂以Si-O-Si为主链,含有大量的疏水基团Si-CH3基。实验优化得出硅树脂的最佳合成条件:TEOS、MTES、乙醇和水摩尔比3:4:3:24,催化剂盐酸pH 3-4,反应温度60℃,反应时间4h。在该条件下,硅树脂成膜后,具有很好的耐水性,接触角随着MTES含量的增加而增大, n TEOS / nMTES>5时,接触角稳定在138°漆膜的附着力为1级,硬度为3H。
以马来酸酐(MA)、三羟甲基丙烷(TMP)、桐油为原料,通过酯化反应与Diels– Alder加成反应,合成桐油醇酸树脂,再利用硅树脂通过酯化反应对其进行改性,合成硅树脂改性桐油醇酸树脂水性绝缘漆。实验得出,当体系酸值在55mgKOH/g,硅树脂含量为7.5wt%时,绝缘漆的固含量达到50%以上,而运动黏度在300mm2·s-1以内。漆膜的耐温性能优良,电气强度达到130MV·m-1,水的接触角大于120°,硬度达到5H
In order to meet environmental requirements and take advantage of china tung oil source, tung oil alkyd resin waterborne insulation paint modified by silicon resin was prepared. The parameters of the reaction was optimized, and the structure and properties of relative products were characterized and tested by FTIR, DSC, TG and withstand voltage tester.
Under catalysis, silicon resin was prepared from tetraethoxysilane(TEOS) and methyl triethoxysilane(MTES) in by sol-gel method. Large amounts of hydrophobic groups Si-CH3 were structured on the main chain Si-O-Si of the silicone resin.The best synthesis conditions from optimized experimental were as following: mole ratio of TEOS, MTES, C2H5OH and H2O is 3:4:3:24, reaction temperature and time are 60℃and 4h respectively, catalyst is HCl, whose pH is ranged from 3 to 4. When the above silicone resin was cured, the film has excellent adhesin, hardness and water resistance. With the increase of MTES content, the contact angle is increasing and reaches about 138°for nMTES/nTEOS >5.
Tung oil alkyd resin was prepared from tung oil, maleic anhydride (MA) and trimethylolpropane(TMP) by esterification and Diels-Alder addition reaction.Then, the waterborne insulation paint was prepared from tung oil alkyd resin modified by silicon resin. When acid value of system is 55mgKOH/g, content of silicone resin is 7.5wt%, the solid content of waterborne insulation paint is 55% while kinematic viscosity is wthin 300mm2 ?s-1. The heat resistance of the waterborne insulation paint film is excellent, electrical strength reaches 130MV·m-1, contact angle is above 120°and hardness reaches 5H.
引文
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[9]苏倩倩,刘伟区,侯孟华.聚甲基三乙氧基硅烷改性环氧树脂的研究.中国塑料, 2007, 21(8): 33-36.
[10]马悦欣,刘坤,周楠.甲基苯基硅树脂及其复合材料的性能研究.化学与黏合, 2007, 29(6): 390-394.
[11]谢伟,潘志煜.有机硅树脂对环氧树脂浇注体性能的影响.哈尔滨商业大学学报(自然科学版), 2003, 19(4): 507-508.
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[16] K Hayashida, H Ohtani, S Tsuge, et al. Flame retardanting mechanism of polycarbonate containing trifunctional phenylsilicone additive studied by analytical pyrolysis techniques. Polymer Bulletin, 2002, 48(6): 483-490.
[17]李步春.甲基硅树脂合成新工艺.有机硅材料及应用, 1999, 3: 4-7.
[18]闵春英,黄玉东,刘丽,等.温度及甲基硅树脂基复合材料介电性能及力学性能的影响.固体火箭技术, 2007, 30(4): 348-352.
[19] P Bajpai, M Bajpai. Development of a high performance hybridepoxy silicone resin for coatings. Pigment & Resin Technology, 2010, 39(2): 96-100.
[20]王瑜润,刘述梅,叶华,等.高苯基含量硅树脂阻燃剂的合成.化工新型材料, 2007, 35(4): 55-62.
[21]周文君,杨辉.甲基苯基硅树脂的制备工艺优化及阻燃性能.化工学报., 2006, 57(9): 2218-2222.
[22]暴峰,孙争光,黄世强. MQ硅树脂的合成及性能.有机硅材料, 2002, 16(3): 9-12.
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