卡拉胶包覆APP微球阻燃水性环氧树脂
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摘要
以氯化钡提纯k-卡拉胶,经过氧化氢降解,通过反相乳液聚合的方式制备了一系列卡拉胶包覆聚磷酸铵(APP)阻燃微球(k-CM/APP);将其加入到水性环氧树脂(EP)中,制备了3种钢结构防火涂层EP2,EP3和EP4.利用红外光谱(IR)、扫描电子显微镜(SEM)及元素分析(EDS)对k-CM/APP的结构及形貌进行了表征.利用极限氧指数(LOI)、垂直燃烧(UL-94)、背温测试法、热重分析(TG)、锥形量热(CONE)、附着力测试、IR和SEM等方法分析了涂层的阻燃、隔热及力学性能.结果表明,k-CM/APP(3/1)球形结构完整,800℃时的残炭量高达59. 5%.与其它阻燃涂层体系相比,添加了k-CM/APP (3/1)的EP3防火涂层的极限氧指数达到28. 5%,UL-94达到了V-0级,60 min防火涂层耐火温度为253℃.相比于纯EP涂层,EP3涂层的热释放速率峰值降低了58. 26%,总热释放量降低了20. 84%,附着力达到8. 74 MPa.
After k-carrageenan was purified by barium chloride and degraded by hydrogen oxidation,a series of k-carrageenan/ammonium polyphosphate( k-CM/APP) inflame-retardant microsphere was prepared using inverse emulsion polymerization method. Then k-CM/APP was added to water-borne epoxy resin to prepare EP2,EP3,EP4 steel structure fire retardant coating. The structure and morphology of k-CM/APP were represented by using infrared spectrograph( IR),scanning electron microscope( SEM),energy dispersive spectrometry( EDS). The limit oxygen index( LOI),vertical combustion( UL-94),back temperature test method,thermogravimetry( TG),cone calorimeter,adhesion tester,IR and SEM were used for analyzing the flame retardant property,heat-insulating property,thermal property and mechanical property. Research results showed that k-CM/APP spherical structure was complete,and the carbon residue at 800 ℃ reached 59. 5%. Compared with other fire retardant coatings,the LOI of the EP3 fire retardant coating with added k-CM/APP( 3/1)reached 28. 5%,UL-94 reached the class V-0,and the fire-resistant temperature of 60 min fire retardant coating was 253 ℃. Compared with pure EP coating,the heat release rate peak of EP2 coating was decreased by58. 26% and the total heat release quantity was decreased by 20. 84%,adhesion reached 8. 74 MPa.
After k-carrageenan was purified by barium chloride and degraded by hydrogen oxidation,a series of k-carrageenan/ammonium polyphosphate( k-CM/APP) inflame-retardant microsphere was prepared using inverse emulsion polymerization method. Then k-CM/APP was added to water-borne epoxy resin to prepare EP2,EP3,EP4 steel structure fire retardant coating. The structure and morphology of k-CM/APP were represented by using infrared spectrograph( IR),scanning electron microscope( SEM),energy dispersive spectrometry( EDS). The limit oxygen index( LOI),vertical combustion( UL-94),back temperature test method,thermogravimetry( TG),cone calorimeter,adhesion tester,IR and SEM were used for analyzing the flame retardant property,heat-insulating property,thermal property and mechanical property. Research results showed that k-CM/APP spherical structure was complete,and the carbon residue at 800 ℃ reached 59. 5%. Compared with other fire retardant coatings,the LOI of the EP3 fire retardant coating with added k-CM/APP( 3/1)reached 28. 5%,UL-94 reached the class V-0,and the fire-resistant temperature of 60 min fire retardant coating was 253 ℃. Compared with pure EP coating,the heat release rate peak of EP2 coating was decreased by58. 26% and the total heat release quantity was decreased by 20. 84%,adhesion reached 8. 74 MPa.
引文
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[2] Rackauskaite E.,El-Rimawi J.,Fire Technology,2015,51(4),867—886
[3] Kwon I. K.,Kwon Y. B.,International Journal of Steel Structures,2012,12(1),25—35
[4] Yan H. W.,Wei J. L.,Yin B.,Yang M. B.,Polymer Bulletin,2015,72(11),2725—2737
[5] Wang Z.,Sui X.,Jie G.,Polymer Materials Science&Engineering,2012,28(4),39—42
[6] Sun L. H.,Qu Y. T.,Journal of Thermal Analysis and Calorimetry,2013,111(2),1099—1106
[7] Wu K.,Song L,Wang Z,Hu Y.,Polymers for Advanced Technologies,2010,19(12),1914—1921
[8] Wang N.,Xu G.,Wu Y. H.,Zhang J.,Hu L. D.,Luan H. H.,Fang Q. H.,Journal of Thermal Analysis and Calorimetry,2016,123(2),1239—1251
[9] Wang N.,Hu L.,Zhang J.,Fang Q.,Journal of Thermal Analysis&Calorimetry,2016,128(2),1—10
[10] Zi X.,Zhang W,Mai Y.,RSC Advances,2017,7(41),25253—25264
[11] Liang X. C.,Duan J. J.,Qi X.,Wei X. Q.,Lu A.,Chemical Engineering Journal,2017,317,766—776
[12] Wang N.,Wang S.,Zhang J.,Fang Q. H.,Fine Chemicals,2017,34(4),451—455,462(王娜,王升,张静,方庆红.精细化工,2017,34(4),451—455,462)
[13] Franco A.,Andrés M.,Betty M.,Jorge P.,Rodrigo T.,Journal of Applied Phycology,2016,28(2),1275—1286
[14] Liu C.,Chen K.,Li J. J.,Acta Materiae Compositae Sinica,2015,32(3),728—736
[15] Wang X.,Hu Y.,Song L.,Polymer,2010,51(11),2435—2445
[16] Zhou Y.,Hao J. W.,Liu G. S.,Du J. X.,Journal of Inorganic Chemistry,2013,29(6),1115—1122(周友,郝建薇,刘国胜,杜建新.无机化学学报,2013,29(6),1115—1122)
[17] Wang X.,Functionalization of Graphene and Its Epoxy Composites,and Study on Their Flame Retardant Properties and Mechanism,University of Science and Technology of China,Hefei,2013(王鑫.石墨烯的功能化及其环氧树脂复合材料的阻燃性能及机理研究,合肥:中国科学技术大学,2013)
[18] Li Q.,Jian H.,Jiu J.,Ying Y.,Chem. Res. Chinese Universities,2017,33(1),1—7
[19] Lv J. Z.,Xu Y. X.,Zhu D. R.,Zhang L.,Fine Chemicals,2001,18(6),341—344(吕九琢,徐亚贤,竺栋荣,张雳.精细化工,2001,18(6),341—344)
[20] Wang K.,Li D. H.,Yang R. J.,Polymer Materials Science and Engineering,2016,32(7),51—56(王珂,李定华,杨荣杰.高分子材料科学与工程,2016,32(7),51—56)
[21] Puri R. G.,Khanna A. S.,Progress in Organic Coatings,2016,92,8—15
[22] White R. H.,Nam S.,Parikh D. V.,Fire&Materials,2013,37(1),46—57
[23] Xie H.,Lai X.,Li H.,China Rubber/plastics Technology&Equipment,2017,130,68—77
[24] Wang A.,Duan Y.,Gu X.,Zhang S.,Chem. Res. Chinese Universities,2017,33(3),492—498
[25] Wang N.,Zhang Y. N.,Chen J. S.,Progress in Organic Coatings,2017,109,126—134
[26] Wang N.,Gao H. Y.,Zhang J.,Kang P.,Coatings,2018,8(5),179—183
[27] Zhang W. W.,Study on Modification and Flame Retardant Mechanism of Carrageenan Fiber,Qingdao University,Qingdao,2017(张伟伟.卡拉胶纤维的改性及阻燃机理研究,青岛:青岛大学,2017)
[28] Liu L. N.,Qian M. B.,Song P. A.,ACS Sustainable Chemistry&Engineering,2016,4(4),2422—2431
[29] Shi Y. C.,Wang G. J.,Journal of Coatings Technology and Research,2016,13(3),457—468
[30] Xu M. J.,Xia S. Y.,Liu C. A.,Li B.,Chinese Journal of Polymer Science,2018,36(5),655—664