双酚硅氧烷型苯并噁嗪/二氧化硅复合材料的制备与性能

doi:10.11949/j.issn.0438-1157.20150503

化工学报 ›› 2015, Vol. 66 ›› Issue (12): 5157-5162.DOI: 10.11949/j.issn.0438-1157.20150503

• 材料化学工程与纳米技术 • 上一篇下一篇

双酚硅氧烷型苯并噁嗪/二氧化硅复合材料的制备与性能

李明, 史铁钧, 袁伟, 徐国梅, 朱林林

合肥工业大学化学与化工学院, 安徽合肥 230009

收稿日期:2015-04-20 修回日期:2015-08-31 出版日期:2015-12-05 发布日期:2015-12-05
通讯作者: 史铁钧
基金资助:
国家自然科学基金项目(51273054)。

Preparation and properties of bisphenol siloxane benzoxazine/silica composites

LI Ming, SHI Tiejun, YUAN Wei, XU Guomei, ZHU Linlin

Chemistry and Chemical Engineering, Hefei University of Technology, Hefei 230009, Anhui, China

Received:2015-04-20 Revised:2015-08-31 Online:2015-12-05 Published:2015-12-05
Supported by:
supported by the National Natural Science Foundation of China (51273054).

摘要/Abstract

摘要：

以双酚A(BPA)、γ-氨丙基三乙氧基硅烷(KH-550)、多聚甲醛为原料,合成双酚硅氧烷型苯并噁嗪(BZ),固化得到聚双酚硅氧烷型苯并噁嗪(PB),再用BZ与溶胶-凝胶法合成的改性二氧化硅共混,固化得到双酚硅氧烷型苯并噁嗪/二氧化硅复合材料(PBS)。采用FI-IR,¹H NMR等分析手段对BZ的化学结构进行了表征;采用DSC对BZ固化性能进行研究,使用TG分析PBS的稳定性。结果表明:在氮气氛围中,BZ在181℃开环聚合;PB失重5%时的温度为302℃,失重10%时的温度为375℃,在800℃时的残炭率为53%;PBS失重5%时的温度为316℃,失重10%时的温度为407℃,在800℃时的残炭率为59%。聚合物表面及断面扫描电镜图像分析表明:BZ与溶胶-凝胶法合成的改性二氧化硅有较好的相容性且提高了韧性。

关键词: 合成, 改性二氧化硅, 复合材料, 稳定性, 表面, 相容性, 韧性

Abstract:

BZ was synthesized by using BPA, KH-550 and paraformaldehyde as raw materials. PB was formed by curing of BZ. Then PBS was obtained by curing of co-mixed BZ and modified silica. The chemical structure of BZ was characterized by FT-IR, ¹H NMR. The curing characteristics was studied by DSC and the thermostability was analyzed by TG. The results showed that ring opening polymerization of BZ was 181℃ in N₂. To PB, the temperature of 5% weight loss was 302℃ and that of 10% weight loss was 375℃, while carbon residue was 53% in 800℃. For PBS, the temperature of 5% weight loss was 316℃ and that of 10% weight loss was 407℃, while carbon residue was 59% in 800℃. The SEM image of polymers indicated that bisphenol siloxane benzoxazine with modified silica had a good compatibility and ductibility.

Key words: synthesis, modified silica, composites, stability, surface, compatibility, ductibility

中图分类号:

李明, 史铁钧, 袁伟, 徐国梅, 朱林林. 双酚硅氧烷型苯并噁嗪/二氧化硅复合材料的制备与性能[J]. 化工学报, 2015, 66(12): 5157-5162.

LI Ming, SHI Tiejun, YUAN Wei, XU Guomei, ZHU Linlin. Preparation and properties of bisphenol siloxane benzoxazine/silica composites[J]. CIESC Journal, 2015, 66(12): 5157-5162.

参考文献 24

[1]	Holly F W, Cope A C.Condensation products of aldehydes and ketones with o-aminobenzyl alcoholand o-hydroxybenzylamine [J]. Journal of the America Chemical Society, 1944, 66: 1875-1879.
[2]	Ning X, Ishida H. Phenolic materials via ring-opening polymerization of benzoxazines: effect of molecular structure on mechanical and dynamic mechanical properties [J]. J. Polym. Sci., Part B: Polym. Physics., 1994, 32: 921- 927.
[3]	Ghosh N N, Kiskan B, Yagci Y. Polybenzoxazines-new high performance thermosetting resins: synthesis and properties [J]. Prog. Polym. Sci., 2007, 32: 1344-1391.
[4]	Ishida H, Low H Y. A study on the volumetric expansion of benzoxazine-based phenolic Resin [J]. Macromalecules, 1997, 30: 1099-1106.
[5]	Herrera P V, Doyama K, Abe H, Ishida H. Sythesis and characterization of highly fluorinated polymer with the benzoxazine moiety in the main chain [J]. Macromalecules, 2008, 41: 9704-9714.
[6]	Agag T, Geiger S, Alhassan S M, Qutubuddin S, Ishida H. Low-viscosity polyether-based main-chain benzoxazine polymers: precursors for flexible thermosetting polymers [J]. Macromolecues, 2010, 43: 7122-7127.
[7]	Wang Zhen, Dai Zhen, Wu Junjie, Zhao Ning, Xu Jian. Vacuum-dried robust bridged silsequioxane aerogels [J]. Advanced Materials, 2013, 25: 4494-4497.
[8]	Capadona L A, Meador M B, Alunni A, Fabrizio E F, Vassilaras P, Leventis N. Flexible, low-density polymer crosslinked silica aerogels [J]. Polymer, 2006, 47: 5754-5761.
[9]	Liu Jianhua (刘建华), Shi Tiejun (史铁钧). Synthesis, characteri- zation and curing characteristics of double benzoxazine contained double DOPO based on bisphenol A [J]. CIESC Journal (化工学报), 2014, 65(11): 4607-4613.
[10]	Wang Qidong (王启东), Shi Tiejun (史铁钧), Xu Guomei (徐国梅). Synthesis, characterization of PT-ala resin and thermal degradation kinetics of its polymer [J]. CIESC Journal (化工学报), 2013, 64(10): 3851-3857.
[11]	Jia Yanping (贾艳萍), Ma Jiao (马姣), Zhang Lanhe (张兰河), Dong Changqing (董长青), Wang Xiaoqiang (王孝强). Progress in the application of porous silica materials [J]. Bulletin of the Chinese Ceramic Society (硅酸盐通报), 2014, 33(12): 3206-3212.
[12]	Liu Yang (刘洋), Zhang Yi (张毅), Li Dongxu (李东旭). Ambient pressure drying preparation of hydrophobic SiO2 aerogel [J]. Journal of Functional Materials (功能材料), 2015, 46(5): 5132-5135.
[13]	Xiong Gang (熊刚), Chen Xiaohong (陈晓红), Wu Wenjun (吴文军), Hu Zijun (胡子军), Sun Chencheng (孙陈诚), Song Huaihe (宋怀河). Research progress on the toughness of silica aerogels [J]. Bulletin of the Chinese Ceramic Society (硅酸盐通报), 2010, 29(5): 1079-1085.
[14]	Shi Fei (史非), Wang Lijiu (王立久), Liu Jingxiao (刘敬肖). Ambient pressure drying preparation and characterization of nano mesoporous SiO2 aerogels [J]. Journal of the Chinese Ceramic Society (硅酸盐学报), 2005, 33(8): 964-974.
[15]	Duan Yannan, Jana S C, Lama B, Espe M P. Reinforcement of silica aerogels using silane-end-capped polyurethanes [J]. Langmuir, 2013, 29: 6156-6165.
[16]	Sun Jianxin (孙建新), Shi Tiejun (史铁钧), Xu Hui (徐慧), Wu Xinglin (吴星林). Synthesis, structure and thermal properties of bisphenol fluorene diamine benzoxazine [J]. Chemical Journal of Chinese Universities (高等学校化学学报), 2011, 32: 1216-1220.
[17]	Xu Guomei, Shi Tiejun, Liu Jianhua, Wang Qidong. Preparation of a liquid benzoxanzine based on cardanol and the thermal stability of its graphene oxide composites [J]. Journal of Applied Polymer Science, 2014, 10: 1-8.
[18]	Wen Tinglei (文听雷), Shi Tiejun (史铁钧), Zhang Ming (张明), et al. Synthesis, characterization and non-isothermal curing kinetics of PT-eda benzoxazine [J]. Journal of Solid Rocket Technology (固体火箭技术), 2013, 36: 408-412.
[19]	Bai Huichao (白会超). Research on high char yield benzoxazine resin [D]. Wuhan: Wuhan University of Technology, 2007.
[20]	Chen Wenjin (陈文瑾). Research on the synthesis, modification and properties of benzoxazine resins [D]. Chengdu: University of Electronic Science and Technology of China, 2012.
[21]	Zhang Shijie (张世杰), Zhang Wei (张炜), Guo Yalin (郭亚林). Performance study of nano carbon powder modified benzo oxazine resin ablative [J]. Thermosetting Resin (热固性树脂), 2008, 23(6): 13-17.
[22]	Yu Liping (于丽萍), Yan Chun (颜春), Zhang Xiaoqing (张笑晴), Li Hongzhou (李红周), et al. Study on toughening of epoxy terminated methylphenyl silicone oil benzoxazine resin [J]. Journal of Materials (材料导报), 2012, (22): 71-75.
[23]	Yan Chun (颜春), Fan Xinyu (范欣愉), Zhu Chunyan (朱春燕), Jiang Yanhua (江艳华). Study of nano silica toughening of benzoxazine [G/OL]. http://www.polymer.cn/polymer2009/
[24]	Zhang Jian (张建), Liu Xiangyang (刘向阳), Gu Yi (顾宜). Research on high performance of molding compound materials [J]. China Plastics Industry (塑料工业), 2009, 37(3): 78-81.

双酚硅氧烷型苯并噁嗪/二氧化硅复合材料的制备与性能

Preparation and properties of bisphenol siloxane benzoxazine/silica composites

PDF (PC)

可视化

被引次数

摘要/Abstract

引用本文

使用本文

参考文献 24

相关文章 15

编辑推荐

Metrics

本文评价

[1]	吴馨, 龚建英, 靳龙, 王宇涛, 黄睿宁. 超声波激励下铝板表面液滴群输运特性的研究[J]. 化工学报, 2023, 74(S1): 104-112.
[2]	江河, 袁俊飞, 王林, 邢谷雨. 均流腔结构对微细通道内相变流动特性影响的实验研究[J]. 化工学报, 2023, 74(S1): 235-244.
[3]	王琪, 张斌, 张晓昕, 武虎建, 战海涛, 王涛. 氯铝酸-三乙胺离子液体/P₂O₅催化合成伊索克酸和2-乙基蒽醌[J]. 化工学报, 2023, 74(S1): 245-249.
[4]	杨越, 张丹, 郑巨淦, 涂茂萍, 杨庆忠. NaCl水溶液喷射闪蒸-掺混蒸发的实验研究[J]. 化工学报, 2023, 74(8): 3279-3291.
[5]	郑玉圆, 葛志伟, 韩翔宇, 王亮, 陈海生. 中高温钙基材料热化学储热的研究进展与展望[J]. 化工学报, 2023, 74(8): 3171-3192.
[6]	胡兴枝, 张皓焱, 庄境坤, 范雨晴, 张开银, 向军. 嵌有超小CeO₂纳米粒子的碳纳米纤维的制备及其吸波性能[J]. 化工学报, 2023, 74(8): 3584-3596.
[7]	杨菲菲, 赵世熙, 周维, 倪中海. Sn掺杂的In₂O₃催化CO₂选择性加氢制甲醇[J]. 化工学报, 2023, 74(8): 3366-3374.
[8]	孟令玎, 崇汝青, 孙菲雪, 孟子晖, 刘文芳. 改性聚乙烯膜和氧化硅固定化碳酸酐酶[J]. 化工学报, 2023, 74(8): 3472-3484.
[9]	杨欣, 彭啸, 薛凯茹, 苏梦威, 吴燕. 分子印迹-TiO₂光电催化降解增溶PHE废水性能研究[J]. 化工学报, 2023, 74(8): 3564-3571.
[10]	陈天华, 刘兆轩, 韩群, 张程宾, 李文明. 喷雾冷却换热强化研究进展及影响因素[J]. 化工学报, 2023, 74(8): 3149-3170.
[11]	李彬, 徐正虎, 姜爽, 张天永. 双氧水催化氧化法清洁高效合成促进剂CBS[J]. 化工学报, 2023, 74(7): 2919-2925.
[12]	葛加丽, 管图祥, 邱新民, 吴健, 沈丽明, 暴宁钟. 垂直多孔碳包覆的FeF₃正极的构筑及储锂性能研究[J]. 化工学报, 2023, 74(7): 3058-3067.
[13]	张澳, 罗英武. 低模量、高弹性、高剥离强度丙烯酸酯压敏胶[J]. 化工学报, 2023, 74(7): 3079-3092.
[14]	王杰, 丘晓琳, 赵烨, 刘鑫洋, 韩忠强, 许雍, 蒋文瀚. 聚电解质静电沉积改性PHBV抗氧化膜的制备与性能研究[J]. 化工学报, 2023, 74(7): 3068-3078.
[15]	涂玉明, 邵高燕, 陈健杰, 刘凤, 田世超, 周智勇, 任钟旗. 钙基催化剂的设计合成及应用研究进展[J]. 化工学报, 2023, 74(7): 2717-2734.