聚苯乙烯纳米复合材料的制备、结构和性能的研究
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摘要
本文主要研究了蒙脱土的插层改性，采用插层聚合、熔融插层复合和原位聚合方法制备了各自的聚苯乙烯／蒙脱土纳米复合材料，利用红外光谱、X射线衍射、扫描电镜、差热分析和热失重分析等手段对其结构与性能进行表征。结果表明，十二烷基磺酸钠阴离子表面活性剂对蒙脱土有优异的插层改性效果。三种不同复合方法均得到了纳米复合材料。复合材料的结构与热性能随着蒙脱土含量的改变而变化，它们的热学性能和力学性能较纯聚苯乙烯有较大提高。
In this thesis, montmorillonite were modified and PS/MMT nanocomposites were prepared by intercalation polymerization melt blend and in situ polymerization respectively. The structure and physical properties were studied by FT-IR, XRD, TEM, DDA, TG. The results indicated that Sodium laurylsulfonate has excellent intercalation effect on Montmorillonite. The materials obtained through three different methods are all nanocomposites, possessing changed structure and properties with different contents of Montmorillonite. Compared with pure PS, the nanocomposites possessed desired property, such as increased thermal stability and impulsion intensity.
In this thesis, montmorillonite were modified and PS/MMT nanocomposites were prepared by intercalation polymerization melt blend and in situ polymerization respectively. The structure and physical properties were studied by FT-IR, XRD, TEM, DDA, TG. The results indicated that Sodium laurylsulfonate has excellent intercalation effect on Montmorillonite. The materials obtained through three different methods are all nanocomposites, possessing changed structure and properties with different contents of Montmorillonite. Compared with pure PS, the nanocomposites possessed desired property, such as increased thermal stability and impulsion intensity.
引文
1 朱军，李毕忠．聚合物／无机纳米复合材料研究进展．化工新型材料，2000，28(10)：3～8
2 R.Roy,S. Komarneni,D.M. Roy.Mater.Res.Soc.Symp.Proc., 1984,32:347
3 严东生．纳米材料的合成与制备．无机材料学报．1995，10(1)：1～6
4 刘英俊，刘伯元等．塑料填充改性．第1版．北京：中国轻工业出版社，1998
5 王新宇，漆宗能，王佛松．聚合物．层状硅酸盐纳米复合材料制备与应用．工程塑料应用．1999，27(2)：1～5
6 J Ishida H., Campbell S., Blackwell. General approach to nanocomposite preparetion. J. Chem, Mater. 2000, 12(5): 1260～1267
7 Sukpiron N., Lerner M., Preparation of organic-inorganic nanocomposites with a layered titanate. Chem. Mater. 2001, 13(6): 2179～2185
8 甘景镐．天然高分子化学．第1版．北京：高等教育出版社，1993
9 Nalwa H. S., Handbook of Nanostructured materials and nanotechnology, Chap. 1, Intercalation compounds in layered host lattices: supramolecular chemistry in nanodimensions, Academic press, San Diego, 1999
10 曹明礼．蒙脱石层间化合物的制备及应用前景．材料导报．2001，15(4)：30～32
11 Van Olphen H. An introduction to clay colloid chemistry. 2nd ed. New york: Wiley, 1997
12 陈光明,韩布兴, 阎海科.A study on the interaction of FeCl_3 with montmorillonite suspensions. Adsopt. Sci Technol. 1998, 16(3):235～242
13 陈光明，赵扬，宋湘等．全国第8届化学热力学和热分析(CTTA)学术会议．上海：1996：8～13
14 陈光明,宋湘, 赵扬等. Adsorption enthalpy and adsorption isotherm of teteradecylpyridinium bromide in Na-montmorillonite. J. Colloid Interface. Sci. 1997, 186(1):206～208
15 陈光明,韩布兴, 阎海科. Interaction of cationic surfactants with iron and sodium montmorillonite suspensions, J. Colloid Interf.Sci. 1998,201(2): 158～163
16 陈光明, 潘竟军, 韩布兴等 . Adsorption of methylene blue on montmorillonite. J. Dispersion Sci. Techn. 1999, 20(4):1179～1187
17 潘竟军，陈光明．亚甲基蓝在钠、铝和铁蒙脱土上的吸附研究．油田化学．1999，16(3)：195～197
18 Gianelis E P. Polymer layer silicate nanocomposites. Adv. Mater. 1996,8(1):29～35
19 N.ogata, S.kawakage. Poly(vinyl alcohol)-clay and poly(ethylene oxide)-clay blends prepared using water as solvent, J. Appl. Polym.Sci, 1997,66:573～581
20 R.Levy, C.W.Franeis. Interlayer adsorption of poly(vinylpyrolidene) on montmorillonite. J. Colliod Interface Sci, 1975, 50:442～450
21 N.ogata, G. Jimenez, et al. Poly(ethylene oxide)-clay mineral blends. Polymer,1997, 38(20):5115～5118
22 N.ogata, G.Jimenez, H.kawai, et al. Structure and thermal/mechanical properties of poly(1-lactide)-clay blend. J. Poly. Sci. Part B: Polymer. Phys., 1997, 35(2):389～396
23 Lee.C.D., Wang.L.W. Preparation and characterization of PMMA-Clay Hybrid Composite by Emulsion Polymerization, J.Appl.Polym. Sci., 1996,61 : 1117～1122.
24 Whan, M., Lee.D.C., Synthesis and characterization of PS-Clay nanocomposite by Emulsion Polymerization,Polymer Bull., 1999,42:619～626
25 Vaia, R.; Giannelis, E. P. Lattice model of Polymer melt intercalation in o9rganically-modified layered silicates. Macrolecules., 1997,30:7990～7999
26 K. Masenelli-Varlot et al. Mechanical properties of clay-reinforced polyamide. J. Polym. Sci. part B: 2002,40(3):272～283
27 M.W.Weimer, Chen et al. Direct synthesis of dispersed nanocomposites by in situ living free radical polymerization using a silicate-anchored initiator. J.Am. Chem. Soc. 1999,121:1615～1616
28 A.Usuki, Y.kojima et al. Synthesis of nylon 6-clay hybrid. J. Mater. Res., 1993,8(5): 1179～1184
29 Y.kojima, A.Usuki, et al. One-pot synthesis of nylon 6-clay hybrid. J. Polym Sci. Part A:Polym Chem., 1993,31 (7): 1755～1758
30 余鼎声，王一中．粘土／尼龙6嵌入化合物的合成与表征．高分子材料科学与工程，1998，14(3)：26～29
31 P.Reichert, J. Kessler et al. Nanocomposites based on a synthetic layer silicate and polyamide-12. Acta Polym., 1998,49, 116～123
32 X.Kornmann.; L.A.Berglvnd et al. Nanocomposites based on montmorillonite and unsaturated polyester. Polym. Eng. Sci., 1998 38(8) 1351～1358
33 吴德峰 史铁钧等．丙烯酰胺与蒙脱土的接枝反应．胶体与聚合物 2002，20(1)：18～21
34 杜慷慨，林志勇，吴季怀．苯乙烯与蒙脱土的接枝反应．塑料工业 2001，29(1)：21～22
35 刘晓辉 范家起等．聚丙烯／蒙脱土纳米复合材料1：制备、表征及动态力学性能．高分子学报．2000，5：563～567
36 陈光明，马永梅，漆宗能．甲苯—2，4—二异氰酸酯修饰蒙脱土及聚苯乙烯／蒙脱土纳米复合材料的制备与表征．高分子学报，2000，5：599～603
37 T.J.Pinnavaia, T. Lan et al. Clay-polymer nanocomposites: polether and polyimide systems. Mater. Res.Soc.Symp.Proc., 1994,346:81～88
38 R.A.Vaia, S.Vasudevant, W.Krawiec et al. New polymer electrolyte nanocomposites: Melt intercalation of poly(ethylene oxide) in micatype silicates. Adv. mater., 1995,7(2): 154～156
39 M.W.Noh, D.Lee. Synthesis & characterization of PS-clay nanocomposite by emulsion polymerization.Polym. Bull., 1999,42(5):619～626
40 吕建坤，柯毓才，漆宗能等．插层聚合制备粘土／环氧树脂纳米复合材料过程中粘土剥离行为的研究．高分子学报，2000，(1)：85～89
41 B.Hoffmann, C.Dietrich, R.Thomann et al. Mophology & rheology of polystyrene nanocomposites based upon organoclay. Macromol. Rapid Commun., 2000,21(1):57～61
42 N.hasegawa, M. Kawasumi, M. Kato et al. Preparation and mechanical properties of
polypropylene-clay hybrids using a maleic anhydride-modified polypropylene oligomer. J.Appl. Polym. Sci., 1998,67(1):87～92
43 M.Kawasumi, N.Hasegawa, M. Kato et al. Preparation and mechanical properties of polypropylene-clay hybrids. Macromolecules, 1997,30:6333～6338
44 Giannelis E P. Polymer layered silicate nanocomposites. Adv. Maer.. 1996,8(1):29～35
45 Wang M S, Pinnavaia T, Clay-polymer nanocomposites formed from acidic derivatives of montmorillonite and epoxy resin. J. Chem Mater 1994,6:468～674
46 Vaia R.A, Giannelis E. P. et al. Dynamics in a confined polymer electrolhyte: A 7Li and 2H NMR study. J. Am. Chem. Soc. 1995,117(28):7568～7569
47 王立新，赵金玲，任丽，刘盘阁，姬荣琴，聚吡咯／蒙脱土纳米复合材料的表征与复合机理．功能材料，2003，34(3)：325～327
48 Gabried C., Ossenkamp, et al. New approaches to surface-alkylated silica with increased hydrolytic stability. Chem. Mater 2002, from the internet
49 Eduardo R. H. Conducting polymers intercalated in layered solids. Adv. Mater 1993, 5:334～340
2 R.Roy,S. Komarneni,D.M. Roy.Mater.Res.Soc.Symp.Proc., 1984,32:347
3 严东生．纳米材料的合成与制备．无机材料学报．1995，10(1)：1～6
4 刘英俊，刘伯元等．塑料填充改性．第1版．北京：中国轻工业出版社，1998
5 王新宇，漆宗能，王佛松．聚合物．层状硅酸盐纳米复合材料制备与应用．工程塑料应用．1999，27(2)：1～5
6 J Ishida H., Campbell S., Blackwell. General approach to nanocomposite preparetion. J. Chem, Mater. 2000, 12(5): 1260～1267
7 Sukpiron N., Lerner M., Preparation of organic-inorganic nanocomposites with a layered titanate. Chem. Mater. 2001, 13(6): 2179～2185
8 甘景镐．天然高分子化学．第1版．北京：高等教育出版社，1993
9 Nalwa H. S., Handbook of Nanostructured materials and nanotechnology, Chap. 1, Intercalation compounds in layered host lattices: supramolecular chemistry in nanodimensions, Academic press, San Diego, 1999
10 曹明礼．蒙脱石层间化合物的制备及应用前景．材料导报．2001，15(4)：30～32
11 Van Olphen H. An introduction to clay colloid chemistry. 2nd ed. New york: Wiley, 1997
12 陈光明,韩布兴, 阎海科.A study on the interaction of FeCl_3 with montmorillonite suspensions. Adsopt. Sci Technol. 1998, 16(3):235～242
13 陈光明，赵扬，宋湘等．全国第8届化学热力学和热分析(CTTA)学术会议．上海：1996：8～13
14 陈光明,宋湘, 赵扬等. Adsorption enthalpy and adsorption isotherm of teteradecylpyridinium bromide in Na-montmorillonite. J. Colloid Interface. Sci. 1997, 186(1):206～208
15 陈光明,韩布兴, 阎海科. Interaction of cationic surfactants with iron and sodium montmorillonite suspensions, J. Colloid Interf.Sci. 1998,201(2): 158～163
16 陈光明, 潘竟军, 韩布兴等 . Adsorption of methylene blue on montmorillonite. J. Dispersion Sci. Techn. 1999, 20(4):1179～1187
17 潘竟军，陈光明．亚甲基蓝在钠、铝和铁蒙脱土上的吸附研究．油田化学．1999，16(3)：195～197
18 Gianelis E P. Polymer layer silicate nanocomposites. Adv. Mater. 1996,8(1):29～35
19 N.ogata, S.kawakage. Poly(vinyl alcohol)-clay and poly(ethylene oxide)-clay blends prepared using water as solvent, J. Appl. Polym.Sci, 1997,66:573～581
20 R.Levy, C.W.Franeis. Interlayer adsorption of poly(vinylpyrolidene) on montmorillonite. J. Colliod Interface Sci, 1975, 50:442～450
21 N.ogata, G. Jimenez, et al. Poly(ethylene oxide)-clay mineral blends. Polymer,1997, 38(20):5115～5118
22 N.ogata, G.Jimenez, H.kawai, et al. Structure and thermal/mechanical properties of poly(1-lactide)-clay blend. J. Poly. Sci. Part B: Polymer. Phys., 1997, 35(2):389～396
23 Lee.C.D., Wang.L.W. Preparation and characterization of PMMA-Clay Hybrid Composite by Emulsion Polymerization, J.Appl.Polym. Sci., 1996,61 : 1117～1122.
24 Whan, M., Lee.D.C., Synthesis and characterization of PS-Clay nanocomposite by Emulsion Polymerization,Polymer Bull., 1999,42:619～626
25 Vaia, R.; Giannelis, E. P. Lattice model of Polymer melt intercalation in o9rganically-modified layered silicates. Macrolecules., 1997,30:7990～7999
26 K. Masenelli-Varlot et al. Mechanical properties of clay-reinforced polyamide. J. Polym. Sci. part B: 2002,40(3):272～283
27 M.W.Weimer, Chen et al. Direct synthesis of dispersed nanocomposites by in situ living free radical polymerization using a silicate-anchored initiator. J.Am. Chem. Soc. 1999,121:1615～1616
28 A.Usuki, Y.kojima et al. Synthesis of nylon 6-clay hybrid. J. Mater. Res., 1993,8(5): 1179～1184
29 Y.kojima, A.Usuki, et al. One-pot synthesis of nylon 6-clay hybrid. J. Polym Sci. Part A:Polym Chem., 1993,31 (7): 1755～1758
30 余鼎声，王一中．粘土／尼龙6嵌入化合物的合成与表征．高分子材料科学与工程，1998，14(3)：26～29
31 P.Reichert, J. Kessler et al. Nanocomposites based on a synthetic layer silicate and polyamide-12. Acta Polym., 1998,49, 116～123
32 X.Kornmann.; L.A.Berglvnd et al. Nanocomposites based on montmorillonite and unsaturated polyester. Polym. Eng. Sci., 1998 38(8) 1351～1358
33 吴德峰 史铁钧等．丙烯酰胺与蒙脱土的接枝反应．胶体与聚合物 2002，20(1)：18～21
34 杜慷慨，林志勇，吴季怀．苯乙烯与蒙脱土的接枝反应．塑料工业 2001，29(1)：21～22
35 刘晓辉 范家起等．聚丙烯／蒙脱土纳米复合材料1：制备、表征及动态力学性能．高分子学报．2000，5：563～567
36 陈光明，马永梅，漆宗能．甲苯—2，4—二异氰酸酯修饰蒙脱土及聚苯乙烯／蒙脱土纳米复合材料的制备与表征．高分子学报，2000，5：599～603
37 T.J.Pinnavaia, T. Lan et al. Clay-polymer nanocomposites: polether and polyimide systems. Mater. Res.Soc.Symp.Proc., 1994,346:81～88
38 R.A.Vaia, S.Vasudevant, W.Krawiec et al. New polymer electrolyte nanocomposites: Melt intercalation of poly(ethylene oxide) in micatype silicates. Adv. mater., 1995,7(2): 154～156
39 M.W.Noh, D.Lee. Synthesis & characterization of PS-clay nanocomposite by emulsion polymerization.Polym. Bull., 1999,42(5):619～626
40 吕建坤，柯毓才，漆宗能等．插层聚合制备粘土／环氧树脂纳米复合材料过程中粘土剥离行为的研究．高分子学报，2000，(1)：85～89
41 B.Hoffmann, C.Dietrich, R.Thomann et al. Mophology & rheology of polystyrene nanocomposites based upon organoclay. Macromol. Rapid Commun., 2000,21(1):57～61
42 N.hasegawa, M. Kawasumi, M. Kato et al. Preparation and mechanical properties of
polypropylene-clay hybrids using a maleic anhydride-modified polypropylene oligomer. J.Appl. Polym. Sci., 1998,67(1):87～92
43 M.Kawasumi, N.Hasegawa, M. Kato et al. Preparation and mechanical properties of polypropylene-clay hybrids. Macromolecules, 1997,30:6333～6338
44 Giannelis E P. Polymer layered silicate nanocomposites. Adv. Maer.. 1996,8(1):29～35
45 Wang M S, Pinnavaia T, Clay-polymer nanocomposites formed from acidic derivatives of montmorillonite and epoxy resin. J. Chem Mater 1994,6:468～674
46 Vaia R.A, Giannelis E. P. et al. Dynamics in a confined polymer electrolhyte: A 7Li and 2H NMR study. J. Am. Chem. Soc. 1995,117(28):7568～7569
47 王立新，赵金玲，任丽，刘盘阁，姬荣琴，聚吡咯／蒙脱土纳米复合材料的表征与复合机理．功能材料，2003，34(3)：325～327
48 Gabried C., Ossenkamp, et al. New approaches to surface-alkylated silica with increased hydrolytic stability. Chem. Mater 2002, from the internet
49 Eduardo R. H. Conducting polymers intercalated in layered solids. Adv. Mater 1993, 5:334～340