等离子体引发苯乙烯/马来酸酐共聚及其与聚丙烯的复合
摘要
本文实现了常温常压条件下低温等离子体引发苯乙烯(St)/马来酸酐(MAH)的共聚合反应,制备了St-MAH共聚物(SMA),并用FTIR和NMR对其结构进行了表征,结果表明,共聚合产物的分子结构以St和MAH的交替结构为主,并伴有少量无规结构。将自由基捕获剂DPPH引入该共聚合反应体系,发现二氧化碳,氩气等离子体引发St/MAH共聚合反应符合自由基反应特征。论文进一步研究了DBD放电条件下氩气、二氧化碳低温等离子体引发St和MAH共聚合的反应条件,结果显示,单体摩尔比对产率有较大影响,当St与MAH摩尔比为1:1时产率具有最大值,延长引发时间能够导致凝胶现象发生,从而大幅提高SMA的产率及其数均相对分子质量。相对于引发时间而言,后聚合时间和聚合温度对产率和数均相对分子量的影响不大。
将St-MAH共聚物体系与等离子体表面改性的聚丙烯(PPP)共混,制备了改性聚丙烯与St-MAH共聚物的共混物(PPP/SMA),并采用动态流变学方法研究了共混物的线性粘弹行为。结果表明,在实验温度范围内,PPP/SMA (80/20)共混物不同温度下的Han曲线均能很好地重合,且时温叠加原理也适用于本体系,证明PPP/SMA(80/20)共混物呈现均相相容体系的特征;不同SMA含量PPP/SMA共混物的零切粘度、储能模量、损耗模量等流变参数均明显高于PPP,且随着SMA含量增加而增加,表明共混体系内PPP和SMA间可能存在源于低温等离子体引发聚合的复杂的相互作用。
In this dissertation, the copolymerization of styrene (St) with maleic anhydride(MAH) under room temperature and atmosphere was completed by the plasma of ArandCO2initiationinthedielectricbarrierdischarge(DBD).Thechemical structureofcopolymer(SMA) was characterizedbyFTIR andNMR,showingSMAwas alternatecopolymer and random copolymer in a little part. The radical polymerization in thecopolymerization of St with MAH was proved by radical scavenger, DPPH. Thereactive conditions in the copolymerization of St with MAH were studied by theplasma of Ar and CO2 initiation under DBD. The variation of the rate production ofSMA with molar ratio was discussed, showing the rate production of SMA existedmaximum when molar ratio was 1:1. The gel should be formatted with increasinginitiation time in the copolymerization, leading to increasing rate production of SMAand number average molecular weight. In this experiment, the effect of postpolymerization time and temperature were small as compared with the effect of theinitiationtimeonrateproductionandmolecularweightofSMA.
In this work, the modification of surface for PPwas studied byplasma. Also themixingof SMAwith modified PP(PPP) was studied. The linear viscoelastic behaviorof PPP/SMAcompound was measured by the dynamic rheology method. Han curveswere coincident, showing this system (PPP/SMAcompound system) was uniform, asthe chemical-bound was formed between PPP and SMA in this compound. Also theexperiment of time-temperature superposition principle showed PPP/SMA systemhomogeneous system. The zero shear viscosity,η0 , storage modulus,G?, and lossmodulus,G?? , increase with increasing component of SMAand they was greater thanPPP. So the complex chemical-bound was arose between PPPand SMAin PPP/SMAstructurebecausethereactionofplasmainitiationtoleadtonewpolymer.
将St-MAH共聚物体系与等离子体表面改性的聚丙烯(PPP)共混,制备了改性聚丙烯与St-MAH共聚物的共混物(PPP/SMA),并采用动态流变学方法研究了共混物的线性粘弹行为。结果表明,在实验温度范围内,PPP/SMA (80/20)共混物不同温度下的Han曲线均能很好地重合,且时温叠加原理也适用于本体系,证明PPP/SMA(80/20)共混物呈现均相相容体系的特征;不同SMA含量PPP/SMA共混物的零切粘度、储能模量、损耗模量等流变参数均明显高于PPP,且随着SMA含量增加而增加,表明共混体系内PPP和SMA间可能存在源于低温等离子体引发聚合的复杂的相互作用。
In this dissertation, the copolymerization of styrene (St) with maleic anhydride(MAH) under room temperature and atmosphere was completed by the plasma of ArandCO2initiationinthedielectricbarrierdischarge(DBD).Thechemical structureofcopolymer(SMA) was characterizedbyFTIR andNMR,showingSMAwas alternatecopolymer and random copolymer in a little part. The radical polymerization in thecopolymerization of St with MAH was proved by radical scavenger, DPPH. Thereactive conditions in the copolymerization of St with MAH were studied by theplasma of Ar and CO2 initiation under DBD. The variation of the rate production ofSMA with molar ratio was discussed, showing the rate production of SMA existedmaximum when molar ratio was 1:1. The gel should be formatted with increasinginitiation time in the copolymerization, leading to increasing rate production of SMAand number average molecular weight. In this experiment, the effect of postpolymerization time and temperature were small as compared with the effect of theinitiationtimeonrateproductionandmolecularweightofSMA.
In this work, the modification of surface for PPwas studied byplasma. Also themixingof SMAwith modified PP(PPP) was studied. The linear viscoelastic behaviorof PPP/SMAcompound was measured by the dynamic rheology method. Han curveswere coincident, showing this system (PPP/SMAcompound system) was uniform, asthe chemical-bound was formed between PPP and SMA in this compound. Also theexperiment of time-temperature superposition principle showed PPP/SMA systemhomogeneous system. The zero shear viscosity,η0 , storage modulus,G?, and lossmodulus,G?? , increase with increasing component of SMAand they was greater thanPPP. So the complex chemical-bound was arose between PPPand SMAin PPP/SMAstructurebecausethereactionofplasmainitiationtoleadtonewpolymer.
引文
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[3]陈杰瑢,低温等离子体化学及其应用,北京:科学出版社,2001,5-12
[4]孟月东,钟少锋,熊新阳,低温等离子体技术应用研究进展,物理2006,35(2):140-146
[5] AnnemieBogaerts,ErikNeyts,RenaatGijbels,etal,Gasdischargeplasmaandtheirapplications,SpectrochimicaActa,PartB,2002,57:609-658
[6]郭楚,聚丙烯,聚苯乙烯表面等离子体改性及其合金化的研究:[硕士毕业论文],天津;天津大学,2007
[7]许根慧,姜恩永,盛京等.等离子体技术与应用,北京:化学工业出版社,2006,19-23
[8] Yao, S. Li., Nakayama A., Suzuki E., Methane conversion Using aHigh-Frequency Pulsed Plasma: Important Factors, AICHE J., 2001, 47(2):413-418
[9] Yasuda H., Hirotsu T., Distribution of polymer deposition in plasmapolymerzation. I. Acetylene, Ethylene and the effect of carrier gas, J. ofPolymerSci.,1978,16,229-241
[10]王雪梅,沈宁祥,盛京,等离于体引发聚合及其研究进展,河北化工,2002,2:9-13
[11] Johnson D.R., Y.Osada, A.T.Bell et al, Studies of the mechanism and kineticsof plasma-initiated polymerization of methyl methacrylate, Macromolecules,1981,14:118-124
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[18] Osada, Yoshihito, Preparation, structure and electric properties ofplasma-polymerized metal-containing organic thin films, Polymeric MaterialsScience and Engineering, Proceedings of the ACS Division of PolymericMaterialsScienceandEngineering,1990,62,533-537
[19] Barron P R, Hill D J T, O'Donnell J H. Applications of DEPT experiments tothe carbon -13NMR of copolymers: poly(styrene-co-maleic anhydride) andpoly(styrene-co-acrylonitrile),Macromolecules,1984,17:1967-1972
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[21] BenoitD,HawkerCJ,HuangEE,etal,One-StepFormationofFunctionalizedBlockCopolymers,Macromolecules,2000,33:1505-1507
[22] De Brouwer H, Schellekens M A J, Klumperman B, et al, Controlled radicalcopolymerization of styrene and maleic anhydride and the synthesis of novelpolyolefin-based block copolymers by reversible addition-fragmentationchain-transfer (RAFT) polymerization, Polym. Sci. Part A: Polym. Chem,2000,38:3596-603
[23] Zhu M Q, Wei L H, Li M, et al. A unique synthesis of a well-defined blockcopolymer having alternating segments constituted by maleic anhydride andstyrene and the self-assembly aggregating behavior thereof, Chem Commun,2001,40:365-366
[24] Wu D C, Hong C Y, Pan C Y, et al. Study on controlled radical alternatingcopolymerization of styrene with maleic anhydride under UV irradiation,Polym.Int,2003,52:98-103
[25] RaetzschM,SchichtG.,Acta.Polym,1980,31:419-423
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[28] Anayei R A, ODriscoll K F, Klumperman B. Pulsed laser copolymerization ofstyreneandmaleicanhydride,Macromolecules,1994,27:5577-5582
[29] QiuGuangming,ZhuKubao,XuYou yietal.Synthesisofultrahighmolecularweight poly(styrene-alt-maleic anhydride) in supercritical carbon dioxide,Macromolecules,2006,39(9):3231-3237
[30]王亚,无水氯化铝原位催化增容聚丙烯/聚苯乙烯共混物的研究,[博士学位论文],天津;天津大学材料学院,2008
[31] Macaubas P H P, Demarquette N R. Morphologies and interfacial tensions ofimmiscible polypropylene/polystyrene blends modified with triblockcopolymer,Polymer,2001,42:2543-2554
[32] Diaz M. F., S. E. Barbosa, N. J. Capiati, Polyethylene-Polystyrene graftingreaction: effects of polyethylene molecular weight, Polymer, 2002,43:4851-4858
[33] Sun YJ, Richard J G W, Liu T M et al, In situ compatibilization of polyolefinand polystyrene using Friedel-Crafts alkylation through reactive extrusion,Polymer,1998,39(1):2201-2208
[34] HuangC.Y.,C.L.Chen,Theeffectofplasmasurfacemodificationfromarotaryplasma reactor on the styrene grafting onto a polypropylene surface, SurfaceandCoatingsTechnology,2002,153:194-202
[35] Vahdat A. , Hajir Bahrami, N. Ansari et al, Radiation grafting of styrene ontopolypropylene fibres by a 10 MeV electron beam, Radiation Physics andChemistry
[36] FredericksP.M.,IKeen,G.A.George,Selectiveplasma-inducedgraftingofpolystyreneontopolyolefinblends,Journalofappliedpolymerscience,2003,88: 1643-1652
[37] OmonovT.S.,CHarrats,GGreoninckxetal,Anisotropyandinstabilityoftheco-continuousphasemorphologyinuncompatibilizedandreactivelycompatibilizedpolypropylene/polystyreneblends,Polymer,2007,48:5289-5302
[38] Potschke P, Malz H, Pionteck J Influence of interfacial reaction onmorphology in modified PP/PS blends, Macromolecular Symposia, 2000,149:231-246
[39] You Q L, Wang JH, Meng Y D et al, A novel continuously initiatedpolymerization by one- atmosphere low temperature plasma device, Plasmascienceandchemistry,2005,7(2):2758-2760
[40]房江华,黄士力,沈之荃等,Fe-Al络合催化苯乙烯-马来酸酐交替共聚,高分子学报,1999,4:465-469
[41] George B Butler, Choon H. Do, Michael C, Zerner. The Stereochemistry ofStyrene-Maleic Anhydride Copolymers: 13C-NMR Study andCalculations,Macromol.Sci.Chem.,1989,26(8):1115-1135
[42] Maurizio S. Montaudo, Determination of the Compositional Distribution andCompositional Drift in Styrene/Maleic Anhydride Copolymers,Macromolecules,2001,34(9):2792-2797
[43] Peter F. Barron, David J. T. Hill, James H, Applications of DEPT experimentsto the carbon-13 NMR of copolymers: poly(styrene-co-maleic anhydride) andpoly(styrene-co-acrylonitrile),Macromolecules,1984,17(10):1967-1972
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