HPMA/OMMT和HPMA/CPMI/OMMT纳米复合材料的制备与表征

通过甲基丙烯酸羟丙酯(HPMA)单体与N-(4-羧基苯基)马来酰亚胺(CPMI)单体在有机蒙脱土(OMMT)中经原位插层自由基聚合反应制备了聚合物-无机纳米复合材料.OMMT由钠基蒙脱土通过十六烷基溴化铵插层处理制备.通过XRD和TEM对复合材料结构进行了表征,证实HPMA单体和HPMA/CPMI共单体在OMMT中原位插层共聚得到的复合材料均为剥离型纳米复合材料.OMMT含量为3 wt%的PolyHPMA/OMMT纳米复合材料起始分解温度为250℃,比相应的纯聚合物的热分解温度提高30℃.随着OMMT含量的增加,热分解温度进一步提高.但在测试温度范围内,PolyHPMA/OMMT纳米复合材料均没有出现明显的玻璃化转变温度.     

原位插层聚合制备聚丁二烯/蒙脱土纳米复合材料及其结构与性能研究

采用负离子引发原位插层聚合法制备了聚丁二烯(PB)/有机蒙脱土(OMMT)纳米复合材料(NC).对OMMT纯化方法、OMMT种类和溶剂等因素对聚合反应的影响进行了研究.不同方法纯化的OMMT消耗的BuLi量相差一倍;采用OMMT-DK1制备的NC具有较宽的分子量分布,而采用OMMT-DK1B和OMMT-DK4制备的NC则具有较窄的分子量分布;OMMT在环己烷中不溶解,在甲苯和二甲苯等溶剂中可形成均匀溶液.采用XRD、TEM和H-NMR等仪器对PB/OMMT NC的插层结构、化学结构和形态进行了分析;采用DSC、TGA和DMA等仪器对PB/OMMT NC的Tg、热学性能和动态力学性能进行了研究,结果表明,采用负离子原位插层聚合可得到剥离型PB/OMMT纳米复合材料;与OMMT插层复合明显改变了PB的微观结构组成,在OMMT含量为6.2wt%时,1,2-结构含量增加了近一倍,Tg和Tdc分别增加了10 K和16 K;E′、E″均明显提高,而tanδ下降.     

氢化丁腈橡胶/聚甲基丙烯酸镁/有机蒙脱土纳米复合材料制备及其耐介质老化性能

采用原位聚合和混炼插层相结合技术制备了氢化丁腈橡胶/聚甲基丙烯酸镁/有机蒙脱土(HNBR/PMgMA/OMT)纳米复合材料,通过XRD,SEM和TEM等测试方法研究了HNBR/PMgMA/OMT纳米复合材料的结构、形态和性能.PMgMA离子簇与未反应完全的MgMA单体形成纳米-微米共存形态结构,PMgMA对HNBR有显著的增强效果,HNBR/PMgMA/OMT纳米复合材料具有良好的加工性能、物理机械性能和耐介质老化性能.TEM结果显示MgMA/OMT并用有助于OMT剥离分散,有机蒙脱土在硫化胶中形成以剥离和插层为主、反插层和未插层共存的微观结构;SEM显示当MgMA/OMT用量为20/10份时能明显改善复合材料的界面结合,此时纳米复合材料的拉伸强度、扯断伸长率和扯断永久变形分别为30.2 MPa,520%和30%;同时具有优异的耐热空气和耐油老化性能,耐热水性能也明显改善,在165℃的热空气、水和油中长期老化14天的老化系数分别达到0.61,0.63和0.84,其耐介质老化性能明显好于炭黑增强HNBR硫化胶及HNBR/PMgMA复合材料.良好的蒙脱土片层分散结构是提高HNBR/PMgMA/OMT纳米复合材料耐介质老化性能的主要原因.     

聚苯乙烯/蒙脱土纳米复合材料的制备及结构研究

以可与苯乙烯发生共聚的阳离子表面活性剂乙烯苄基二甲基十八烷基氯化铵(VOAC)为插层处理剂改性蒙脱土(VC18-MMT),有机蒙脱土在超声波强剪切作用以及乳化剂作用下预分散在乳化剂溶液中,然后引入苯乙烯单体进行原位乳液聚合制备聚苯乙烯/蒙脱土纳米复合材料.采用XRD和TEM对纳米复合材料的结构进行了表征.结果表明,绝大多数的蒙脱土被剥离成单个片层均匀的分散在聚合物基体中;动态力学分析表明,纳米复合材料的储能模量和玻璃化温度均有所增加,而动态损耗有所降低;接枝在蒙脱土片层上的聚合物通过与锂离子进行阳离子交换反应提取下来,采用GPC和NMR对接枝聚合物的结构进行了表征,结果表明,接枝聚合物是较基体分子量低且分布很宽的苯乙烯和乙烯苄基二甲基十八烷基氯化铵的共聚物,计算表明每一个共聚物分子链上平均含有大约25个乙烯苄基二甲基十八烷基氯化铵分子.     

聚乙二醇／锂化蒙脱土溶液插层纳米复合的研究

通过溶液插层方法制备了聚乙二醇/锂化蒙脱土纳米复合材料。采用XRD、TEM、电子衍射、TGA及DTA对制得的材料进行了分析和表征。结果表明,聚乙二醇插入到锂化蒙脱土层中形成了具有良好离子导电性的纳米复合材料。     

聚丙烯/层状硅酸盐纳米复合材料的制备、结构和性能

聚丙烯／层状硅酸盐纳米复合材料可通过丙烯单体插层聚合、聚丙烯溶液插层和聚丙烯熔融插层等方法制备，得到插层型或剥离型纳米复合材料，形成了与传统填充型聚合物复合材料不同的微观结构，其机械性能，热性能，阻隔性能和流变性能等明显提高，由于聚丙烯的非极性及层状硅酸盐纳米复合材料制备方法的特殊性，该研究具有一定的理论价值。     

聚合物/粘土纳米复合材料中的粘土有机化

回顾了聚合物/粘土纳米复合材料中所用粘土的有机化方法与有机粘土的热稳定性,及其对复合材料性能的影响,指出在聚合物/粘土复合材料中粘土片层间距的变化同样有可能受到层间插层剂构象变化的影响、聚合物/粘土纳米材料的长期热氧稳定性与热失重结果可能不一致。     

原位插层聚合制备聚丁二烯/蒙脱土纳米复合材料的结构与性能研究

聚合物 /粘土纳米复合材料由于具有常规复合材料所没有的结构、形态及更优异的力学、热学、阻燃、阻隔等性能 ,自 1 987由日本丰田公司首次报道了制备尼龙 6 粘土纳米复合材料以来 ,立刻引起人们的普遍关注[1～ 17] .目前报道的聚合物 /粘土纳米复合材料主要集中在以树脂为基体 ,例如 ,聚酰胺[1～ 4] 、聚苯乙烯[5～ 8] 、聚甲基丙烯酸甲酯[9,10 ] 、聚丙烯[11,12 ] 等 .制备以橡胶为基体的橡胶/粘土纳米复合材料研究较少 ,采用的方法多为通过橡胶大分子插层 ,如熔融插层法[1 3] 、溶液插层法[14 ] 、乳液法[15,16] 等 ,这些方法均存在插层…     

Laponite/聚氨酯纳米复合材料制备与性能研究

通过溶剂交换法将无机Laponite从水相转移到N,N-二甲基乙酰胺(DMAC)中,在超声波作用下,Laponite与热塑性聚氨酯(TPU)溶液进行共混复合,Laponite插层到PU分子链间而制备Laponite/聚氨酯纳米复合材料.利用TEM,AFM,TGA,DSC,DMA和静态拉伸对其结构、组成、形貌和性能进行表征,研究结果表明,Laponite优先插层到聚氨酯的硬段中,片层和硬段通过氢键相互作用和尺寸匹配性,进而形成一种插层网络结构.由于这种网络结构的存在,使Laponite/聚氨酯复合材料的强度、硬度及韧性得到同步提高.     

茂钛催化剂苯乙烯原位间规聚合制备sPS/蒙脱土纳米复合材料

聚合物基纳米复合材料具有常规有机 /无机复合材料所没有的结构和形态 ,其性能较普通的聚合物复合材料更优异 ,因而引起人们的广泛关注 [1～ 4 ] .近年来的研究表明 ,运用插层聚合和熔融插层等方法可使某些具有层状结构的硅酸盐与聚合物产生特殊的界面作用 ,并以纳米尺寸均匀分     

Preparation,characterization and thermal behavior of poly(vinyl alcohol)/organic montmorillonite nanocomposites through solid-state shear pan-milling

In this study, the solid-state shear pan-milling was employed to prepare a series of polymer/layered silicate (PLS) nanocomposites. During the process of pan-milling at ambient temperature, poly(vinyl alcohol)/organic montmorillonite (PVA/OMMT) can be effectively pulverized, resulting in coexistence of intercalated and exfoliated OMMT layers. The obtained PLS nanocomposites were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). TEM analysis indicated that OMMT dispersed homogeneously in PVA matrix and XRD results illustrated that pan-milling had an obvious effect on increase in the interlayer spacing of OMMT, and resulted in coexistence of intercalated and exfoliated OMMT layers formed. Thermal gravimetric analysis showed that thermal stability of PVA was improved owing to the incorporation of OMMT. Thermal decomposition kinetics of PVA/OMMT nanocomposites with different milling cycles of OMMT was also studied. Two types of OMMT are chosen to compare the effect of hydrophilicity of OMMT on PVA/OMMT nanocomposites.     

本质阻燃聚苯乙烯/蒙脱土纳米复合物的制备及性能

通过原位聚合法制备了本质阻燃聚苯乙烯[P(St-co-AEPPA)]/有机改性蒙脱土(OMMT)纳米复合物[P(St-co-AEPPA)/OMMT], 并用普通聚苯乙烯/有机改性蒙脱土(PS/OMMT)复合物作为对比实验, 研究了含磷、氮单体丙烯酸羟乙基-苯氧基-二乙基磷酰胺(AEPPA)和OMMT等添加物对本质阻燃聚苯乙烯性能的影响.用X射线衍射仪(XRD)和透射电子显微镜(TEM)分析了复合材料的结构与形貌, 并对OMMT在基体中的分散机理进行了讨论.用差示扫描量热仪(DSC)、热重分析(TGA)和微型量热仪(MCC)研究了材料的热性能和燃烧性能.结果表明, AEPPA和OMMT能够显著提高基体的热稳定性和阻燃性.     

Preparation and characterization of poly(propylene carbonate)/montmorillonite nanocomposites by solution intercalation

Poly(propylene carbonate) (PPC) is a new biodegradable aliphatic polycarbonate. However, the poor thermal stability and low glass transition temperatures (T_g) have limited its applications. To improve the thermal properties of PPC, organophilic montmorillonite (OMMT) was mixed with PPC by a solution intercalation method to produce nanocomposites. An intercalated-and-flocculated structure of PPC/OMMT nanocomposites was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The thermal and mechanical properties of PPC/OMMT nanocomposites were investigated by thermal gravimetric analysis (TGA), differential scanning calorimetric (DSC), and electronic tensile tester. Due to the nanometer-sized dispersion of layered silicate in polymer matrix, PPC/OMMT nanocomposites exhibit improved thermal and mechanical properties than pure PPC. When the OMMT content is 4 wt%, the PPC/OMMT nanocomposite shows the best thermal and mechanical properties. These results indicate that nanocomposition is an efficient and convenient method to improve the properties of PPC.     

β-羟基丁酸与β-羟基戊酸共聚物 (PHBV)/蒙脱土纳米复合材料的结构与性能

用溶液复合法成功地制备了插层型PHBV／蒙脱土纳米复合材料。采用X射线衍射（XRD）和透射电子显微镜（TEM）研究了复合材料的结构，硅酸盐片层间距从1.8nm升至2.4nm左右。同时研究了复合材料的结晶，熔融，动态力学行为和力学性能，发现有机蒙脱土的加入，可以加快PHBV的结晶,降低熔融温度，使基体的玻璃化转变温度升高，提高了材料的力学性能，有机蒙脱土含量在3％时，其综合性能最佳。     

Structure Characterization and Thermal Properties of PMMA／Montmorillonite Nanocomposites via Emulsion Polymerization

Montmorillonite(MMT) modified with sodium silicate can change the arrangement of its layers fromedge-face and edge-edge to face-face. With the fine dispersion of the modified MMT in water, the cation-ex-change reaction was carried out with cetyltrimethyl ammonium bromide (CTAB) to obtain organo-montmoril-lonite (OMMT). As OMMT was uniformly dispersed in methyl methacrylate (MMA) monomer, PMMA/OMMT nanocomposites were formed via a common emulsion polymerization. The products were extractedwith hot acetone and characterized by FTIR, molecular weight, X-ray diffraction(XRD), transmission elec-tron microscopy(TEM), DSC and TGA. These results show that most of the OMMT layers have been exfo-liated, while the thermal stability is increased obviously. By means of FTIR spectral analysis, the ratios ofthe macromolecular radicals‘ termination of disproportionation patterns to combination are increased with theaddition of OMMT. This result further confirms the increase of the thermal degradation temperatures andglass transition temperatures of the PMMA/OMMT nanocomposites.     

Radiation-induced synthesis of vinyl copolymer based nanocomposites filled with reactive organic montmorillonite clay

Vinyl copolymer–clay nanocomposites were prepared by γ-irradiation-initiated radical polymerization using a mixture of styrene (St) and divinyl benzene (DVB) in the presence of reactive organic montmorillonite clay (OMMT) in methanol at room temperature. Reactive OMMT was synthesized by a cation exchange reaction of Na⁺-MMT and 1-[(4-ethylphenyl)methyl]-3-butyl-imidazolium chloride as a reactive organic modifier in an aqueous solution. The microstructures of the nanocomposites were confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The thermal stability was examined by thermo gravimetric analysis (TGA). As a result, the reactive OMMT was a good additive material for preparing vinyl copolymer–clay nanocomposites.     

COMPARISON OF POLYAMIDE 66/MONTMORILLONITE NANOCOMPOSITES PREPARED FROM POLYAMIDE 6 AND POLYAMIDE 66 BASED MASTER-BATCHES

Two master-batches,polyamide 66 (PA66)/organo-montmorillonite (OMMT) and polyamide 6 (PA6)/OMMT, prepared by melt compounding with methyl methacrylate (MMA) as co-intercalation agent,have been used to prepare nearly exfoliated PA661montmorillonite (MMT) nanocomposites.The resulting nanocomposites are compared in view of their morphology and properties.Nano-scale dispersion of OMMT is realized in both types of nanocomposites,as revealed by XRD,TEM and Molau tests.PA66/MMT nanocomposites having superior me...     

三元乙丙橡胶/蒙脱土纳米复合材料制备中硫化体系的比较

采用了熔融插层和两种硫化体系硫磺 促进剂和过氧化物体系制备了三元乙丙橡胶 蒙脱土纳米复合材料 ,并将这两种体系形成的纳米复合材料进行了形态、力学性能和光学性能的比较 ,同时采用Flory Rehner方程对它们的硫化行为进行了评价 .X射线衍射 (XRD)、透射电镜 (TEM)、力学性能和光学性能的测试结果表明 ,由硫磺硫化体系制备的纳米复合材料为不透明和剥离型 .其原有的d0 0 1 衍射峰消失 ,有序层被剥离成 10 0～ 2 0 0nm的片层均匀分散在EPDM基体中 ,其力学性能有了极大的提高 ;而过氧化物体系制备的纳米复合材料为半透明和插层型 .对两种体系的硫化行为的评价结果表明 ,随着有机蒙脱土加入量的增加 ,硫磺 促进剂硫化体系的t90 延长 ,交联密度减小 ,最大 最小转矩也变小 ;而过氧化物硫化体系的相应值却变化不大     

Effect of organo‐modified montmorillonite on flame retardant poly(1,4‐butylene terephthalate) composites

In this paper, the effect of organo‐modified montmorillonite (OMMT) on a novel intumescent flame retardant (IFR) system was studied in poly(1,4‐butylene terephthalate) (PBT) composites containing microencapsulated ammonium polyphosphate (MAPP) and melamine cyanurate (MC). Nanocomposite morphology was characterized by X‐ray diffraction (XRD) and transmission electron microscopy (TEM). Thermal decomposition analysis was studied via thermogravimetric analysis (TGA). Combustion behavior was investigated by microcombustion calorimeter (MCC), limited oxygen index (LOI), and UL‐94 test. Residues obtained after samples treated in muffle furnace at 500°C under air condition for 10 min were analyzed through X‐ray powder diffraction (XRD) and scanning electron microscopy (SEM). It was found that the addition of OMMT improved the flame retardancy of PBT/IFR composites significantly. A mass of microcomposite structure particles formed in the heating or combustion process of PBT/IFR/OMMT nanocomposites were found for the first time in the SEM images, which is strong evidence to confirm the migration or accumulation of montmorillonite and carbonaceous‐silicate materials during the heating or combustion process. Copyright © 2010 John Wiley & Sons, Ltd.