反应器颗粒技术聚丙烯接枝物制备、性能及应用的研究
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摘要
本文多孔的反应器颗粒技术聚丙烯为接枝基体,以过氧化苯甲酰为引发剂,通过悬浮接枝聚合与固相接枝聚合的方法,制备出具有高接枝率及高接枝效率的聚丙烯接枝物。详细探讨了水相悬浮接枝聚合的反应特点及反应机理,研究了聚丙烯接枝物在与极性聚合物共混、与无机粒子复合方面的应用。主要研究结果如下：
1,对于水相悬浮接枝聚甲基丙烯酸甲酯体系,接枝率随着反应体系之中单体含量的增多而逐渐增大。当以甲基内烯酸甲酯为单一接枝单体时,接枝率最高能够达到13.6%;接枝效率随着反应体系之中单体含量的增多而逐渐减小,并可控制在61.8%到78.0%之间。第二单体苯乙烯的加入能够提高水相悬浮接枝聚合的接枝率,最高可达24.5%。随着反应体系之中引发剂含量的增加,接枝率先增大而后开始降低,接枝效率却逐渐降低。经过丙酮抽提之后的接枝物的傅立叶红外谱图中1734cm-1处的羰基的特征吸收峰明显,说明甲基丙烯酸甲酯成功接枝到聚丙烯分子链上。随着接枝率的升高,接枝物的熔融指数呈现出先升高后降低的趋势,相对结晶度与熔点则逐渐降低,剪切黏度逐渐升高。扫描电子显微镜显示接枝链能够渗透到聚丙烯的微孔之重,包围在聚丙烯次级粒子周围;透射电子显微镜显示熔融密炼之后的接枝物中,聚甲基丙烯酸甲酯相仍然能够良好分散在聚丙烯之中,直径小于1微米。接枝物在聚丙烯与丙烯腈-苯乙烯-丙烯酸酯共聚物的共混中能够起到大分子相容剂的作用。
2,对于水相悬浮接枝聚丙烯酸丁酯体系,接枝率随反应体系中单体含量的增多逐渐升高到32.6%；与此同时接枝效率逐渐从86.1%下降到78.3%。随着引发剂增多,接枝率起初升高明显,之后逐渐平缓；而接枝效率则逐渐下降。交联剂三乙二醇二丙烯酸酯的加入能够提高接枝率,最高到36.3%。接枝率小于7.4%时,熔融指数随接枝率的升高而升高,之后随着接枝率的升高,熔融指数开始迅速降低。随着交联剂的增多,熔融指数逐渐下降。随着接枝率的升高,接枝物的相对结晶度与熔点都逐渐降低。动态力学热分析显示接枝物的储能模量随着接枝率的升高而逐渐降低,力学损耗显示聚丙烯酸丁酯与聚丙烯的玻璃化转变温度分别为-50℃与10℃,交联剂的加入使得聚丙烯酸丁酯与聚丙烯的玻璃化转变温度相互靠近。随着接枝率的升高,接触角从纯PP的102.6°逐渐下降95.1°。透射电子显微镜显示聚丙烯酸丁酯能够以直径大约500纳米均匀分散在聚丙烯基体之中,交联剂三乙二醇二丙烯酸酯的加入使得聚丙烯与聚丙烯酸丁酯两相逐渐融合,无明显的两相结构。
3,对于固相接枝聚(苯乙烯-马来酸酐)接枝物制备二氧化硅复合物体系,复合物中二氧化硅含量与溶胶-凝胶反应中正硅酸乙酯的含量成正比。通过电子显微镜观察,以接枝物为基体制备的二氧化硅复合物中,二氧化硅以10纳米至20纳米的尺寸均匀分散在聚丙烯中；以纯聚丙烯为基体时,二氧化硅则团聚结块。纳米二氧化硅的加入,降低了聚丙烯的结晶尺寸,提高了结晶速率,促进了β型结晶的生成。当纳米二氧化硅含量超过4.39wt%时,可见光透过率可达85%以上。纳米二氧化硅对聚丙烯的机械性能的提高作用明显。
A facile, green, versatile protocol to prepare poly(propylene) based grafting copolymer with high grafting percentage (GP) and grafting efficiency (GE), in which the porous poly(propylene) particles produced by Reactor Granule Technology as reaction bed, was developed using water-solid phase suspension grafting or solid phase grafting. The reaction mechanism of water-solid phase suspension grafting was discussed, and so does the application of grafting copolymer in poly(propylene) blends. The main research results were listed as followed:
1. In the system of water-solid phase suspension grafting of methyl methacrylate (MMA), grafting percentage increased with the increasing of the monomer ratios and which could reach13.6%. While the grafting efficiency decreased from78.0%to61.8%as the monomer ratio increased. A second monomer styrene improved grafting percentage up to24.5%. Along with the increasing of initiator, GP first increased and then decreased, and GE always decreased. FTIR spectra of the samples after extraction by acetone demonstrated that PMMA was successfully grafted onto poly(propylene). TEM micrographs demonstrated PMMA domains distributed in PP with sizes ranging less than1μm. It was found that PP-g-PMMA was effective in improving the compatibility of PP and acrylonitrile-styrene-acrylate blends.
2. In the system of water-solid phase suspension grafting of butyl acrylate (BA), GP could reach to32.6%along with the increasing of monomer ratio, and GE would decrease from86.1%to78.3%at the same time. The crosslinking agent, triethylene glycol diacrylate (TEGDA), could improve GP as high as36.3%. Melt flow index (MFI) of the grafting compolymer would increase as the increasing of GP when it was less than7.4%, and a further increasing of GP would decrease MFI rapidly. Dynamic mechanical thermal analysis showed that the storage modulus decreased as the increasing of GP. The contact angle demonstrated that the grafting chains could improve the polarity of PP. TEM photos showed that the PBA domains distributed in PP with sizes about500nm.
3. In the system of PP/silica nanocomposites using solid phase grafting of styrene and maleic anhydride as reaction loci, the silica content increased with the increasing of tetraethyl orthosilicate (TEOS). SEM and TEM micrographs demonstrated that silica nanoparticles would fine disperse in PP with the diameter of10-20nm. The DSC tests showed that the existence of silica nanoparticles accelerated the generation of PP crystal nucleus during cooling; meanwhile, it urged generation of double melting peaks under rapid cooling which demonstrated β-form crystalline and recrystallization occurred in the heat-cool-heat cycles. The transmittance of visible light could increase from80-85%to87.5-90%in the case of neat PP and silica content of4.39wt%, respectively. And the mechanical properties of the composites were improved significantly.
1,对于水相悬浮接枝聚甲基丙烯酸甲酯体系,接枝率随着反应体系之中单体含量的增多而逐渐增大。当以甲基内烯酸甲酯为单一接枝单体时,接枝率最高能够达到13.6%;接枝效率随着反应体系之中单体含量的增多而逐渐减小,并可控制在61.8%到78.0%之间。第二单体苯乙烯的加入能够提高水相悬浮接枝聚合的接枝率,最高可达24.5%。随着反应体系之中引发剂含量的增加,接枝率先增大而后开始降低,接枝效率却逐渐降低。经过丙酮抽提之后的接枝物的傅立叶红外谱图中1734cm-1处的羰基的特征吸收峰明显,说明甲基丙烯酸甲酯成功接枝到聚丙烯分子链上。随着接枝率的升高,接枝物的熔融指数呈现出先升高后降低的趋势,相对结晶度与熔点则逐渐降低,剪切黏度逐渐升高。扫描电子显微镜显示接枝链能够渗透到聚丙烯的微孔之重,包围在聚丙烯次级粒子周围;透射电子显微镜显示熔融密炼之后的接枝物中,聚甲基丙烯酸甲酯相仍然能够良好分散在聚丙烯之中,直径小于1微米。接枝物在聚丙烯与丙烯腈-苯乙烯-丙烯酸酯共聚物的共混中能够起到大分子相容剂的作用。
2,对于水相悬浮接枝聚丙烯酸丁酯体系,接枝率随反应体系中单体含量的增多逐渐升高到32.6%；与此同时接枝效率逐渐从86.1%下降到78.3%。随着引发剂增多,接枝率起初升高明显,之后逐渐平缓；而接枝效率则逐渐下降。交联剂三乙二醇二丙烯酸酯的加入能够提高接枝率,最高到36.3%。接枝率小于7.4%时,熔融指数随接枝率的升高而升高,之后随着接枝率的升高,熔融指数开始迅速降低。随着交联剂的增多,熔融指数逐渐下降。随着接枝率的升高,接枝物的相对结晶度与熔点都逐渐降低。动态力学热分析显示接枝物的储能模量随着接枝率的升高而逐渐降低,力学损耗显示聚丙烯酸丁酯与聚丙烯的玻璃化转变温度分别为-50℃与10℃,交联剂的加入使得聚丙烯酸丁酯与聚丙烯的玻璃化转变温度相互靠近。随着接枝率的升高,接触角从纯PP的102.6°逐渐下降95.1°。透射电子显微镜显示聚丙烯酸丁酯能够以直径大约500纳米均匀分散在聚丙烯基体之中,交联剂三乙二醇二丙烯酸酯的加入使得聚丙烯与聚丙烯酸丁酯两相逐渐融合,无明显的两相结构。
3,对于固相接枝聚(苯乙烯-马来酸酐)接枝物制备二氧化硅复合物体系,复合物中二氧化硅含量与溶胶-凝胶反应中正硅酸乙酯的含量成正比。通过电子显微镜观察,以接枝物为基体制备的二氧化硅复合物中,二氧化硅以10纳米至20纳米的尺寸均匀分散在聚丙烯中；以纯聚丙烯为基体时,二氧化硅则团聚结块。纳米二氧化硅的加入,降低了聚丙烯的结晶尺寸,提高了结晶速率,促进了β型结晶的生成。当纳米二氧化硅含量超过4.39wt%时,可见光透过率可达85%以上。纳米二氧化硅对聚丙烯的机械性能的提高作用明显。
A facile, green, versatile protocol to prepare poly(propylene) based grafting copolymer with high grafting percentage (GP) and grafting efficiency (GE), in which the porous poly(propylene) particles produced by Reactor Granule Technology as reaction bed, was developed using water-solid phase suspension grafting or solid phase grafting. The reaction mechanism of water-solid phase suspension grafting was discussed, and so does the application of grafting copolymer in poly(propylene) blends. The main research results were listed as followed:
1. In the system of water-solid phase suspension grafting of methyl methacrylate (MMA), grafting percentage increased with the increasing of the monomer ratios and which could reach13.6%. While the grafting efficiency decreased from78.0%to61.8%as the monomer ratio increased. A second monomer styrene improved grafting percentage up to24.5%. Along with the increasing of initiator, GP first increased and then decreased, and GE always decreased. FTIR spectra of the samples after extraction by acetone demonstrated that PMMA was successfully grafted onto poly(propylene). TEM micrographs demonstrated PMMA domains distributed in PP with sizes ranging less than1μm. It was found that PP-g-PMMA was effective in improving the compatibility of PP and acrylonitrile-styrene-acrylate blends.
2. In the system of water-solid phase suspension grafting of butyl acrylate (BA), GP could reach to32.6%along with the increasing of monomer ratio, and GE would decrease from86.1%to78.3%at the same time. The crosslinking agent, triethylene glycol diacrylate (TEGDA), could improve GP as high as36.3%. Melt flow index (MFI) of the grafting compolymer would increase as the increasing of GP when it was less than7.4%, and a further increasing of GP would decrease MFI rapidly. Dynamic mechanical thermal analysis showed that the storage modulus decreased as the increasing of GP. The contact angle demonstrated that the grafting chains could improve the polarity of PP. TEM photos showed that the PBA domains distributed in PP with sizes about500nm.
3. In the system of PP/silica nanocomposites using solid phase grafting of styrene and maleic anhydride as reaction loci, the silica content increased with the increasing of tetraethyl orthosilicate (TEOS). SEM and TEM micrographs demonstrated that silica nanoparticles would fine disperse in PP with the diameter of10-20nm. The DSC tests showed that the existence of silica nanoparticles accelerated the generation of PP crystal nucleus during cooling; meanwhile, it urged generation of double melting peaks under rapid cooling which demonstrated β-form crystalline and recrystallization occurred in the heat-cool-heat cycles. The transmittance of visible light could increase from80-85%to87.5-90%in the case of neat PP and silica content of4.39wt%, respectively. And the mechanical properties of the composites were improved significantly.
引文
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