地聚物/聚氯乙烯复合材料的制备及性能研究
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摘要
地质聚合物(简称地聚物,Geopolymer)是一种由[A104]和[SiO4]四面体构成具有三维非晶结构的铝硅酸盐无机聚合物,主要制备原料为铝硅酸盐矿物及固体工业废弃物等。地聚物具有强度高、耐腐蚀、耐水、耐高温、固封金属离子等许多优点,但其材料最大的缺点是“脆”,由此对地聚物进行增韧改性的研究比较活跃。
聚氯乙烯(简称PVC)是五大通用热塑性树脂之一,因其具有柔韧的分子链,优良的综合性能,其材料的应用已涉及到各种领域。如果将高韧性聚氯乙烯树脂与地聚物脆性材料复合,将会大大提高地聚物材料的韧性；同时地聚物的存在也会提高聚氯乙烯树脂的高温稳定性。基于上述思想,本文系统研究了地聚物/聚氯乙烯复合材料的高温制备工艺,并对复合材料的性能进行了表征和应用探索。
研究中采用偏高岭土、水玻璃、片碱等制备纯地聚物,并对地聚物的制备工艺参数进行优化,获得力学性能优良的基体材料；利用聚氯乙烯具有有机高分子柔性分子链特征,通过塑炼压制法对地聚物进行增韧改性。另外,研究中利用地聚物无机刚性粒子和耐高温的优点,经共混法和原位聚合法对PVC进行了改性,并将其研究成果应用于PVC片材的制备中。其研究结果如下：
(1)在纯地聚物的制备过程中,研究了地聚物在高温条件下的流变学特性、固化时间、微观结构和力学性能。结果表明,以地聚物的强度为依据,确定了地聚物中各氧化物摩尔比：n(SiO2)/n(Al2O3)=3.3,n(Na2O)/n (SiO2)=0.27,n(H2O)/n(Na2O)=11.0,最佳工艺参数为：水玻璃陈化时间24h,养护温度60℃,养护时间48h等工艺控制条件。由此制备的28d地聚物抗压强度、抗弯强度高达89.63MPa、13.87MPa。高温成型研究结果显示,170℃时,地聚物浆体的初凝和终凝时间分别为11和16分钟,增大水钠比为14后,其浆体的凝结时间延长；升高养护温度可提高地聚合反应速度并缩短浆体的硬化时间；流变性能研究发现在地聚物成型加工中施加一定的剪切力,有利于地聚物材料的流动成型。
(2)PVC对地聚物的增韧改性(PVC小于50wt%),是在地聚物网络结构形成之前加入PVC,在塑炼加工作用下使熔融态的PVC分子链与正在发生地质聚合反应的浆料共混,形成互穿网络的地聚物复合材料。通过高温流变学测试,发现当PVC含量小于50wt%时,由于PVC贡献的粘性特征被大量的地聚物贡献的弹性响应掩盖,导致复合材料模量越来越大,整个复合材料表现出地聚物的固体特征。其高温加工成型工艺参数如下：塑炼温度为170℃,塑炼时间为5分钟,塑炼后的薄片在170℃,15MPa的压力下,保温保压7分钟。PVC增韧地聚物复合材料的机械强度检测结果表明,复合材料的抗弯强度随PVC含量的增加而增大,PVC加入量为50wt%时,复合材料的抗弯强度达到67.06MPa,比纯地聚物28d龄期的抗弯强度提高了3.73倍。
(3)地聚物增韧PVC的共混改性方法(PVC大于50wt%),则是在地聚物形成的未固化阶段,将正在进行地聚合反应的浆体加入PVC树脂中,在共混物的塑炼压制加工过程中,正在形成的地聚物网络结构与己解缠绕而伸展的PVC分子链之间存在较好的结合,从而增强了地聚物与基体PVC的界面作用。力学性能测试结果表明,与纯PVC相比,地聚物含量在10wt%以内时,复合材料有较好的力学性能,其中以4wt%为最佳,其材料的抗冲击强度达到了9.13KJ·m-2,比纯PVC材料提高了约40%。维卡软化、热重分析、差示扫描量热法表征结果表明,与纯PVC相比较,复合材料的维卡软化温度提高了2-6℃,地聚物的加入对PVC分子链缺陷结构脱HC1具有吸收和抑制的作用,从而提高了地聚物/PVC复合材料的热稳定性。
(4)原位聚合法地聚物/PVC复合材料的制备,是将经硅烷偶联剂有机化改性的地聚物和氯乙烯单体,采用倒加料工艺经原位聚合生成地聚物/PVC复合树脂,然后经塑炼压制制备出复合材料。研究了地聚物对悬浮聚合体系的温度、压力、转化率、搅拌电流等参数的影响。力学性能检测结果表明,在地聚物含量为3wt%时,与纯PVC相比,复合材料抗冲击强度提高了59.4%,拉伸强度提高了13.8%,断裂伸长率提高了7.65%。由Kissinger法所计算的热分解活化能表明,原位聚合法地聚物/PVC复合材料和纯PVC材料的反应表观活化能分别为274.78J.mol-1和152.06J.mol-1地聚物/PVC的热分解活化能明显高于PVC的热分解活化能,证明地聚物的引入提高了PVC基体树脂的分解活化能,表明其热稳定性得以提高。
(5)在上述研究的基础上,将不同量的地聚物与PVC熟料充分混合后应用到PVC片材的生产过程中,在保证复合材料力学性能的前提下,使复合片材成本大大降低,耐老化性能得到提高。
Geopolymer is a kind of three dimensional structure aluminum silicate inorganic polymer composed by the [AlO4] and [SiO4] tetrahedron, which was mainly preparared by aluminum silicate or industrial waste. Geopolymer has high strength, corrosion resistance, water resistance, high temperature resistance, enclosed metal ion, and many other advantages, but its typical defect is "brittle", so toughening modification of geopolymer is more active.
Polyvinyl chloride (PVC) is one of the five biggest common thermoplastic resins, because it has flexible molecular chain, excellent comprehensive performance, the application of PVC material has related to various fields. If the high toughness PVC resin is compounded with brittle geopolymer materials, which will greatly improve toughness of geopolymer material, simultaneously geopolymer will also improve high temperature performanceresin of PVC. Based on the above ideas, this dissertation systematically studied thepreparation technology at high temperature of geopolymer/polyvinyl chloride (PVC) composites, and the performances of the composites were characterized and explored.
In the dissertation, pure geopolymer was prepared with metakaolin, sodium silicate, sheet alkali and water, and the preparation technology parameters of geopolymer were also optimized. Moreover, geopolymer matrix materials with high mechanics performance were prepared. geopolymer was toughened by polyvinyl chloride (PVC) with organic polymer flexible molecular chain characteristics, through the plasticate pressing method. In addition, with the characteristic of inorganic rigid particles and high temperature resistance for the geopolymer, PVC was modified by the blending method and in situ polymerization, and the research results were used in the preparation of PVC sheets. The research results are as follows:
(1) In the pure geopolymer preparation process, the rheological properties, curing time, microstructure and mechanical properties of geopolymer under the high temperature condition were studied. The results showed that, according to the strength of the geopolymer as the basis, the optimum proportion and technological parameters of geopolymer was determined as:the molar ratio of (SiO2)/(Al2O3) was3.3, the molar ratio of (Na2O)/(SiO2) was0.27, the molar ratio of (H2O)/(Na2O) was11, and the aging time of sodium silicate was24h, the curing temperature was60℃, the curing time was48h. So the strength of geopolymer reached to the highest,28d compressive strength and folding strength of geopolymer reached to89.63MPa,13.87MPa, respectively. High temperature moulding results showed that170℃,the initial setting time and final setting time of geopolymer slurry were11and16minutes, respectively. After the water sodium ratio of geopolymer was increased (14), the condensation time of geopolymer slurry extended. The reaction heat of geopolymer reflected that the increase of curing temperature could improve polymerization reaction rate and shorten the slurry setting time. Rheological properties showed that exerting shear force in polymer processing during the high temperature moulding process was helpful for flow moulding of geopolymer materials.
(2)Toughening modification of geopolymer was used PVC during the network structure process of geopolymer, because molten PVC molecular chain and polymerization of geopolymer worked together, which formed interpenetrating network of geopolymer composites. Through the high temperature rheology test, it was found that when PVC content was less than50wt%, the modulus of composites was bigger and bigger and the whole composites were characteristic of solid features of geopolymer because the contribution of the viscous features of PVC have been covered by the contribution of the elastic response. Its processing parameters were as follows: plastification temperature of PVC was175℃, plastification time of PVC was6minutes, heat preservation time was10minutes after plasticated under170℃,15MPa. The mechanical strength results of geopolymer toughened by showed that the28d bending strength reached to55.87MPa when the addition of PVC was40wt%, which was improved by3.1times compared with that of the pure geopolymer.
(3) The toughening modification of PVC was joined the geopolymer slury into PVC resin under coagulation stage of geopolymer, whose network structure was bonded by winding PVC molecular chain, resulting in enhancing the geopolymer and matrix PVC interface effect. Mechanics performance test results showed that, the geopolymer composites had good mechanical properties when geopolymer content was less then10wt%compared with pure PVC, of which4wt%content geopolymer was the optimum, and the impact strength of the PVC based composites reached to9.13KJ·m-2, which increased by40%compared with that of pure PVC. Vicat softening, thermogravimetric analysis, differential scanning calorimetry characterization results of PVC based composites showed that, vicat softening temperature increased by2-6℃compared with that of pure PVC. After geopolymer was joined into PVC, thermal stability of the Geolymer/PVC composites was enhanced because geopolymer inhibited and absorbed the releases of the HCl from PVC resulting from the molecular chain defect structure of PVC.
(4) In situ polymerization of Geolymer/PVC composites was prepared with geopolymer modfied by silane coupling agent organic and vinyl chloride monomer through the fall loading process by in situ polymerization, and then by plasticated pressing.The temperature, pressure, conversion, stirring electric current of suspension polymerization system were studied. Mechanical properties testing results showed that the impact strength of Geolymer/PVC composites increased by59.4%, the tensile strength of Geolymer/PVC composites increased by13.8%, the elongation at break of Geolymer/PVC composites increased by7.65%compared with that of pure PVC when the geopolymer content was3wt%. The thermal decomposition activation energy calculated by Kissinger method showed that apparent activation energy of PVC/polymer composite by in situ polymerization and pure PVC material were274.78J·mol-1and152.06J·mol-1, respectively. The thermal decomposition activation energy of Geolymer/PVC was obviously higher than that of the PVC,which proved that the introduction of geopolymer improved the decomposition activation energy of PVC matrix resin and showed that its thermal stability was improved.
(5) According to the above research conclusion, different amount of geopolymer were mixing fully with PVC and applied in PVC sheet production process, the mechanical properties of PVC composites were higher than that of the pure PVC sheets. In addition, aging resistance of PVC composite was greatly increased and significantly improved the durability of PVC sheets composites.
聚氯乙烯(简称PVC)是五大通用热塑性树脂之一,因其具有柔韧的分子链,优良的综合性能,其材料的应用已涉及到各种领域。如果将高韧性聚氯乙烯树脂与地聚物脆性材料复合,将会大大提高地聚物材料的韧性；同时地聚物的存在也会提高聚氯乙烯树脂的高温稳定性。基于上述思想,本文系统研究了地聚物/聚氯乙烯复合材料的高温制备工艺,并对复合材料的性能进行了表征和应用探索。
研究中采用偏高岭土、水玻璃、片碱等制备纯地聚物,并对地聚物的制备工艺参数进行优化,获得力学性能优良的基体材料；利用聚氯乙烯具有有机高分子柔性分子链特征,通过塑炼压制法对地聚物进行增韧改性。另外,研究中利用地聚物无机刚性粒子和耐高温的优点,经共混法和原位聚合法对PVC进行了改性,并将其研究成果应用于PVC片材的制备中。其研究结果如下：
(1)在纯地聚物的制备过程中,研究了地聚物在高温条件下的流变学特性、固化时间、微观结构和力学性能。结果表明,以地聚物的强度为依据,确定了地聚物中各氧化物摩尔比：n(SiO2)/n(Al2O3)=3.3,n(Na2O)/n (SiO2)=0.27,n(H2O)/n(Na2O)=11.0,最佳工艺参数为：水玻璃陈化时间24h,养护温度60℃,养护时间48h等工艺控制条件。由此制备的28d地聚物抗压强度、抗弯强度高达89.63MPa、13.87MPa。高温成型研究结果显示,170℃时,地聚物浆体的初凝和终凝时间分别为11和16分钟,增大水钠比为14后,其浆体的凝结时间延长；升高养护温度可提高地聚合反应速度并缩短浆体的硬化时间；流变性能研究发现在地聚物成型加工中施加一定的剪切力,有利于地聚物材料的流动成型。
(2)PVC对地聚物的增韧改性(PVC小于50wt%),是在地聚物网络结构形成之前加入PVC,在塑炼加工作用下使熔融态的PVC分子链与正在发生地质聚合反应的浆料共混,形成互穿网络的地聚物复合材料。通过高温流变学测试,发现当PVC含量小于50wt%时,由于PVC贡献的粘性特征被大量的地聚物贡献的弹性响应掩盖,导致复合材料模量越来越大,整个复合材料表现出地聚物的固体特征。其高温加工成型工艺参数如下：塑炼温度为170℃,塑炼时间为5分钟,塑炼后的薄片在170℃,15MPa的压力下,保温保压7分钟。PVC增韧地聚物复合材料的机械强度检测结果表明,复合材料的抗弯强度随PVC含量的增加而增大,PVC加入量为50wt%时,复合材料的抗弯强度达到67.06MPa,比纯地聚物28d龄期的抗弯强度提高了3.73倍。
(3)地聚物增韧PVC的共混改性方法(PVC大于50wt%),则是在地聚物形成的未固化阶段,将正在进行地聚合反应的浆体加入PVC树脂中,在共混物的塑炼压制加工过程中,正在形成的地聚物网络结构与己解缠绕而伸展的PVC分子链之间存在较好的结合,从而增强了地聚物与基体PVC的界面作用。力学性能测试结果表明,与纯PVC相比,地聚物含量在10wt%以内时,复合材料有较好的力学性能,其中以4wt%为最佳,其材料的抗冲击强度达到了9.13KJ·m-2,比纯PVC材料提高了约40%。维卡软化、热重分析、差示扫描量热法表征结果表明,与纯PVC相比较,复合材料的维卡软化温度提高了2-6℃,地聚物的加入对PVC分子链缺陷结构脱HC1具有吸收和抑制的作用,从而提高了地聚物/PVC复合材料的热稳定性。
(4)原位聚合法地聚物/PVC复合材料的制备,是将经硅烷偶联剂有机化改性的地聚物和氯乙烯单体,采用倒加料工艺经原位聚合生成地聚物/PVC复合树脂,然后经塑炼压制制备出复合材料。研究了地聚物对悬浮聚合体系的温度、压力、转化率、搅拌电流等参数的影响。力学性能检测结果表明,在地聚物含量为3wt%时,与纯PVC相比,复合材料抗冲击强度提高了59.4%,拉伸强度提高了13.8%,断裂伸长率提高了7.65%。由Kissinger法所计算的热分解活化能表明,原位聚合法地聚物/PVC复合材料和纯PVC材料的反应表观活化能分别为274.78J.mol-1和152.06J.mol-1地聚物/PVC的热分解活化能明显高于PVC的热分解活化能,证明地聚物的引入提高了PVC基体树脂的分解活化能,表明其热稳定性得以提高。
(5)在上述研究的基础上,将不同量的地聚物与PVC熟料充分混合后应用到PVC片材的生产过程中,在保证复合材料力学性能的前提下,使复合片材成本大大降低,耐老化性能得到提高。
Geopolymer is a kind of three dimensional structure aluminum silicate inorganic polymer composed by the [AlO4] and [SiO4] tetrahedron, which was mainly preparared by aluminum silicate or industrial waste. Geopolymer has high strength, corrosion resistance, water resistance, high temperature resistance, enclosed metal ion, and many other advantages, but its typical defect is "brittle", so toughening modification of geopolymer is more active.
Polyvinyl chloride (PVC) is one of the five biggest common thermoplastic resins, because it has flexible molecular chain, excellent comprehensive performance, the application of PVC material has related to various fields. If the high toughness PVC resin is compounded with brittle geopolymer materials, which will greatly improve toughness of geopolymer material, simultaneously geopolymer will also improve high temperature performanceresin of PVC. Based on the above ideas, this dissertation systematically studied thepreparation technology at high temperature of geopolymer/polyvinyl chloride (PVC) composites, and the performances of the composites were characterized and explored.
In the dissertation, pure geopolymer was prepared with metakaolin, sodium silicate, sheet alkali and water, and the preparation technology parameters of geopolymer were also optimized. Moreover, geopolymer matrix materials with high mechanics performance were prepared. geopolymer was toughened by polyvinyl chloride (PVC) with organic polymer flexible molecular chain characteristics, through the plasticate pressing method. In addition, with the characteristic of inorganic rigid particles and high temperature resistance for the geopolymer, PVC was modified by the blending method and in situ polymerization, and the research results were used in the preparation of PVC sheets. The research results are as follows:
(1) In the pure geopolymer preparation process, the rheological properties, curing time, microstructure and mechanical properties of geopolymer under the high temperature condition were studied. The results showed that, according to the strength of the geopolymer as the basis, the optimum proportion and technological parameters of geopolymer was determined as:the molar ratio of (SiO2)/(Al2O3) was3.3, the molar ratio of (Na2O)/(SiO2) was0.27, the molar ratio of (H2O)/(Na2O) was11, and the aging time of sodium silicate was24h, the curing temperature was60℃, the curing time was48h. So the strength of geopolymer reached to the highest,28d compressive strength and folding strength of geopolymer reached to89.63MPa,13.87MPa, respectively. High temperature moulding results showed that170℃,the initial setting time and final setting time of geopolymer slurry were11and16minutes, respectively. After the water sodium ratio of geopolymer was increased (14), the condensation time of geopolymer slurry extended. The reaction heat of geopolymer reflected that the increase of curing temperature could improve polymerization reaction rate and shorten the slurry setting time. Rheological properties showed that exerting shear force in polymer processing during the high temperature moulding process was helpful for flow moulding of geopolymer materials.
(2)Toughening modification of geopolymer was used PVC during the network structure process of geopolymer, because molten PVC molecular chain and polymerization of geopolymer worked together, which formed interpenetrating network of geopolymer composites. Through the high temperature rheology test, it was found that when PVC content was less than50wt%, the modulus of composites was bigger and bigger and the whole composites were characteristic of solid features of geopolymer because the contribution of the viscous features of PVC have been covered by the contribution of the elastic response. Its processing parameters were as follows: plastification temperature of PVC was175℃, plastification time of PVC was6minutes, heat preservation time was10minutes after plasticated under170℃,15MPa. The mechanical strength results of geopolymer toughened by showed that the28d bending strength reached to55.87MPa when the addition of PVC was40wt%, which was improved by3.1times compared with that of the pure geopolymer.
(3) The toughening modification of PVC was joined the geopolymer slury into PVC resin under coagulation stage of geopolymer, whose network structure was bonded by winding PVC molecular chain, resulting in enhancing the geopolymer and matrix PVC interface effect. Mechanics performance test results showed that, the geopolymer composites had good mechanical properties when geopolymer content was less then10wt%compared with pure PVC, of which4wt%content geopolymer was the optimum, and the impact strength of the PVC based composites reached to9.13KJ·m-2, which increased by40%compared with that of pure PVC. Vicat softening, thermogravimetric analysis, differential scanning calorimetry characterization results of PVC based composites showed that, vicat softening temperature increased by2-6℃compared with that of pure PVC. After geopolymer was joined into PVC, thermal stability of the Geolymer/PVC composites was enhanced because geopolymer inhibited and absorbed the releases of the HCl from PVC resulting from the molecular chain defect structure of PVC.
(4) In situ polymerization of Geolymer/PVC composites was prepared with geopolymer modfied by silane coupling agent organic and vinyl chloride monomer through the fall loading process by in situ polymerization, and then by plasticated pressing.The temperature, pressure, conversion, stirring electric current of suspension polymerization system were studied. Mechanical properties testing results showed that the impact strength of Geolymer/PVC composites increased by59.4%, the tensile strength of Geolymer/PVC composites increased by13.8%, the elongation at break of Geolymer/PVC composites increased by7.65%compared with that of pure PVC when the geopolymer content was3wt%. The thermal decomposition activation energy calculated by Kissinger method showed that apparent activation energy of PVC/polymer composite by in situ polymerization and pure PVC material were274.78J·mol-1and152.06J·mol-1, respectively. The thermal decomposition activation energy of Geolymer/PVC was obviously higher than that of the PVC,which proved that the introduction of geopolymer improved the decomposition activation energy of PVC matrix resin and showed that its thermal stability was improved.
(5) According to the above research conclusion, different amount of geopolymer were mixing fully with PVC and applied in PVC sheet production process, the mechanical properties of PVC composites were higher than that of the pure PVC sheets. In addition, aging resistance of PVC composite was greatly increased and significantly improved the durability of PVC sheets composites.
引文
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