氯乙烯—醋酸乙烯酯共聚物制备新技术及其纳米复合材料研究
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摘要
本论文系统研究了氯乙烯-醋酸乙烯酯共聚物(PVVA)新的合成方法、官能团化及与纳米粒子复合改性等问题。围绕提高PVVA共聚物性能,采用清洁,过程简单,适合于工业化的制备技术实现了PVVA树脂羧基功能化；通过混合微悬浮聚合技术制备PVVA乳液及糊树脂；引入纳米Si02粒子原位复合PVVA共聚物,提高了共聚物的加工性能、力学性能等。
1.以悬浮聚合制备氯乙烯-醋酸乙烯酯(VC-VAc)二元共聚物为基础,讨论了醋酸乙烯酯(VAc)单体对PVVA共聚树脂性能的影响,如树脂链段均匀性、分子量及颗粒特性的影响因素和控制手段,探讨了困扰工业化产品质量提高的几个关键问题。通过控制反应过程中饱和蒸汽压及它的变化区间,提高了共聚物组成均一性。
2.纳米Si02通过悬浮聚合与PVVA树脂原位复合,研究了PVVA/nano-SiO2复合树脂颗粒特性及其熔融流变特性间的关系。PVVA/nano-SiO2复合树脂中适量纳米Si02提高了树脂孔隙率及疏松程度,缩短了物料熔融时间,降低了物料熔融温度,其变化规律与树脂的疏松程度呈对应关系。
3.研究在VC-VAc体系中引入不饱和酸(酐),在水相体系中通过化学转变使羧基成功接到共聚链段上,实现PVVA树脂的羧基功能化,开创了利用传统合成方法获得PVVA树脂功能化的工艺路线。重点研究了马来酸酐(MAH)与乙醇(EtOH)酯化反应条件对马来酸单乙酯(MEM)产率影响,研究结果表明MEM加入体系后树脂的酸值提高,附着力上升。红外图谱(FTIR)分析表明水相悬浮聚合制备的氯乙烯-醋酸乙烯酯-马来酸酐三元共聚物(PVVM)中羧基已经成功被引入。
4.纳米SiO2与VC-VAc-MAH体系经悬浮聚合方法原位复合,对PVVM/nano-SiO2复合树脂的性能进行了全面对比,PVVM复合树脂的耐热性能及力学性能均得到显著提高,原位复合方式得到的PVVM/nano-SiO2树脂与溶液共混复合方式相比,纳米粒子在树脂基体中的分散更均匀,纳米粒子改性效果更突出。
5.采用混合微悬浮聚合技术合成PVVA共聚胶乳,系统剖析了PVVA胶乳粒径的控制手段,探索PVVA乳液干燥工艺对次级粒子及增塑糊粘度的影响规律。结果表明采用SDS/CA-SA皂化体系与单体形成增溶胶束,同时加入二代复合种子乳液,可增大胶乳粒径且使乳液粒径呈双峰分布。调整喷雾干燥条件制得了初级粒子堆彻松散、形态规整的次级粒子,使PVVA糊树脂的增塑糊粘度较低。
This paper described systematically a novel synthesis method of Poly (vinyl chloride-co-vinyl acetate)(PVVA) copolymer by suspension radical copolymerization. The functionalization of the copolymer and its modification by the incorporation of nano-SiO2particles were also studied. In order to enhancing the property of PVVA copolymer, a simple synthesis technique which was clean and available in the industrial production was developed to introduce carboxyl group into PVVA copolymer, and then PVVA emulsion and paste resin were prepared by hybrid micro-suspension polymerization technique. When nano-SiO2particles were dispersed into PVVA copolymer resin by in-situ suspension copolymerization, the processing properties and the inherent qualities of PVVA production were improved significantly.
1. Poly (vinyl chloride-co-vinyl acetate) copolymer was prepared by suspension polymerization. The effect of VAc monomer to the properties of PVVA copolymer was investigated and discussed in this paper. The influence factors and control methods of the chain segment uniformity of PVVA copolymer, the average molecular weight and particle characteristics of PVVA were explored. Several key problems which restricted the improvement of PVVA product quality in industrial production were solved. Especially, the chain segment uniformity of copolymer was enhanced by controlling the variation range of saturated vapor pressure in the polymerization.
2. PVVA/SiO2nanocomposite was prepared by radical suspension polymerization of the monomers in the presence of fumed nano-SiO2pre-modified with y-methylacryloxypropl trimethoxy silane. Through CPA and Mercury injection measurement, morphology comparison (SEM), it can be concluded that the grain porosity and specific surface area of nanocomposite resin could be enhanced due to the incorporation of suitable amount of nano-SiO2to PVVA. The relation between grain characteristics and plasticizing process rheology properties of PVVA/nano-SiO2composite resin was studied by torque rheometer. From the plasticizing curve, it can be seen that the melting time of the mixture sample was shortened, and the melting temperature was lowered. The processing charactristic was correlated with the porosity degree of the composite resin.
3. To achieve the carboxyl-functionalization of the Poly (vinyl chloride-co-vinyl acetate) copolymer, a novel preparation technique was developed based on the traditional method. Maleic anhydride (MAH) was esterified by ethanol (EtOH) to obtain mono-ethyl maleate (MEM). The influence of reaction conditions, such as temperature and reaction time, on the yield rate of MEM was studied in order to attain a higher yield rate of MEM. PVVA containing carboxyl group was synthesized by reacting esterified MAH with vinyl chloride and vinyl acetate in terms of aqueous suspension polymerization method. FT-IR spectra showed that carboxyl group was successfully introduced into the PVVA molecular structure through this method. The addition of MEM resulted in the acid value of copolymer increasing obviously. Meanwhile, the coating adhesive force of Poly (vinyl chloride-co-vinyl acetate-co-maleic anhydride) resin was also improved.
4. Nano-SiO2particles were incorporated into Poly (vinyl chloride-co-vinyl acetate-co-maleic anhydride)(PVVM) resin by in-situ copolymerization. Morphology observation showed that the nano-SiO2were well dispersed by nanometer scale in the copolymer matrix of the nanocomposite films, while nano-SiO2tend to agglomerate in the composites films prepared by solution blending PVVM/nano-SiO2composite. The in-situ PVVM/nano-SiO2composite resin showed a better heat resistance and mechanical properties than that obtained from solution blending. Solution viscosity and adhesive ability of the nanocomposite can be significantly enhanced by incorporation of nano-SiO2through in-situ polymerization. The enhancement is related to better dispersion of nano-SiO2particles in polymer matrix. Therefore the modification effect of the nanocomposite resin was more excellent.
5. PVVA copolymer latex was prepared by Hybrid Micro-suspension Polymerization technique and the control method of the latex particle size was analyzed systematically. The research results showed the mixing of SDS/CA-SA saponification system and oily monomer could produce solubilizing micellar phase and increase PVVA latex particle size effectively. When the composite seed emulsion was added, the particle size of PVVA latex synthesized would display a bimodal distribution. The influence of spray and drying process of PVVA latex on secondary particle of PVVA resin and Brookfield paste viscosity of PVVA plastisol was also explored. Through paste viscosity measurement and grain morphology comparison, it can be concluded that the secondary particle of PVVA resin play an important role in paste viscosity control. The grain which have regular form and gathered with incompact primary particles would have lower paste viscosity. The secondary particle characteristic of PVVA could be obtained by adjusting spray and drying conditions, such as outlet and inlet dry temperature.
1.以悬浮聚合制备氯乙烯-醋酸乙烯酯(VC-VAc)二元共聚物为基础,讨论了醋酸乙烯酯(VAc)单体对PVVA共聚树脂性能的影响,如树脂链段均匀性、分子量及颗粒特性的影响因素和控制手段,探讨了困扰工业化产品质量提高的几个关键问题。通过控制反应过程中饱和蒸汽压及它的变化区间,提高了共聚物组成均一性。
2.纳米Si02通过悬浮聚合与PVVA树脂原位复合,研究了PVVA/nano-SiO2复合树脂颗粒特性及其熔融流变特性间的关系。PVVA/nano-SiO2复合树脂中适量纳米Si02提高了树脂孔隙率及疏松程度,缩短了物料熔融时间,降低了物料熔融温度,其变化规律与树脂的疏松程度呈对应关系。
3.研究在VC-VAc体系中引入不饱和酸(酐),在水相体系中通过化学转变使羧基成功接到共聚链段上,实现PVVA树脂的羧基功能化,开创了利用传统合成方法获得PVVA树脂功能化的工艺路线。重点研究了马来酸酐(MAH)与乙醇(EtOH)酯化反应条件对马来酸单乙酯(MEM)产率影响,研究结果表明MEM加入体系后树脂的酸值提高,附着力上升。红外图谱(FTIR)分析表明水相悬浮聚合制备的氯乙烯-醋酸乙烯酯-马来酸酐三元共聚物(PVVM)中羧基已经成功被引入。
4.纳米SiO2与VC-VAc-MAH体系经悬浮聚合方法原位复合,对PVVM/nano-SiO2复合树脂的性能进行了全面对比,PVVM复合树脂的耐热性能及力学性能均得到显著提高,原位复合方式得到的PVVM/nano-SiO2树脂与溶液共混复合方式相比,纳米粒子在树脂基体中的分散更均匀,纳米粒子改性效果更突出。
5.采用混合微悬浮聚合技术合成PVVA共聚胶乳,系统剖析了PVVA胶乳粒径的控制手段,探索PVVA乳液干燥工艺对次级粒子及增塑糊粘度的影响规律。结果表明采用SDS/CA-SA皂化体系与单体形成增溶胶束,同时加入二代复合种子乳液,可增大胶乳粒径且使乳液粒径呈双峰分布。调整喷雾干燥条件制得了初级粒子堆彻松散、形态规整的次级粒子,使PVVA糊树脂的增塑糊粘度较低。
This paper described systematically a novel synthesis method of Poly (vinyl chloride-co-vinyl acetate)(PVVA) copolymer by suspension radical copolymerization. The functionalization of the copolymer and its modification by the incorporation of nano-SiO2particles were also studied. In order to enhancing the property of PVVA copolymer, a simple synthesis technique which was clean and available in the industrial production was developed to introduce carboxyl group into PVVA copolymer, and then PVVA emulsion and paste resin were prepared by hybrid micro-suspension polymerization technique. When nano-SiO2particles were dispersed into PVVA copolymer resin by in-situ suspension copolymerization, the processing properties and the inherent qualities of PVVA production were improved significantly.
1. Poly (vinyl chloride-co-vinyl acetate) copolymer was prepared by suspension polymerization. The effect of VAc monomer to the properties of PVVA copolymer was investigated and discussed in this paper. The influence factors and control methods of the chain segment uniformity of PVVA copolymer, the average molecular weight and particle characteristics of PVVA were explored. Several key problems which restricted the improvement of PVVA product quality in industrial production were solved. Especially, the chain segment uniformity of copolymer was enhanced by controlling the variation range of saturated vapor pressure in the polymerization.
2. PVVA/SiO2nanocomposite was prepared by radical suspension polymerization of the monomers in the presence of fumed nano-SiO2pre-modified with y-methylacryloxypropl trimethoxy silane. Through CPA and Mercury injection measurement, morphology comparison (SEM), it can be concluded that the grain porosity and specific surface area of nanocomposite resin could be enhanced due to the incorporation of suitable amount of nano-SiO2to PVVA. The relation between grain characteristics and plasticizing process rheology properties of PVVA/nano-SiO2composite resin was studied by torque rheometer. From the plasticizing curve, it can be seen that the melting time of the mixture sample was shortened, and the melting temperature was lowered. The processing charactristic was correlated with the porosity degree of the composite resin.
3. To achieve the carboxyl-functionalization of the Poly (vinyl chloride-co-vinyl acetate) copolymer, a novel preparation technique was developed based on the traditional method. Maleic anhydride (MAH) was esterified by ethanol (EtOH) to obtain mono-ethyl maleate (MEM). The influence of reaction conditions, such as temperature and reaction time, on the yield rate of MEM was studied in order to attain a higher yield rate of MEM. PVVA containing carboxyl group was synthesized by reacting esterified MAH with vinyl chloride and vinyl acetate in terms of aqueous suspension polymerization method. FT-IR spectra showed that carboxyl group was successfully introduced into the PVVA molecular structure through this method. The addition of MEM resulted in the acid value of copolymer increasing obviously. Meanwhile, the coating adhesive force of Poly (vinyl chloride-co-vinyl acetate-co-maleic anhydride) resin was also improved.
4. Nano-SiO2particles were incorporated into Poly (vinyl chloride-co-vinyl acetate-co-maleic anhydride)(PVVM) resin by in-situ copolymerization. Morphology observation showed that the nano-SiO2were well dispersed by nanometer scale in the copolymer matrix of the nanocomposite films, while nano-SiO2tend to agglomerate in the composites films prepared by solution blending PVVM/nano-SiO2composite. The in-situ PVVM/nano-SiO2composite resin showed a better heat resistance and mechanical properties than that obtained from solution blending. Solution viscosity and adhesive ability of the nanocomposite can be significantly enhanced by incorporation of nano-SiO2through in-situ polymerization. The enhancement is related to better dispersion of nano-SiO2particles in polymer matrix. Therefore the modification effect of the nanocomposite resin was more excellent.
5. PVVA copolymer latex was prepared by Hybrid Micro-suspension Polymerization technique and the control method of the latex particle size was analyzed systematically. The research results showed the mixing of SDS/CA-SA saponification system and oily monomer could produce solubilizing micellar phase and increase PVVA latex particle size effectively. When the composite seed emulsion was added, the particle size of PVVA latex synthesized would display a bimodal distribution. The influence of spray and drying process of PVVA latex on secondary particle of PVVA resin and Brookfield paste viscosity of PVVA plastisol was also explored. Through paste viscosity measurement and grain morphology comparison, it can be concluded that the secondary particle of PVVA resin play an important role in paste viscosity control. The grain which have regular form and gathered with incompact primary particles would have lower paste viscosity. The secondary particle characteristic of PVVA could be obtained by adjusting spray and drying conditions, such as outlet and inlet dry temperature.
引文
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