苯乙烯微波等离子体聚合研究
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摘要
当今,可持续发展作为指导各国经济社会发展的一项总体战略,已经逐渐被人们所认同。化学工业在给人们带来众多利益的同时,也给生态环境带来了沉重的负担。开发清洁高效的化学反应过程,以达到标本兼治的效果,已成为当代化学的学科前沿和重点发展方向之一。作为现代物理技术的微波、等离子体,应用在化学领域中具有操作方便、清洁、高效、环保、反应快速、选择性好、无滞后效应等优点,引起各国研究者的广泛关注和极大兴趣。
本文以苯乙烯为主要原料,采用辉光等离子体技术,以二氧化碳为反应气体和利用微波辐射与溶胶凝胶、乳液聚合相结合,分别合成了苯乙烯/CO_2共聚膜和苯乙烯/TiO_2复合微球,研究了在非常规条件下苯乙烯/TiO_2和苯乙烯/CO_2的聚合反应规律,并采用IR、XPS等手段对所得产物进行了表征。
研究结果显示,所得等离子体共聚膜不仅具有明显的聚苯乙烯特征峰;且等离子体聚合膜在1709 cm-1(C=O)和3296 cm-1(-OH)处出现了新吸收峰,其吸收峰的相对强度随二氧化碳流量值的增大而增强,表明等离子体聚合反应过程中二氧化碳与苯乙烯发生了反应。但一些苯环在等离子体聚合过程中遭到了破坏,枝化程度增加。采用偏光显微镜对所得等离子体聚合膜表面进行了观察,结果显示,以二氧化碳作为反应气体的等离子体聚合膜表面呈现类似波状的图形;随着二氧化碳流量的增加,相邻两个波之间的宽度变大;无二氧化碳作为反应气体的聚合膜没有明显的波纹图形。
在微波技术协助下,本研究利用溶胶-凝胶法合成的二氧化钛溶胶与苯乙烯进行原位乳液聚合制备了核-壳结构的复合微球,微球表面光滑,粒径较小,且呈单分散性。常规加热乳液聚合与微波辐射乳液聚合结果的比较表明,常规加热乳液聚合所得复合微球的粒径明显大于微波辐射乳液聚合所得的复合微球,微球直径分布较宽,说明微波辐射乳液聚合适用于制备单分散且粒径较小的复合微球。
In recent years, lasting developable policy has become an important strategy, which triggers many countries economical development, and is gradually accepted by people. Though chemical industry brings large economical benefits, but it gives rise to severe environment damage. For the sake of environment protection, to develope green chemical reaction process has become one of the important research aspects. Microwave and plasma technologies, which are applied in chemical field, have many advantages, such as easy operation, higher efficiency, quick reaction, environmentally friendly, and so on, thus attracting much attention.
In this thesis, the studies on the rules of polymerization of CO2/styrene under glow discharge and TiO2/styrene under microwave are presented. The experimental results show that newly formed groups, -COOH and -C-O, are present in the plasma polymerized polystyrene films, suggesting that chemical reactions have happened between CO2 and styrene. XPS analysis confirms that the content of C=O and C-O groups increases with CO2 flow rate. Optical microscope observations demonstrate that the plasma polymerized styrene films show a wave-like pattern and that the wavelength increases with CO2 flow rate.
TiO2/polystyrene core-shell nanospheres have been successfully synthesized by a novel combination of sol-gel and microwave assisted emulsion polymerization. The obtained nanoparticles, whose diameter is very uniform, have clear core-shell structure and smooth surfaces.
本文以苯乙烯为主要原料,采用辉光等离子体技术,以二氧化碳为反应气体和利用微波辐射与溶胶凝胶、乳液聚合相结合,分别合成了苯乙烯/CO_2共聚膜和苯乙烯/TiO_2复合微球,研究了在非常规条件下苯乙烯/TiO_2和苯乙烯/CO_2的聚合反应规律,并采用IR、XPS等手段对所得产物进行了表征。
研究结果显示,所得等离子体共聚膜不仅具有明显的聚苯乙烯特征峰;且等离子体聚合膜在1709 cm-1(C=O)和3296 cm-1(-OH)处出现了新吸收峰,其吸收峰的相对强度随二氧化碳流量值的增大而增强,表明等离子体聚合反应过程中二氧化碳与苯乙烯发生了反应。但一些苯环在等离子体聚合过程中遭到了破坏,枝化程度增加。采用偏光显微镜对所得等离子体聚合膜表面进行了观察,结果显示,以二氧化碳作为反应气体的等离子体聚合膜表面呈现类似波状的图形;随着二氧化碳流量的增加,相邻两个波之间的宽度变大;无二氧化碳作为反应气体的聚合膜没有明显的波纹图形。
在微波技术协助下,本研究利用溶胶-凝胶法合成的二氧化钛溶胶与苯乙烯进行原位乳液聚合制备了核-壳结构的复合微球,微球表面光滑,粒径较小,且呈单分散性。常规加热乳液聚合与微波辐射乳液聚合结果的比较表明,常规加热乳液聚合所得复合微球的粒径明显大于微波辐射乳液聚合所得的复合微球,微球直径分布较宽,说明微波辐射乳液聚合适用于制备单分散且粒径较小的复合微球。
In recent years, lasting developable policy has become an important strategy, which triggers many countries economical development, and is gradually accepted by people. Though chemical industry brings large economical benefits, but it gives rise to severe environment damage. For the sake of environment protection, to develope green chemical reaction process has become one of the important research aspects. Microwave and plasma technologies, which are applied in chemical field, have many advantages, such as easy operation, higher efficiency, quick reaction, environmentally friendly, and so on, thus attracting much attention.
In this thesis, the studies on the rules of polymerization of CO2/styrene under glow discharge and TiO2/styrene under microwave are presented. The experimental results show that newly formed groups, -COOH and -C-O, are present in the plasma polymerized polystyrene films, suggesting that chemical reactions have happened between CO2 and styrene. XPS analysis confirms that the content of C=O and C-O groups increases with CO2 flow rate. Optical microscope observations demonstrate that the plasma polymerized styrene films show a wave-like pattern and that the wavelength increases with CO2 flow rate.
TiO2/polystyrene core-shell nanospheres have been successfully synthesized by a novel combination of sol-gel and microwave assisted emulsion polymerization. The obtained nanoparticles, whose diameter is very uniform, have clear core-shell structure and smooth surfaces.
引文
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