磺化超细聚苯乙烯颗粒的制备和吸附性能研究
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摘要
本文采用苯乙烯(St)微乳液聚合方法,成功合成了超细聚苯乙烯(SfPS)稳定分散体系。采用独创的稀H2SO4和有机溶剂混合破乳技术,成功获得了SfPS颗粒。通过固相磺化反应,得到了超细聚苯乙烯型阳离子交换树脂(SSPS)。基于紫外-可见分光光度计方法,研究了SSPS对铜离子和阳离子红染料吸附性能,同时,制成交联的SSPS-PVA离子交换膜,探讨了离子交换膜的吸附性能。通过LS-800型激光粒度仪测定了SfPS粒子和SSPS离子交换树脂粒子的粒径分布,借助H-600型透射电镜研究了粒子的微观形貌特征,用NICOLET 5700型红外光谱仪表征了SSPS离子交换树脂的磺化程度。本论文研究的主要内容包括以下几个方面:
1、通过正交试验设计,研究了乳化剂OP-10、助乳化剂DBS、交联剂DVB等对聚苯乙烯(SfPS)粒径分布的影响,成功找到了苯乙烯微乳液聚合的最佳实验配方。
2、探讨了聚苯乙烯微乳液的各种破乳方法,并通过抽滤、特殊干燥工艺等方法解决了纳米粒子的团聚问题。
3、研究了浓H2SO4对SfPS粒子的磺化工艺,探讨了影响SfPS磺化的主要因素。
4、研究了超细SSPS离子交换树脂与离子交换膜对铜离子和阳离子红染料的吸附性能。
经过一系列的研究得到以下结论:
1、本实验苯乙烯微乳液聚合体系中苯乙烯的含量可达44%左右,接近单体的最大增溶量,对于实际工业化生产很有指导意义。
2、通过正交设计试验分析和验证,苯乙烯微乳液聚合的最佳方案考虑如下:采用乳化剂OP-10为34 ml,助乳化剂DBS为4.85 ml,交联剂DVB为4.85 ml,引发剂K2S2O8为25ml,单体St为114 ml的配方。
3、采用稀H2SO4和有机溶剂混合破乳的方法,破乳效果十分明显。
4、为了获得最好的SSPS离子交换性能,SfPS磺化工艺应采用H2SO4浓度为95%,温度为85℃,反应时间3h的方案。
5、SSPS离子交换树脂研制的工艺过程可归纳为:苯乙烯微乳液聚合→破乳→洗涤、沉降→抽滤、干燥→磺化→洗涤、沉降→抽滤、干燥。
6、用红外光谱仪分析得到,SSPS树脂中约83%的苯环接上了磺酸基。
7、从激光粒度测量和透射电镜观察结果看,SSPS离子交换树脂颗粒直径较小,大小比较均匀,其中存在一部分纳米粒子,没有出现团聚现象,最大的SSPS树脂粒径处在2μm以内。
8、SSPS离子交换树脂对阳离子染料的吸附速度很快,吸附率较高。
本课题的特色与创新之处:
1、独创了采用稀H2SO4和有机溶剂对聚苯乙烯微乳液混合破乳的方法;
2、基于红外光谱测量,定量计算出聚苯乙烯磺化度;
3、在国内外较早地开展了超细聚苯乙烯型离子交换树脂及其离子交换膜对阳离子染料的吸附作用的研究。
The stable polystyrene microemulsion was successfully synthesized, and superfine polystyrene particles (SfPS) were made via the cosolvent system developed in our lab. The superfine sulfonated polystyrene particles (SSPS) were obtained by using solid state sulfonation. The adsorption of copper ions (II) and cationic dye (5GN) of SSPS particles and the blend films of SSPS and polyvinyl alcohol were investigated with ultraviolet-visible spectrophotometer. The particle dimensional distributions of SfPS and SSPS were measured with LS-800 Laser Particle Analyser. The particle morphologies of SfPS and SSPS were observed with H-600 Transimission Electron Microscope. The sulfonation and sulfonation degree of SSPS were analysed by NICOLET 5700 Infrared Spectroscopy. The following aspects were carefully studied in this thesis:
1. Based on the orthogonal experiment design, the dosages of emulsifier OP-10, auxillary emulsifier DBS, crosslinker DVB were optimized according to the stability of microemulsion and the resulted SfPS particle size.
2. The demulsifying methods, filtration via vaccum and drying were investigated to avoid the formation of particle clusters or aggregate.
3. The factors which affacted the sulfonation of superfine polystyrene via concentrated sulfuric acid route were considered and discussed.
4. The copper ion(II) and cationic dye adsorptions with SSPS particles and the blend film of SSPS and polyvinyl alcohol were studied.
The general conclusions were made in the following aspects:
1. A very large quantity of monomer styrene and polymer, 44%, was solublized with the emulsifier system. This could be direactly applied on an industiral scale.
2. The optimized formula included emulsifier OP-10 34 parts, auxillary emulsifier DBS 4.85 parts, crosslinker DVB 4.85 parts, initiator K2S2O8 25 parts (3wt% aqueous solution), and monomer 114 parts.
3. The remarkable demulsification was achieved by the combination of dilute sulfuric acid and organic solvent.
4. The optimized sulfonation conditions for superfine polystyrene were: sulfuric acid 95%, reaction temperature 85℃and reaction time 3h.
5. The superfine sulfonated polystyrene particles can be obtained by the following processes: microemulsion polymerization of styrene, demulsification, precipitation and washing, filtration and drying, sulfonation and washing, and filtration and drying.
6. Around 83 % benzene ring of polystyrene was sulfonated according to the analysis of infrared spectra.
7. Both the diameter distributions of SfPS and SSPS particles were uniform, the maximum particle showed the diameter of 2μm for SSPS.
8. SSPS indicated the rapid and strong adsorption for cationic dye.
The feature and innovation points of this thesis could include:
1. The combination of dilute sulfuric acid and organic solvent has been developed to demulsify the highly stable polystyrene microemulsion.
2. The degree of sulfonation was quantified based on the infrared spectra.
3. The superfine sulfonated polystyrene particles and the crosslinked polyvinyl alcohol films imbedded SSPS particles were employed to conduct out the adsorption for cationic red dye (5GN), and showed a satisfied results.
1、通过正交试验设计,研究了乳化剂OP-10、助乳化剂DBS、交联剂DVB等对聚苯乙烯(SfPS)粒径分布的影响,成功找到了苯乙烯微乳液聚合的最佳实验配方。
2、探讨了聚苯乙烯微乳液的各种破乳方法,并通过抽滤、特殊干燥工艺等方法解决了纳米粒子的团聚问题。
3、研究了浓H2SO4对SfPS粒子的磺化工艺,探讨了影响SfPS磺化的主要因素。
4、研究了超细SSPS离子交换树脂与离子交换膜对铜离子和阳离子红染料的吸附性能。
经过一系列的研究得到以下结论:
1、本实验苯乙烯微乳液聚合体系中苯乙烯的含量可达44%左右,接近单体的最大增溶量,对于实际工业化生产很有指导意义。
2、通过正交设计试验分析和验证,苯乙烯微乳液聚合的最佳方案考虑如下:采用乳化剂OP-10为34 ml,助乳化剂DBS为4.85 ml,交联剂DVB为4.85 ml,引发剂K2S2O8为25ml,单体St为114 ml的配方。
3、采用稀H2SO4和有机溶剂混合破乳的方法,破乳效果十分明显。
4、为了获得最好的SSPS离子交换性能,SfPS磺化工艺应采用H2SO4浓度为95%,温度为85℃,反应时间3h的方案。
5、SSPS离子交换树脂研制的工艺过程可归纳为:苯乙烯微乳液聚合→破乳→洗涤、沉降→抽滤、干燥→磺化→洗涤、沉降→抽滤、干燥。
6、用红外光谱仪分析得到,SSPS树脂中约83%的苯环接上了磺酸基。
7、从激光粒度测量和透射电镜观察结果看,SSPS离子交换树脂颗粒直径较小,大小比较均匀,其中存在一部分纳米粒子,没有出现团聚现象,最大的SSPS树脂粒径处在2μm以内。
8、SSPS离子交换树脂对阳离子染料的吸附速度很快,吸附率较高。
本课题的特色与创新之处:
1、独创了采用稀H2SO4和有机溶剂对聚苯乙烯微乳液混合破乳的方法;
2、基于红外光谱测量,定量计算出聚苯乙烯磺化度;
3、在国内外较早地开展了超细聚苯乙烯型离子交换树脂及其离子交换膜对阳离子染料的吸附作用的研究。
The stable polystyrene microemulsion was successfully synthesized, and superfine polystyrene particles (SfPS) were made via the cosolvent system developed in our lab. The superfine sulfonated polystyrene particles (SSPS) were obtained by using solid state sulfonation. The adsorption of copper ions (II) and cationic dye (5GN) of SSPS particles and the blend films of SSPS and polyvinyl alcohol were investigated with ultraviolet-visible spectrophotometer. The particle dimensional distributions of SfPS and SSPS were measured with LS-800 Laser Particle Analyser. The particle morphologies of SfPS and SSPS were observed with H-600 Transimission Electron Microscope. The sulfonation and sulfonation degree of SSPS were analysed by NICOLET 5700 Infrared Spectroscopy. The following aspects were carefully studied in this thesis:
1. Based on the orthogonal experiment design, the dosages of emulsifier OP-10, auxillary emulsifier DBS, crosslinker DVB were optimized according to the stability of microemulsion and the resulted SfPS particle size.
2. The demulsifying methods, filtration via vaccum and drying were investigated to avoid the formation of particle clusters or aggregate.
3. The factors which affacted the sulfonation of superfine polystyrene via concentrated sulfuric acid route were considered and discussed.
4. The copper ion(II) and cationic dye adsorptions with SSPS particles and the blend film of SSPS and polyvinyl alcohol were studied.
The general conclusions were made in the following aspects:
1. A very large quantity of monomer styrene and polymer, 44%, was solublized with the emulsifier system. This could be direactly applied on an industiral scale.
2. The optimized formula included emulsifier OP-10 34 parts, auxillary emulsifier DBS 4.85 parts, crosslinker DVB 4.85 parts, initiator K2S2O8 25 parts (3wt% aqueous solution), and monomer 114 parts.
3. The remarkable demulsification was achieved by the combination of dilute sulfuric acid and organic solvent.
4. The optimized sulfonation conditions for superfine polystyrene were: sulfuric acid 95%, reaction temperature 85℃and reaction time 3h.
5. The superfine sulfonated polystyrene particles can be obtained by the following processes: microemulsion polymerization of styrene, demulsification, precipitation and washing, filtration and drying, sulfonation and washing, and filtration and drying.
6. Around 83 % benzene ring of polystyrene was sulfonated according to the analysis of infrared spectra.
7. Both the diameter distributions of SfPS and SSPS particles were uniform, the maximum particle showed the diameter of 2μm for SSPS.
8. SSPS indicated the rapid and strong adsorption for cationic dye.
The feature and innovation points of this thesis could include:
1. The combination of dilute sulfuric acid and organic solvent has been developed to demulsify the highly stable polystyrene microemulsion.
2. The degree of sulfonation was quantified based on the infrared spectra.
3. The superfine sulfonated polystyrene particles and the crosslinked polyvinyl alcohol films imbedded SSPS particles were employed to conduct out the adsorption for cationic red dye (5GN), and showed a satisfied results.
引文
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