Highly Uniform and Porous Polyurea Microspheres:Preparation,
发布时间:2022-01-05 17:23
Polyureas(PU)are known for long as important engineering materials thanks to their high chemical,mechanical,thermal shock and abrasion resistance,good flexibility,and water repellency etc.Their common applications have been limited to protective coating materials for different structural materials.PU are commonly synthesized either through condensation polymerization using diisocyanate(NCO)and diamines or through the reaction of NCO groups with water,turning itself into amine by release of CO
【文章来源】:济南大学山东省
【文章页数】:136 页
【学位级别】:博士
【文章目录】:
Abstract
Chapter1 Introduction
1.1 Polyurea Materials
1.1.1 Historical Perspective of PU
1.2 Porous Polymer Microspheres
1.2.1 Preparation Methods of Porous Polymer Microspheres
1.2.1.1 Precipitation Polymerization
1.2.1.2 Interfacial Polymerization
1.2.1.3 Microfluidics
1.3 PU Microspheres
1.4 Polymer-Metal Composite Microspheres
1.5 Motivation of the Thesis
Chapter2 Preparation of Highly Uniform and Porous PU Microspheres(PPM)
2.1 Introduction
2.2 Experimental Section
2.2.1 Materials Details
2.2.2 Laboratory Equipment
2.2.3 Microfluidic Device Design
2.2.4 Characterization of PPM
2.3 Results and Discussions
2.3.1 PPM Formation Mechanism
2.3.2 Effect of Aqueous Phase Flow Rate on PPM Formation
2.3.3 Effect of TDI Flow Rate on PPM Formation
2.3.4 Effect of PVA Amount on PPM Formation
2.3.5 Effects of Polymerization Time
2.3.6 Effects of Polymerization Temperature
2.3.7 PPM Morphology Observation by SEM
2.3.8 Porous Properties of PPM
2.4 Summary
Chapter3 Preparation of Pd-PPM Composites by Different Process(Pd@PPM1,Pd@PPM2)
3.1 Introduction
3.2 Experimental Section
3.2.1 Synthesis Approach of Pd@PPM1 and Pd@PPM
3.2.2 Characterization
3.3 Results and Discussion
3.3.1 Preparation of Pd@PPM1 and Pd@PPM
3.3.2 Morphology observation by OM and SEM
3.3.3 Porous Properties
3.3.4 EDX Analysis
3.3.5 FTIR Analysis
3.3.6 XRD Analysis
3.3.7 NMR Analysis
3.3.8 XPS Analysis
3.3.9 H_2-TPR Analysis
3.4 Summary
Chapter4 Pd-PPM Composites as Catalyst in Dye Degradations
4.1 Introduction
4.2 Experimental Section
4.2.1 Degradation of Dyes by Pd@PPM1 and Pd@PPM
4.3 Results and Discussion
4.3.1 MO Degradation
4.3.2 Rh B Degradation
4.3.3 MB Degradation
4.3.4 Mechanism of Dyes Degradation
4.3.5 Reusability of Pd@PPM1 and Pd@PPM2 in Dyes Degradation
4.4 Summary
Chapter5 Pd-PPM Composites as Catalyst in4-NP Reduction
5.1 Introduction
5.2 Experimental Section
5.2.1 4-NP Reduction by Pd@PPM1 and Pd@PPM
5.2.2 Characterization
5.3 Results and Discussion
5.3.1 CO Pulse Chemisorption Analysis
5.3.2 Catalytic Activity of Pd@PPM2 for4-NP Reduction
5.3.3 Effect of Pd@PPM2 Amount on4-NP Reduction
5.3.4 Effect of NaBH_4 Amount on4-NP reduction
5.3.5 Pd Loading Effect on Pd@PPM2 Activity for4-NP Reduction
5.3.6 Effect of 4-NP Initial Concentration
5.3.7 Effect of Temperature on4-NP Reduction
5.3.8 Effect of pH on4-NP Reduction
5.3.9 4-NP Reduction by Pd@PPM
5.3.10 Catalytic Activity Comparison of Pd@PPM1 to Pd@PPM2 in4-NP Reduction
5.3.11 Mechanism of4-NP Reduction
5.3.12 Reusability of Pd@PPM1 and Pd@PPM2 in4-NP Reduction
5.4 Summary
Chapter6 Pd@PPU Composite as Catalyst in Cr~(6+)Reduction
6.1 Introduction
6.2 Experimental Section
6.2.1 Preparation of Pd@PPU
6.2.2 Characterization f Pd(OAc)2@PPU and Pd@PPU
6.2.3 Catalytic Performance of Pd@PPU in Cr~(~(6+)) Reduction
6.3 Results and Discussion
6.3.1 Synthesis and Characterizations of Pd@PPU
6.3.2 Morphology observation by OM and SEM
6.3.3 EDS Analysis
6.3.4 BET Analysis
6.3.5 FTIR Analysis
6.3.6 NMR Analysis
6.3.7 XPS Analysis
6.3.8 XRD Analysis
6.3.9 TEM Analysis
6.3.10 Performance of Pd@PPU for the Reduction of Cr~(6+)to Cr~(3+)
6.3.11 Effect of Pd Amount on Cr~(6+)Reduction
6.3.12 Effects of FA and SF Concentrations on Cr~(6+)Reduction
6.3.13 Effect of Initial Concentration of K2Cr2O7 on Catalytic Activity of Pd@PPU
6.3.14 Effect of Temperature on Cr~(6+)Reduction
6.3.15 Mechanism of Cr~(6+)Reduction
6.3.16 Catalytic Activity Comparison of Pd@PPU with Commercial Pd@C
6.3.17 Reusability of Pd@PPU
6.4 Summary
Chapter7 Conclusions and Future Outlook
7.1 Conclusions
7.2 Future Outlook
References
Acknowledgements
Appendix
【参考文献】:
期刊论文
[1]NMR Analysis to Identify Biuret Groups in Common Polyureas[J]. Wei-Guang Qiu,Fei-Long Zhang,Xu-Bao Jiang,Xiang-Zheng Kong. Chinese Journal of Polymer Science. 2018(10)
[2]Biosynthesis of gold nanoparticles by Trichoderma sp.WL-Go for azo dyes decolorization[J]. Yuanyuan Qu,Wenli Shen,Xiaofang Pei,Fang Ma,Shengnan You,Shuzhen Li,Jingwei Wang,Jiti Zhou. Journal of Environmental Sciences. 2017(06)
[3]Preparation and Formation Mechanism of Porous Polyurea by Reaction of Toluene Diisocyanate with Water and Its Application as Adsorbent for Anionic Dye Removal[J]. Shu-sheng Li,Hui Han,朱晓丽,Xu-bao Jiang,孔祥正. Chinese Journal of Polymer Science. 2015(08)
[4]A novel and simple pathway to synthesis of porous polyurea absorbent and its tests on dye adsorption and desorption[J]. Shu-Sheng Li,Xiang-Zheng Kong,Xu-Bao Jiang,Xiao-Li Zhu. Chinese Chemical Letters. 2013(04)
[5]Synthesis and Characterization of Suspension Polymerized Styrene-Divinylbenzene Porous Microsphere Using as Slow-Release-Active Carrier[J]. 李璐,程江,文秀芳,皮丕辉,杨卓如. Chinese Journal of Chemical Engineering. 2006(04)
本文编号:3570761
【文章来源】:济南大学山东省
【文章页数】:136 页
【学位级别】:博士
【文章目录】:
Abstract
Chapter1 Introduction
1.1 Polyurea Materials
1.1.1 Historical Perspective of PU
1.2 Porous Polymer Microspheres
1.2.1 Preparation Methods of Porous Polymer Microspheres
1.2.1.1 Precipitation Polymerization
1.2.1.2 Interfacial Polymerization
1.2.1.3 Microfluidics
1.3 PU Microspheres
1.4 Polymer-Metal Composite Microspheres
1.5 Motivation of the Thesis
Chapter2 Preparation of Highly Uniform and Porous PU Microspheres(PPM)
2.1 Introduction
2.2 Experimental Section
2.2.1 Materials Details
2.2.2 Laboratory Equipment
2.2.3 Microfluidic Device Design
2.2.4 Characterization of PPM
2.3 Results and Discussions
2.3.1 PPM Formation Mechanism
2.3.2 Effect of Aqueous Phase Flow Rate on PPM Formation
2.3.3 Effect of TDI Flow Rate on PPM Formation
2.3.4 Effect of PVA Amount on PPM Formation
2.3.5 Effects of Polymerization Time
2.3.6 Effects of Polymerization Temperature
2.3.7 PPM Morphology Observation by SEM
2.3.8 Porous Properties of PPM
2.4 Summary
Chapter3 Preparation of Pd-PPM Composites by Different Process(Pd@PPM1,Pd@PPM2)
3.1 Introduction
3.2 Experimental Section
3.2.1 Synthesis Approach of Pd@PPM1 and Pd@PPM
3.2.2 Characterization
3.3 Results and Discussion
3.3.1 Preparation of Pd@PPM1 and Pd@PPM
3.3.2 Morphology observation by OM and SEM
3.3.3 Porous Properties
3.3.4 EDX Analysis
3.3.5 FTIR Analysis
3.3.6 XRD Analysis
3.3.7 NMR Analysis
3.3.8 XPS Analysis
3.3.9 H_2-TPR Analysis
3.4 Summary
Chapter4 Pd-PPM Composites as Catalyst in Dye Degradations
4.1 Introduction
4.2 Experimental Section
4.2.1 Degradation of Dyes by Pd@PPM1 and Pd@PPM
4.3 Results and Discussion
4.3.1 MO Degradation
4.3.2 Rh B Degradation
4.3.3 MB Degradation
4.3.4 Mechanism of Dyes Degradation
4.3.5 Reusability of Pd@PPM1 and Pd@PPM2 in Dyes Degradation
4.4 Summary
Chapter5 Pd-PPM Composites as Catalyst in4-NP Reduction
5.1 Introduction
5.2 Experimental Section
5.2.1 4-NP Reduction by Pd@PPM1 and Pd@PPM
5.2.2 Characterization
5.3 Results and Discussion
5.3.1 CO Pulse Chemisorption Analysis
5.3.2 Catalytic Activity of Pd@PPM2 for4-NP Reduction
5.3.3 Effect of Pd@PPM2 Amount on4-NP Reduction
5.3.4 Effect of NaBH_4 Amount on4-NP reduction
5.3.5 Pd Loading Effect on Pd@PPM2 Activity for4-NP Reduction
5.3.6 Effect of 4-NP Initial Concentration
5.3.7 Effect of Temperature on4-NP Reduction
5.3.8 Effect of pH on4-NP Reduction
5.3.9 4-NP Reduction by Pd@PPM
5.3.10 Catalytic Activity Comparison of Pd@PPM1 to Pd@PPM2 in4-NP Reduction
5.3.11 Mechanism of4-NP Reduction
5.3.12 Reusability of Pd@PPM1 and Pd@PPM2 in4-NP Reduction
5.4 Summary
Chapter6 Pd@PPU Composite as Catalyst in Cr~(6+)Reduction
6.1 Introduction
6.2 Experimental Section
6.2.1 Preparation of Pd@PPU
6.2.2 Characterization f Pd(OAc)2@PPU and Pd@PPU
6.2.3 Catalytic Performance of Pd@PPU in Cr~(~(6+)) Reduction
6.3 Results and Discussion
6.3.1 Synthesis and Characterizations of Pd@PPU
6.3.2 Morphology observation by OM and SEM
6.3.3 EDS Analysis
6.3.4 BET Analysis
6.3.5 FTIR Analysis
6.3.6 NMR Analysis
6.3.7 XPS Analysis
6.3.8 XRD Analysis
6.3.9 TEM Analysis
6.3.10 Performance of Pd@PPU for the Reduction of Cr~(6+)to Cr~(3+)
6.3.11 Effect of Pd Amount on Cr~(6+)Reduction
6.3.12 Effects of FA and SF Concentrations on Cr~(6+)Reduction
6.3.13 Effect of Initial Concentration of K2Cr2O7 on Catalytic Activity of Pd@PPU
6.3.14 Effect of Temperature on Cr~(6+)Reduction
6.3.15 Mechanism of Cr~(6+)Reduction
6.3.16 Catalytic Activity Comparison of Pd@PPU with Commercial Pd@C
6.3.17 Reusability of Pd@PPU
6.4 Summary
Chapter7 Conclusions and Future Outlook
7.1 Conclusions
7.2 Future Outlook
References
Acknowledgements
Appendix
【参考文献】:
期刊论文
[1]NMR Analysis to Identify Biuret Groups in Common Polyureas[J]. Wei-Guang Qiu,Fei-Long Zhang,Xu-Bao Jiang,Xiang-Zheng Kong. Chinese Journal of Polymer Science. 2018(10)
[2]Biosynthesis of gold nanoparticles by Trichoderma sp.WL-Go for azo dyes decolorization[J]. Yuanyuan Qu,Wenli Shen,Xiaofang Pei,Fang Ma,Shengnan You,Shuzhen Li,Jingwei Wang,Jiti Zhou. Journal of Environmental Sciences. 2017(06)
[3]Preparation and Formation Mechanism of Porous Polyurea by Reaction of Toluene Diisocyanate with Water and Its Application as Adsorbent for Anionic Dye Removal[J]. Shu-sheng Li,Hui Han,朱晓丽,Xu-bao Jiang,孔祥正. Chinese Journal of Polymer Science. 2015(08)
[4]A novel and simple pathway to synthesis of porous polyurea absorbent and its tests on dye adsorption and desorption[J]. Shu-Sheng Li,Xiang-Zheng Kong,Xu-Bao Jiang,Xiao-Li Zhu. Chinese Chemical Letters. 2013(04)
[5]Synthesis and Characterization of Suspension Polymerized Styrene-Divinylbenzene Porous Microsphere Using as Slow-Release-Active Carrier[J]. 李璐,程江,文秀芳,皮丕辉,杨卓如. Chinese Journal of Chemical Engineering. 2006(04)
本文编号:3570761
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