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研究生(外文):Yi-Hsuan Chen
論文名稱(外文):The Optimal Manufacturing Processes of Nano-silver/Polypropylene Plastics for Antibacterial Application
指導教授(外文):Jerry J. Wu
中文關鍵詞:消毒聚乙烯吡咯烷酮 (PVP)奈米銀聚丙烯微波抑菌
外文關鍵詞:Nano-silverPolyvinyl pyrrolidone (PVP)PolypropyleneAntibacterial abilityDisinfectionMicrowave radiation
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本論文主要利用硝酸鐵/過硫酸銨混合溶液來進行疏水性聚丙烯表面的改質,使表面生成極性含氧官能基而變轉為親水性,並透過原位合成的方法,改變各項參數條件來製作出最佳化的Ag/PP複合材料,最後利用上述材料進行對E. coli和S. aureus消毒的影響。
經過1~8小時不同時間的改質,氧化劑FeO2+會氧化聚丙烯的碳鏈而生成極性官能基(C-OH和COOH等),使接觸角度由103.9˚降至 93.9˚,顯示表面已轉變為較極性的狀態;然後利用前述改質後聚丙烯作為載體嵌接PVP,PVP可藉由立體效應減低奈米銀顆粒的團聚效應。利用FTIR-ATR分析不同比例的PVP嵌接情形,發現4%的PVP水溶液與基材接觸時間達18小時可達到最佳的附著量,也代表此條件可鍵結上最多的奈米銀顆粒。然後利用25℃~80℃製作溫度將同濃度硝酸銀還原至基材表面上,當溫度越高時,有效碰撞可導致較多的奈米銀鍵結在基材表面上,因此可得到較佳的消毒效果。本研究使用不同濃度的硝酸銀(0.005~0.5 M)發現在固定面積PP表面添加過多的銀離子會造成銀的團聚,使消毒效果反而變差,0.01 M的硝酸銀濃度為最佳添加條件。
為了瞭解Ag/PP材料的可重複使用性,經消毒後之Ag/PP進行四次重複消毒試驗,當進行到第三次測試時,因為奈米銀的逐漸脫落導致每小時去除率下降了約0.85 Log的細菌量。此現象經新製程-加熱軟化法在高溫條件使聚丙烯與奈米銀彼此交纏在一起,在經過三次重複使用皆與初次使用有類似的效果,並利用四次的抑菌實驗得知,細菌在與材料有接觸的地方並不會長出菌落,可有利於本研發材料的長久使用。兩種製程的Ag/PP材料在經過微波幅射後,發現表面含銀量都有減少的趨勢,導致消毒結果變差,因此本材料目前尚不適宜應用於微波爐內加熱使用。
Ammonium persulfate/ferric nitrate mixtures have been used in this thesis to modify the hydrophobic surface of polypropylene (PP) with allowing polar oxygen-containing functional groups to grow on and become hydrophilic. In-situ synthesis method was then utilized to optimize Ag/PP composite materials by performing different experimental parameters. Finally, E. coli and S. aureus were chosen as the target bacteria for disinfection tests to evaluate the efficacy of using the novel Ag/PP composite materials against microorganisms.
After 1 to 8 hours of modification using oxidation agent, FeO2+ could oxidize the surface of carbon chain to derive the formation of new polar functional groups, such as C-OH and COOH, and the contact angle decreases from 103.9°to 93.9°, indicating that the surface is directed towards polar state. Subsequently polyvinyl pyrrolidone (PVP) was use as a carrier to adhere on the modified PP surface and to prevent the agglomeration of nano silver particles. 4% PVP concentration and 18 hours reaction time were figured out by FTIR-ATR to have the most amounts of nano silver particles. The higher temperature would lead to more effective collision for silver reduction process using nitrate silver as the precursor between 25 to 80℃ and the disinfection efficiency is also corresponding as well. It is found that the addition of 0.01 M silver nitrate has provided the optimal disinfection efficiency due to the aggregation function of silver particles at higher concentration as used.
In order to understand the repeatability of Ag/PP composite for disinfection, four consecutive disinfection tests have been carried out in our experiment. However, it was found the silver content on the Ag/PP becomes less compared to the original one and the disinfection rate falls down to 0.85 Log per hour. After a new preparation process, heat-softening synthesis, was involved in this research, it is found that silver could be better attached on the surface of PP substrate and the disinfection efficiency would not become worse after repeated disinfection, which has also been demonstrated by the inhibitory loop analysis. However, these two types of Ag/PP composites can not resist on microwave radiation due to the dissolution loss of locally high temperature over the melting point of silver element. Therefore, it is not suitable so far to use the Ag/PP composites as microwave containers.
中文摘要 I
1-1 Research Motivation 1
1-2 Research Objectives 2
2-1 Introduction of Polypropylene 3
2-1-1 Structure of Polypropylene 4
2-1-2 Properties of Polypropylene 6
2-2 Surface Modification of Polypropylene 7
2-3 Thermoplastic Composites 9
2-3-1 Types of Thermoplastic Composites 10
2-3-2 Glass Transition Temperature 12
2-3-3 The State-of–the-art of Thermoplastic Composites Studies 13
2-4 Characteristics of Silver 14
2-4-1 Nano silver 15
2-4-2 Preparation of Nano Particles 16
2-4-3 Physical Effect of Nano Material 17
2-4-4 Characterization of Metal Silver after Nano-technology 18
2-5 Antibacterial Mechanism of Silver 21
2-5-1 Silver Bactericidal Concentration and Inhibitory Concentration to Microorganism 25
2-5-2 Bactericidal Mode 27
2-6 Selected References for Silver Disinfection Studies 27
2-7 Use of Protective Agent 28
3-1 Framework and Details of the Experiment 36
3-1-1 Preparation of Materials 36
3-1-2 Disinfection and Antibacterial Inhibition Test 36
3-2 Chemicals and Apparatus Used in the Experiment 39
3-2-1 Chemcials for Material Preparation 39
3-2-2 Microorganisms and Chemicals for Disinfection Test 39
3-2-3 Apparatus 40
3-3 Experimental Procedures 40
3-3-1 Modification of Polypropylene Plastics 40
3-3-2 Implantation of PVP 40
3-3-3 Silver Deposition on the Surface of Modified Polypropylene 41
3-3-4 Analysis of Silver Concentration on Nano-silver/Polypropylene (Ag/PP) Material 41
3-3-5 Hot-softing 42
3-3-6 Disinfection Test of Ag/PP Composite Materials 42
3-4 Characterization Methods of Materials Analysis 43
3-5 Repeated Test 47
3-6 Microwaves Radiation 47
4-1 Preparation of Composite Materials 48
4-1-1 FTIR Detection of PP Modification 48
4-1-2 Contact Angle Analysis of Modified Polypropylene 52
4-1-3 SEM Analysis of Polypropylene Modification 53
4-1-4 FTIR Analysis of the Protective Agent (PVP) Addition 54
4-1-5 Addition and Reduction of Silver Nitrate 56
4-1-6 Comparison of Adding Different Concentrations of Silver Nitrate on the Substrate 59
4-1-7 Comparison of Ag/PP Disinfection Efficiency at Different Synthesis Temperature 61
4-1-8 Comparison of Ag/PP Disinfection Efficiency by Adding Different Concentrations of Silver Nitrate in the Synthesis Process 65
4-2 Characteristic Analysis of Materials 69
4-2-1 Material Surface Structure and Chemical Element Composition 69
4-2-2 XRD Analysis of Ag/PP 73
4-2-3 SERS Measurements 74
4-3 Novel Ag/PP Composite Synthesized by Heat-softening 75
4-3-1 SEM Analysis 76
4-3-2 XPS Analysis 77
4-3-3 FTIR Analysis 79
4-4 Repeated Tests for Disinfection Application 79
4-4-1 Disinfection Application Using Ag/PP by Modification Preparation 79
4-4-2 Disinfection Using Ag/PP by Heat-softening Preparation 82
4-5 Microwave radiation Test for Ag/PP Composites 84
4-5-1 Surface Analysis on Materials by Modification Preparation 84
4-5-2 Effect on Disinfection Efficiency Using Microwave Radiation by Modification Preparation 85
4-5-3 Effect on Disinfection Efficiency Using Microwave Radiation by Hot-softing Preparation 87
4-5-4 Antibacterial Activity by Ag/PP Using Heat-softening Synthesis 89
4-5-5 Antibacterial Activity by Two Methods After Microwave Radiation 91
5-1 Conclusions 93
5-2 Suggestions 94
References 95
Fig. 2-1 Molecular structure of isotactic polypropylene 5
Fig. 2-2 Molecular structure of syndiotactic polypropylene 5
Fig. 2-3 Molecular structure of abnormal polypropylene 5
Fig. 2-4 Concept of biological surface modification 8
Fig. 2-5 Antibacterial mechanism of silver 23
Fig. 2-6 Silver disintegrate the cell membrane and organelle 24
Fig. 2-7 Architecture of a multiply active antimicrobial PEI net work film 31
Fig. 2-8 Synthesis of Ag MPCs using sodium S-dodecylthiosulfate in H2O 32
Fig. 2-9 Preparation of silver nanocomposite LBL multilayer films and structures of polyelectrolytes. 33
Fig. 2-10 PVP formula 34
Fig. 2-11 Protective mechanisms of silver by PVP 35
Fig 3-1 Overall experimental flowchart in this study 37
Fig 3-2 Detailed Experimental Conditions in the Research 38
Fig. 4-1 In 25℃, FTIR spectrum at different modification time 51
Fig. 4-2 The same modification of six hours, FTIR spectrum at different modification temperature 51
Fig. 4-3 The change of contact angle 53
Fig. 4-4 The modified surface conditions of the SEM graph 53
Fig. 4-5 FTIR of adding different ratio of protective agent 55
Fig. 4-6 FTIR of protection agents at different immersion times 56
Fig. 4-7 The TEM results of nano-silver particles at different ratios of PVP protective agents 58
Fig. 4-8 SEM Fig.s for PP substrate deposited by silver particles under different temperatures 60
Fig. 4-9 EDS diagram of Ag-contained PP at 80℃. 61
Fig. 4-10 Effect of Ag/PP synthesis process at different temperatures on 63
E. coli disinfection 63
Fig. 4-11 Effect of Ag/PP synthesis process at different temperatures on 64
S. aureus disinfection 64
Fig. 4-12 Diagram of Inhibition zone experiment at different synthesis temperatures 64
Fig. 4-13 The SEM micrographs of different silver nitrate concentrations deposited on the substrate 66
Fig. 4-14 The EDS diagram of Ag/PP using 0.01 M of silver nitrate 67
Fig. 4-15 The disinfection effect on E. coli using different concentrations of silver nitrate for Ag/PP synthesis processes 68
Fig. 4-16 The disinfection effect on S. aureus using different concentrations of silver nitrate for Ag/PP synthesis processes 68
Fig. 4-17 XPS analysis spectrum of composite materials 70
Fig. 4-18 XPS analysis for Ag 3d spectrum of composite materials 71
Fig. 4-19 XPS analysis for C 1s spectrum of composite materials 71
Fig. 4-20 XPS analysis for O 1s spectrum of composite materials 72
Fig. 4-21 XPS analysis for N1s spectrum of composite materials 72
Fig. 4-22 XPS analysis for Ag 3d spectrum under different temperature synthesis processes 73
Fig. 4-23 XRD spectrum for Ag/PP 74
Fig. 4-24 SERS spectrum of PP and Ag/PP 75
Fig. 4-25 The SEM and EDS analysis of Ag/PP composite by 76
heat-softening synthesis 76
Fig. 4-26 XPS analysis Ag 3d spectrum of Ag/PP composite by heat-softening synthesis 78
Fig. 4-27 XPS analysis N 1s spectrum of Ag/PP composite by heat-softening synthesis 78
Fig. 4-28 The FTIR of Ag/PP composite by heat-softening synthesis 79
Fig. 4-29 Disinfection on E. coli by consecutive uses of Ag/PP 81
Fig. 4-30 Disinfection on S. aureus by consecutive uses of Ag/PP 81
Fig. 4-31 Disinfection effect on E. coli by heat-softening synthesis 83
Fig. 4-32 Disinfection effect on S. aureus by heat-softening synthesis 87
Fig. 4-33 The FTIR analysis of Ag/PP after microwave radiation 84
Fig. 4-34 Contact angle measurement after microwave radiation 85
Fig. 4-35 Disinfection effect on E. coli under different radiation time 86
by microwave 86
Fig. 4-36 Disinfection effect on S. aureus under different rediation time by microwave 91
Fig. 4-37 Disinfection effect on E. coli by heat-softening synthesis under different microwave radiation time 88
Fig. 4-38 Disinfection effect on S. aureus by heat-softening synthesis under different microwave radiation time 89
Fig. 4-39 The antibacterial activity of Ag/PP composite by 90
Fig. 4-40 The antibacterial activity of microwave by modification method 91
Fig. 4-41 The antibacterial activity of microwave by modification method 92

Table 2-1 Types of the thermoplastic composite materials 11
Table 2-2 Metal silver concentration in nature 15
Table 2-3 Silver bactericidal concentration and inhibitory concentration to microorganism 25
Table 4-1 EDS analysis of silver content on modified PP at 80℃. 61
Table 4-2 Silver weight ratio on PP synthesized at different temperatures 61
Table 4-3 The first-order lethal rate constants for the disinfection of E. coli and S. aureus at different synthesis temperatures 65
Table 4-4 The EDS analysis of Ag/PP using 0.01 M silver nitrate 67
Table 4-5 The silver concentration on PP under different silver nitrate concentrations addition. 67
Table 4-6 The first-order lethal rate constant using different concentrations of silver nitrate for Ag/PP synthesis processes 69
Table 4-7 The EDS analysis of Ag/PP composite by heat-softening synthesis 77
Table 4-8 The first-order lethal rate constant for disinfection under a consecutive uses of Ag/PP composites 82
Table 4-9 Silver weight ratios on Ag/PP under different microwave radiation time 86
Table 4-10 The first-order lethal rate constants for the disinfection test underdifferent rediation time by microwave 87
Table 4-11 Silver weigh ratios on PP by heat-softening synthesis under different microwave rediation treatment time 89
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