基于纳米银的几种抗菌膜的合成、表征及性能评价

论文总字数：26003字

摘 要

银具有广谱抗菌、抗菌高效以及安全无毒等突出的优势；纳米尺寸的银粒子拥有小尺寸效应、和宏观量子隧道效应、表面效应等优势，纳米技术的发展,使银在纳米形态下的抗菌能力产生了质的变化。纳米银抗菌剂存在多种形式，如敷料,药膏,凝胶，纤维，塑料制品等。本文主要制备三种不同稳定剂存在下的纳米银，并进行涂膜操作，并且对制备的纳米银以及抗菌膜做出适当的的评价。本文采用氧化还原法分别制备以聚乙烯亚胺为稳定剂制备的纳米银AgNP A；用聚乙烯吡咯烷酮作为稳定剂制备的银纳米粒子AgNP B；以油酸为稳定剂制备的油溶性纳米银粒子AgNP C，并分别进行了聚氨酯制膜或硅橡胶制膜。在检测方面，我们对于制备的纳米银进行了紫外分析测试测试,纳米银在紫外光谱400nm左右有着明显的特征吸收峰，通过观察紫外谱图峰的位置就可以确定纳米银是否被成功制得；并经过透射电子显微镜可以直接观察纳米银的形状、粒径大小以及分散度。最终我们对抗菌膜利用最小抑菌浓度法对样品的对于大肠杆菌的抗菌性能进行定量计算，主要的研究结果如下：

1. 在室温下进行的AgNP A的制备过程中，采用稳定剂与硝酸银摩尔比1：50的配比，成功制备纳米银粒子并添加到聚氨酯膜中制备了抗菌膜。该纳米银粒子，紫外可见光谱表现出良好的正态分布，峰值出现在409nm处，说明成功制备了纳米银，TEM表现出粒径为8nm左右，抗菌膜的抗菌性能表现良好，抗菌率可达95.5%。
2. 在室温下进行的AgNP B得制备过程中，采用稳定剂与硝酸银摩尔比1：20的配比，成功制备纳米银粒子并添加到聚氨酯膜中制备了抗菌膜。紫外可见光谱表现出良好的正态分布，峰值出现在395nm处，说明成功制备了纳米银，TEM表现出该纳米银粒子粒径为15nm左右，抗菌膜的抗菌性能表现良好，抗菌率可达96.9%。
3. 在冰浴下进行的AgNP C的制备过程中，采用稳定剂与硝酸银摩尔比1：4的配比，成功制备纳米银粒子并添加到聚二甲基硅氧烷膜中制备了抗菌膜。紫外可见光谱表现出良好的正态分布，峰值出现在403nm处，说明成功制备了纳米银，TEM表现出该纳米银粒子粒径为15nm左右，抗菌膜的抗菌性能表现良好，抗菌率可达64.4%。

关键词：纳米银； 稳定剂； 抗菌； 抗菌膜

SYNTHESIS AND CHARACTERIZATION OF SEVERAL KINDS SILVER NANOPARTICLES AND PERFORMANCE EVALUATION OF ITS APPLICATION ON ANTIBACTERIAL FILM

Abstract

The antibacterial ability of silver has the advantages of high efficiency，broad spectrum and safety. Nanosized silver particles have the advantages of small size effect, macroscopic quantum tunneling effect, surface effect and so on. The emergence of nano technology bring about a qualitative leap of antibacterial ability to the silver in the nano version. Nano silver antibacterial agents exist in a variety of forms, such as dressing, ointment, gel, fiber, plastic products, etc. In this paper, three kinds of silver nanoparticles with different stabilizers were synthesized, and the coating operation was carried out. Then, appropriate evaluation for the nano silver as well as the antibacterial film was done. In the experiment, using the redox method, we synthesized three kinds of silver nanoparticles AgNP A, AgNP B, AgNP C,with PEI, PVP and oleic acid as stabilizer respectively. Then we coating the silver nanoparticles with polyurethane or polydimethylsiloxane. In characterization part, we analyzed the silver nanoparticles by UV analysis ,TEM and MIC. Nano silver has an obvious characteristic absorption peak in the ultraviolet spectrum around 400nm and the presence of nano silver can be determined quickly by UV spectra. What’s more, the distribution situation and the size of silver nanoparticles can be quickly assumed via the morphology of the UV spectrum. The morphology, particle size and dispersion of nano silver can be observed directly by transmission electron microscope, which is the most direct method for the characterization of nano silver. Finally we use the minimal inhibitory concentration method to do quantitative calculation for the ability of antibacterial membrane against Escherichia coli. The main results are as follows:

1. In preparation of AgNP A under room temperature, the molar ratio of stabilizer to silver nitrate is 1:50. The antibacterial film was synthesized with the successfully synthesized silver nanoparticles added to the polyurethane film. The nano silver particles’ uv-visible spectrum showed a good normal distribution, and at 409nm appeared the peak, which means silver nanoparticles were successfully synthesized. TEM showed the size of silver nanopartilces is about 8nm. The antibacterial film has good antibacterial performance, and the antibacterial rate is up to 95.5%
2. In preparation of AgNP B under room temperature, the molar ratio of stabilizer to silver nitrate is 1:20. The antibacterial film was synthesized with the successfully synthesized silver nanoparticles added to the polyurethane film. The nano silver particles’ uv-visible spectrum showed a good normal distribution, and the peak appeared at 395nm, which means silver nanoparticles were successfully synthesized. TEM showed the size of silver nanopartilces is about 15nm. The antibacterial film has good antibacterial performance, and the antibacterial rate is up to 96.9%
3. In preparation of AgNP C in ice bath, the molar ratio of stabilizer to silver nitrate is 1:4. The antibacterial film was synthesized with the successfully synthesized silver nanoparticles added to the polydimethylsiloxane film. The nano silver particles’ uv-visible spectrum showed a good normal distribution, and the peak appeared at 403nm, which means silver nanoparticles were successfully synthesized. TEM showed the size of silver nanopartilces is about 15nm. The antibacterial film has good antibacterial performance, and the antibacterial rate is up to 64.4%

KEY WORDS： silver nanoparticles; stabilizer; antibacterial; antibacterial membrane

目 录

摘要 ........................................................................................................I

Abstract ........................................................................................................II

第一章 绪论 ............................................................................................................1

1.1引言 .....................................................................................................1

1.2载银抗菌剂的发展 ...................................................................................1

1.3纳米银的抗菌性能与机理 ..........................................................................2

1.4纳米银的制备方法 ....................................................................................2

第二章 以聚乙烯亚胺为稳定剂制备纳米银 ...........................................................3

2.1实验部分 ..............................................................................................3

2.1.1实验试剂与仪器 ......................................................................3

2.1.2实验步骤 .........................................................................3

2.2表征部分 ...................................................................................3

2.2.1紫外检测结果与分析 ...............................................................4

2.2.2透射电镜检测结果与分析 ......................................................4

2.3本章小结 .............................................................................5

第三章 以聚乙烯吡咯烷酮为稳定剂制备纳米银 ............................................6

3.1实验部分 ............................................................................6

3.1.1实验试剂与仪器 ........................................................6

3.1.2实验步骤 ..............................................................6

3.2表征部分 .....................................................................7

3.2.1紫外检测结果与分析 ................................................7

3.2.2透射电镜检测结果与分析 ..............................................7

3.3本章小结 .........................................................................8

第四章 以油酸为稳定剂制备油溶性纳米银 ..............................................9

4.1实验部分 .............................................................................9

4.1.1实验试剂与仪器 .......................................................9

4.1.2实验步骤 .................................................................9

4.2表征部分 .......................................................................10

4.2.1紫外检测结果与分析 ...............................................10

4.2.2透射电镜检测结果与分析 ..............................................10

4.3本章小结 .........................................................................11

第五章 抗菌膜的制备与抗菌检测 ...........................................................12

5.1抗菌膜的制备 .....................................................................12

5.1.1实验试剂与仪器 ......................................................12

5.1.2实验步骤 .........................................................12

5.2抗菌检测结果 .................................................................13

5.3本章小结 ......................................................................15

结论 ...........................................................................................16

致谢 ....................................................................................17

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