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1、. . . .ClassifiedIndex: TB333U.D.C: 620.3Southwest Universityof Science and TechnologyMaster Degree ThesisPreparation of Methoxy Polyethylene Glycol Stabilized Gold Nanoparticles and Their Applications for Detection and Absorption of AcrylamideGrade: 2012Candidate: xxxAcademic Degree Applied for: Ma
2、ster DegreeSpeciality: Materials Science and EngineeringSupervisor: Professor xxx Professor xxxpr 1, 2015独 创 性 声 明本人声明所呈交的论文是我个人在导师指导下进行的研究工作及取得的研究成果。尽我所知,除了文中特别加以标注和致谢的地方外,论文中不包含其他人已经发表或撰写过的研究成果,也不包含为获得西南科技大学或其它教育机构的学位或证书而使用过的材料。与我一同工作的同志对本研究所做的任何贡献均已在论文中作了明确的说明并表示了谢意。签 名: 日 期: 关于论文使用和授权的说明本人完全了解西南
3、科技大学有关保留、使用学位论文的规定,即:学校有权保留学位论文的复印件,允许该论文被查阅和借阅;学校可以公布该论文的全部或部分内容,可以采用影印、缩印或其他复制手段保存论文。(保密的学位论文在解密后应遵守此规定)签 名: 导师签名: 日 期: 学习参考. . . .摘要本文以聚乙二醇单甲醚(PEG)为原料,制备了聚乙二醇单甲醚纳米金(PEG-纳米金),并将聚乙二醇巯基功能化后制备了巯基化聚乙二醇单甲醚纳米金(PEG-HS-纳米金),然后将两种纳米金分别用于有毒小分子丙烯酰胺的检测和吸附上。建立了一种基于聚乙二醇单甲醚稳定的纳米金可视化检测丙烯酰胺(AA)的新方法,并用透射电子显微镜(TEM)、
4、紫外可见光光度计(UV)、激光粒度分析仪(DLS)对聚乙二醇纳米金进行测试分析。结果表明:该聚乙二醇纳米金核呈分散均匀的规则球体,且其平均粒径为19nm。颗粒整体(纳米金核和表面稳定剂)粒径集中分布在40 nm。浓度为0.004 mg/mL的丙烯酰胺能使聚乙二醇纳米金发生团聚,胶体由红色变成紫色,浓度在0.004 mg/mL-0.032 mg/mL之间时,团聚程度随浓度的增加而增加,同时颗粒整体粒径依次增大到170 nm、250 nm、600 nm。相同条件下,N, N-二甲基丙烯酰胺(DMAA)不能使聚乙二醇纳米金发生团聚。因此,可用该方法简单、快速的实现丙烯酰胺选择性检测。将巯基化聚乙二醇
5、纳米金用于丙烯酰胺吸附,研究了其吸附性能、吸附机理以及循环利用。氢核磁(1H-NMR)、高效液相色谱(HPLC)、紫外可见分光光谱(UV)、透射电子显微电镜(TEM)、激光粒度分析仪(DLS)等测试表明:该巯基化聚乙二醇纳米金在有机溶剂和水溶液中均能吸附丙烯酰胺,但不吸附N, N-二甲基丙烯酰胺,这种吸附来源于丙烯酰胺的氢原子与巯基化聚乙二醇的氧原子之间的氢键。二氯甲烷中每个巯基化聚乙二醇纳米金平均吸附25772个丙烯酰胺分子,水溶液中每个巯基化聚乙二醇纳米金平均吸附22420个丙烯酰胺分子,比二氯甲烷中少,这可能是水溶液中水分子使丙烯酰胺与聚乙二醇之间的氢键作用减弱。另外,该巯基化聚乙二醇纳
6、米金前4次循环团聚较少,循环5次之后,团聚量超过50%,这可能是多次离心使纳米金产出团聚引起的。因此,该巯基化聚乙二醇纳米金可能成为新型可循环利用的有毒小分子吸附剂。关键词:聚乙二醇;纳米金;丙烯酰胺;检测;吸附AbstractIn this paper, methoxy polyethylene glycol(PEG) stabilized gold nanoparticles(PEG-AuNPs)and thiol functionalized PEG stabilized gold nanoparticles (PEG-HS-AuNPs) have been prepared. Then
7、 these two gold nanoparticles were used in the detection and adsorption of the toxic small molecules, e.g. acrylamide, respectively.Firstly, the novel visual method for the detection of acrylamide by PEG-AuNPs has been developed. The PEG-AuNPs were characterized by transmission electron microscopy (
8、TEM), ultraviolet spectrophotometer (UV), Dynamic Light Scattering (DLS). The results indicated that the size of the spherical AuNP core was 19 nm and well dispersed. In addition, the size of PEG-AuNPs (including Au cores and surface stabilizers) was around 40 nm. Significantly, 0.004 mg/mL acrylami
9、de could induce the aggregation of the PEG-AuNPs, which caused the color changing of the colloidal solution from red to purple. The aggregations of AuNPs enhanced with the increase of acrylamide concentration from 0.004 mg/mL to 0.032 mg/mL. However, N, N-dimethylacrylamide could not induce aggregat
10、ion of PEG-AuNPs under the same condition. Therefore, this method could provide new opportunities for the rapid, simple and selective detection of acrylamide.Secondly, PEG-HS-AuNPs were used to adsorb acrylamide. The adsorption capacity, adsorption mechanism and recycling have been studied. The PEG-
11、HS-AuNPs were characterized by 1H-NMR, HPLC, TEM, UV and DLS, and the results indicated that the PEG-HS-AuNPs could adsorb acrylamide both in hydrophobic and aqueous media, but could not adsorb N, N-dimethylacrylamide. The adsorption was attributed to the hydrogen bonding between the proton in acryl
12、amide and the oxygen atom in the PEG-HS-AuNPs. Each PEG-HS-AuNP could adsorb about 25772 acrylamide molecules in CH2Cl2, and about 22420 acrylamide molecules in aqueous media, which was less than that in CH2Cl2, This may due to the presence of the H2O in the aqueous media which weakened the hydrogen
13、 bonding between the PEG-HS-AuNPs and the acrylamide. In addition, the PEG-HS-AuNPs could recycled 4 times with small agglomeration, and after 5 times, more than 50% gold nanoparticles are aggregated. This may due to the agglomeration during centrifugation process. Therefore, PEG-HS-AuNPs could be a
14、 new recyclable adsorbent for toxic small molecules.Keywords: methoxy polyethylene glycol; gold nanoparticles; acrylamide; detection; adsorption学习参考目录1绪论11.1聚乙二醇性质及其应用11.1.1聚乙二醇性质简介11.1.2聚乙二醇及其衍生物的应用21.2纳米金制备方法及其应用51.2.1纳米金的制备方法51.2.2功能化巯基配体修饰纳米金的方法81.2.3纳米金的应用91.3聚乙二醇纳米金的应用121.4丙烯酰胺的检测及吸附方法131.4.1丙
15、烯酰胺的检测方法131.4.2丙烯酰胺吸附方法161.5本课题研究意义和主要研究内容171.5.1本课题研究意义171.5.2本课题主要研究内容182聚乙二醇纳米金的制备及表征192.1引言192.2实验部分192.2.1主要药品及仪器192.2.2PEG-纳米金的制备202.2.3PEG-HS-纳米金的制备212.2.4样品表征方法和仪器242.3结果与讨论252.3.1UV光谱分析PEG-纳米金252.3.2TEM分析PEG-纳米金262.3.3DLS分析PEG-纳米金272.3.41H-NMR分析PEG-HS-纳米金282.3.5UV光谱分析PEG-HS-纳米金312.3.6TEM分析PEG-HS-纳米金332.3.7EDS能谱分析PEG-HS-纳米金342.3.8DLS分析PEG-HS-纳米金352.