论文总字数：16645字

摘 要

本论文先用Na₂WO₄·2H₂O和H₃BO₃合成K₇BW₁₁O₃₉Ni。然后，采用化学氧化法、以盐酸为掺杂剂制备聚苯胺，用K₇BW₁₁O₃₉Ni与之发生置换反应，再用碱液处理得到本征态聚苯胺EB，最后用不同量的K₇BW₁₁O₃₉Ni和盐酸共同对EB进行再掺杂，制备含BW₁₁O₃₉Ni^7-的PANI复合材料，结合红外光谱、XRD、电导率测试，研究PANI再掺杂性能。

实验结果表明，制备的K₇BW₁₁O₃₉Ni是具有keggin结构的杂多酸盐。通过再掺杂制备的含BW₁₁O₃₉NI^7-的PANI复合材料既具有PANI结构，杂多阴离子BW₁₁O₃₉NI^7-也进入了聚合物链。

对最终产物的FTIR、XRD光谱分析表明，进入PANI链的杂多阴离子BW₁₁O₃₉NI^7-的数目与合成条件有关，K₇BW₁₁O₃₉Ni的用量为0.6 g时数目最多。对0.9 g和1.5 g的聚苯胺样品，虽然合成时K₇BW₁₁O₃₉Ni的量在增大，但溶液中过多的杂多酸离子抑制了其进入聚苯胺链的数目。

通过对样品的TG分析和电导率测量后发现，掺杂了K₇BW₁₁O₃₉Ni的PANI具有更良好的导电性能和热稳定性，其中K₇BW₁₁O₃₉Ni的用量为0.6 g那组样品的导电性能最佳，这说明聚苯胺的电导率与进入聚苯胺链的BW₁₁O₃₉NI^7-的数目有关，杂多阴离子数目越多，电导率越高。

关键词 :聚苯胺 多金属氧酸盐 化学氧化法 掺杂

Re - doping Properties of PANI Composites Containing BW₁₁O₃₉NI^7-

Abstract

In this paper, K₇BW₁₁O₃₉Ni was synthesized by Na₂WO₄ · 2H₂O and H₃BO₃.Then, the use of chemical oxidation, hydrochloric acid as a dopant to prepare polyaniline,replacement reaction with K₇BW₁₁O₃₉Ni,and then treated with lye to obtain the intrinsic polyaniline EB,Finally, PANI composites containing BW₁₁O₃₉Ni^7- were prepared by re-doping EB with different amounts of K₇BW₁₁O₃₉Ni and hydrochloric acid,combined with infrared spectroscopy, XRD, conductivity test, study PANI re-doping performance.

The experimental results show that the prepared K₇BW₁₁O₃₉Ni is a heteropoly acid salt with keggin structure.The PANI composites containing BW₁₁O₃₉NI^7- prepared by re-doping have both PANI structure and hetero-anionic BW₁₁O₃₉NI^7- have also entered the polymer chain.

The FTIR and XRD spectra of the final product show that the number of heteropolyanion BW₁₁O₃₉NI^7- into the PANI chain is related to the synthesis conditions, and the number of K7BW11O39Ni is the largest when the dosage is 0.6g.For the 0.9 g and 1.5 g polyaniline samples, although the amount of K₇BW₁₁O₃₉Ni was increased during synthesis, too much heteropolyacid ions in the solution inhibited the number of polyaniline chains into the polyaniline chain.

Through the TG analysis and conductivity measurement of the sample, it was found that PANI doped with K₇BW₁₁O₃₉Ni had better conductivity and thermal stability.Which K₇BW₁₁O₃₉Ni dosage of 0.6g that group of samples of the best conductivity,this indicates that the conductivity of polyaniline is related to the number of BW₁₁O₃₉NI^7- entering the polyaniline chain,the more the number of heteropolyanions, the higher the conductivity.

Key words: polyaniline polyoxometalate chemical oxidation doping

摘要 I

Abstract II

第一章 文献综述 1

1.1 多金属氧酸盐简介 1

1.2 聚苯胺介绍 2

1.2.1 聚苯胺的优点及其应用 2

1.3 POMs/PANI的研究现状 5

1.4小结 6

第二章 产物合成及表征方法和原理 7

2.1 实验部分 7

2.1.1 主要试剂 7

2.1.2 主要仪器 8

2.1.3 含BW11O39NI7-的PANI复合材料的合成 8

2.2 表征方法及原理 9

2.2.1 红外光谱（IR) 9

2.2.2 X射线衍射法（XRD） 9

2.2.3 热重法（TG） 10

2.2.4 电导率（ 四探针法） 10

第三章实验结果和分析 11

3.1 钨硼酸镍钾的表征 11

3.1.1 K₇BW₁₁O₃₉Ni的红外吸收光谱 11

3.1.2 K₇BW₁₁O₃₉Ni的x射线衍射谱图 12

3.2 含BW₁₁O₃₉NI^7-的PANI复合材料的表征 12

3.2.1含BW₁₁O₃₉NI^7-的PANI复合材料的红外吸收光谱 13

3.2.2 含BW₁₁O₃₉NI^7-的PANI复合材料的x射线衍射谱图 14

3.2.3 含BW₁₁O₃₉NI^7-的PANI复合材料的电导率 15

3.2.4 含BW₁₁O₃₉NI^7-的PANI复合材料的热重曲线分析 15

第四章 结论和展望 17

参考文献 19

致谢 21

第一章 文献综述

1.1 多金属氧酸盐简介

多金属氧酸盐（Polyoxometalates,缩写为POMs），是一种含有多核金属中心的金属氧簇化合物。经过漫长的科学研究，POMs慢慢的成为了无机化学中不可分割的一部分，由于POMs的结构和性质非常稀有，因而它在许多学科上都有着突出的贡献。近几年的科学研究表明，POMs在电化学，高分子化学，材料化学等领域备受青睐^[1]。、

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