论文总字数：23809字

摘 要

在众多的防腐措施中，涂层防护技术的使用最为普遍。防腐涂层作为一种聚合物基复合材料，在海洋、能源、建筑、交通、航空航天及军用装备等多个领域应用广泛。近年来，为了延长涂层的使用寿命，人们将自修复微胶囊技术应用到涂层领域。随着纳米材料的迅速发展，在涂层中加入具有优异防腐性能的石墨烯材料，将石墨烯和微胶囊相结合加入涂层中，均取得了一定的进展。为了更好地提升石墨烯微胶囊性能，需要对微胶囊的芯材进行了进一步的复合。本课题采用原位聚合法合成了以石墨烯和钨酸钠为复合芯材，脲醛树脂为壁材的复合型微胶囊，讨论在微胶囊中加入缓蚀剂钨酸钠来进一步提升石墨烯微胶囊的性能，并测试了复合型石墨烯微胶囊对涂料的影响，结果显示钨酸钠的加入能有效提升涂料的自修复性能。

粒径分析显示，当加入0.5%的缓蚀剂钨酸钠时，制备的微胶囊具有最小粒径。SEM图显示制备的微胶囊大小均一，直径约1um。交流阻抗结果显示，复合型石墨烯基微胶囊对涂料的修复性能要优于石墨烯微胶囊与钨酸钠的机械混合物，原理是钨酸钠与石墨烯分散剂十二烷基苯磺酸钠形成良好的协同缓蚀效应，且复合型微胶囊能够均匀分散在涂层中，有利于协同缓蚀效果的发挥。

关键词：微胶囊 石墨烯 缓蚀剂 钨酸钠

Study on preparation technology of composite graphene-based microcapsules

Abstract

Among the many anti-corrosion measures, coating protection technology is the most widely used. As a kind of polymer matrix composites, anticorrosive coatings are widely used in many fields, such as ocean, energy, construction, transportation, aerospace and military equipment. In recent years, in order to prolong the service life of coatings, self-repairing microcapsules have been applied to coatings. With the rapid development of nano-materials, the addition of graphene materials with excellent anticorrosive properties to coatings and the combination of graphene and microcapsules into coatings have made some progress. In order to improve the performance of graphene microcapsules, the core materials of microcapsules need to be further compounded. In this paper, sodium tungstate as corrosion inhibitor was added to the microcapsules to further improve the performance of graphene microcapsules, and the effect of composite graphene microcapsules on the coating was discussed.Composite microcapsules with graphene and sodium tungstate as composite cores and urea-formaldehyde resin as wall materials were synthesized by in-situ polymerization. The results show that the self-repairing properties of the coatings can be effectively improved by adding sodium tungstate.

The particle size analysis showed that when 0.5% sodium tungstate was added, the prepared microcapsules had the smallest particle size. SEM images showed that the prepared microcapsules were uniform in size and about 1 um in diameter. The results of AC impedance show that the composite graphene-based microcapsules are superior to the mechanical mixture of graphene microcapsules and sodium tungstate. The principle is that sodium tungstate and graphene dispersant sodium dodecylbenzene sulfonate form a good synergistic corrosion inhibition effect, and the composite microcapsules can be uniformly dispersed in the coating, which is conducive to the synergistic corrosion inhibition effect.

Key words: Microcapsule;graphene ;corrosion inhibitor ;sodium tungstate

目录

摘 要 I

Abstract II

第一章 绪论 1

1.1 涂层防护技术简介 1

1.1.1 涂层防护机制 1

1.1.2 涂层失效机制 1

1.1.3 涂层优化技术的研究进展 3

1.2 涂料用微胶囊的研究进展 6

1.2.1 异氰酸酯型微胶囊在涂层防护中的应用 6

1.2.2环氧树脂型微胶囊在涂层防护中的应用 6

1.2.3 缓蚀－腐蚀抑制剂型微胶囊在涂层防护中的应用 7

1.3 石墨烯复合涂料的研究进展 8

1.3.1 制备技术 8

1.3.2石墨烯的原位改性 9

1.4 石墨烯基微胶囊的研究进展 10

1.5 本课题研究意义及主要研究内容 11

第二章 实验 12

2.1 所需仪器和药品 12

2.1.1 主要仪器 12

2.1.2 药品 12

2.2 原料制备 13

2.2.1 Q235小钢片的制备 13

2.2.2 海水溶液的制备 13

2.2.3常见缓蚀剂的选择 14

2.3腐蚀失重实验 14

2.4复合型石墨烯基微胶囊的制备 15

2.5微胶囊的结构与性能表征 16

2.5.1 微胶囊的粒径测试 16

2.5.2微胶囊的形貌表征 16

2.5.3微胶囊的红外光谱分析 16

2.5.4微胶囊的拉曼光谱分析 16

2.5.5钨酸钠的存在表征 16

2.6微胶囊/环氧树脂复合涂层的性能测试 17

2.6.1复合涂层的制备 17

2.6.2复合涂层的EIS实验 17

2.6.3复合涂层的盐雾实验 18

第三章 实验结果与讨论 19

3.1缓蚀剂的筛选 19

3.2结构表征和成分分析 19

3.2.1微胶囊的粒径测试 19

3.2.2微胶囊的傅里叶红外光谱 20

3.2.3微胶囊的拉曼光谱 22

3.2.4微胶囊芯材钨酸钠的检测 22

3.2.5微胶囊SEM分析 23

3.3复合涂层的性能检测 24

3.3.1复合涂层的EIS实验 24

3.3.2 复合涂层的盐雾试验 26

第四章 结论与展望 28

参考文献 29

致谢 31

第一章 绪论

1.1 涂层防护技术简介

1.1.1 涂层防护机制

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