含氮杂环类化合物及其自组装膜对铜在海水中缓蚀机理的研究
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摘要
缓蚀剂在金属防腐蚀保护工作中占有重要的地位，在国民经济建设中发挥着越来越重要的作用。从目前热力设备防腐、石油开采及其他领域防腐情况来看，缓蚀剂的使用是阻止或延缓金属发生锈蚀一种行之有效、经济效益显著的技术手段。虽然目前缓蚀剂从分子设计、合成路线与工艺、复配协同性、应用性能等方面都取得了较大的发展，但是其理论进展仍远滞后于实践，对于不少缓蚀剂的缓蚀机理尚存争议，因此运用各种方法、手段研究缓蚀剂的缓蚀机理，发展和完善缓蚀剂理论，成为目前缓蚀剂研究领域的热门课题。
本文筛选、合成了两大类共6种新型含氮杂环化合物作为缓蚀剂，运用失重实验、电化学实验、量子化学计算、分子动力学模拟及扫描电镜等实验多种手段和方法测试了所选化合物在海水溶液中对铜的缓蚀性能，分析了它们对铜的缓蚀机理，从理论上探讨了缓蚀剂分子与金属表面的作用方式，归纳总结了分子结构、腐蚀粒子与缓蚀剂吸附膜相互作用与缓蚀效果之间的关系。为了拓展缓蚀剂的应用范围，利用缓蚀剂的吸附成膜特性，将缓蚀剂作为成膜分子，开发自组装体系，将缓蚀剂分子自组装到铜基材的表面，形成一层牢固、致密、排列有序的自组装膜，并通过电化学方法、原子力显微镜、拉曼光谱以及接触角测定仪对自组装膜的疏水性能及防蚀性能进行表征。
本文中涉及的两类新型杂环化合物为：噻二唑类化合物和三氮唑类化合物，研究的主要结果如下：
失重、电化学及扫描电镜实验结果表明，噻二唑类化合物和三氮唑类化合物对铜有较好的缓蚀效果和较高的缓蚀效率。实验结果表明三氮唑化合物和噻二唑化合物在100mg/L时对铜的缓蚀效率达到95%以上。结合实验现象及量子化学计算结果，推断了其吸附特点，证明噻二唑类缓蚀剂与三氮唑类缓蚀剂均符合Langmuir吸附等温模型，缓蚀剂分子的吸附机理为物理吸附和化学吸附共同作用，且化学吸附占主导。
通过分子动力学模拟三种腐蚀性粒子在缓蚀剂吸附膜间的扩散迁移作用研究缓蚀剂的缓蚀机理发现，自由体积、腐蚀性粒子与缓蚀剂分子的相互作用以及缓蚀剂分子的自扩散系数是影响离子扩散的主要因素；同种缓蚀剂膜对正负离子（H_3O~+、Cl~-）的迁移比对H_2O分子具有更强的抑制能力。
将铜基材表面用合成的2-巯基-5-苯基-1,3,4-噻二唑(MPT)、2-巯基-5-苯甲基-1,2,4-三氮唑(MBT)进行修饰，考察了组装时间，化合物浓度，超声波振荡、取代基官能团亲水性对修饰后铜的抗腐蚀性能的影响。在此基础上，研究了MPT和MBT在铜表面的成膜机理。结果表明，MPT和MBT在铜表面形成针状和球状自组装膜，使铜表面的接触角由72°上升到100°左右，达到了疏水性的要求。通过电化学测试发现，当成膜分子浓度大于3×10~(-3)M或组装时间大于2h，自组装膜将变得更加致密，粒子在缓蚀剂吸附膜间的相互扩散迁移效应逐渐消失；在组装过程中外加超声波能够在保持自组装膜足够的缓蚀性能的前提下，大大缩短组装时间。
为了提高自组装膜层的质量和稳定性，将硅烷偶联剂与MPT、MBT对铜进行复合成膜。利用电化学阻抗谱和极化曲线研究了丙基三甲氧基硅烷（PTMS）的水解溶剂，水解时间，溶液浓度，水解pH等对硅烷膜的防蚀性能，并将PTMS分别与MPT、MBT在铜表面形成复合组装膜，实验结果表明，PTMS在铜表面可能形成了三维网状结构，氮杂环化合物添加在其中，使复合组装膜的致密性提高，质量更稳定，可以起到优异的抑制腐蚀进程的作用。
Corrosion inhibitors hold the important status in the metal protection project, and they are playing more and more important role in the national economy construction. According to the present anti-corrosion of thermal energy equipments and anti-corrosion situation in other industry domain, it is an effective and economic method to use corrosion inhibitor. So, it becomes an interesting subject for chemists to study the corrosion inhibiting mechanism and develop or perfect the theory through various means and techniques.
In this paper, two series including six kinds of newly heterocyclic compounds were synthesized to be studied as corrosion inhibitors of copper in seawater using weight loss experiment, electrochemical test, scanning electron micrographs (SEM), quantum chemical calculations and molecular dynamics. And then, we studied their corrosion inhibiting mechanism on copper, discussed theoretically the function way between the corrosion inhibitors and the metal surface and summarized the relationship between the molecular structure and their inhibiting efficiency. In order to extend the usage of inhibitor, the compounds employed to assemble on the copper, forming a solid, dense self-assembled film. Then the anticorrosion property and hydrophobic were detected. The results were drawn as follows:
The triazole derivatives and thiadazole derivatives were proved to have positive inhibiting effect through weight loss experiment, electrochemical test and scanning electron micrographs. According to the experiments, the inhibit effective were more than90%when the concentration was100mg/L. Thermodynamic calculation suggests that the adsorption of the inhibitors was found to follow the Langmuir adsorption isotherm, and the adsorption of the inhibitors on copper surface involve physical as well as chemical adsorption.
Free volume, interaction between particles and membrane, and self-diffusion performance of inhibitors are the three critical factors influencing the performance for prevention of corrosion particles diffusion by inhibitor membrane. Identical inhibitor membrane has more prevention ability for cations and anions (H3O+and Cl-) than that for H2O molecules.
The MPT and MBT synthesized were assembled onto copper surface, and the effects of immersing time, concentration of inhibitors, ultrasonic irradiation and hydrophilic of the function groups are studied. The SEM shown that the morphology of the film is needle-like and globular, the contact angle is increased from72°to100°. The electrochemical tests shown that the layer become more solid after2hours treating or the concentration more than3×10-3M. Employing ultrasonic could reach the same inhibit effective in less treating time.
In order to improve the quality of the self-assembled film, PTMS silane hybrid film was successfully prepared. Using electrochemical methods studied the inhibitive effect of PTMS film with different hydrolysis solvent, hydrolysis time, solution concentration and pH value. The results shown that the PTMS form a three-dimensional structure on copper surface, and then we got a density hybrid film with MPT and MBT, which can inhibit the corrosion process and improve the adsorption of the film.
本文筛选、合成了两大类共6种新型含氮杂环化合物作为缓蚀剂，运用失重实验、电化学实验、量子化学计算、分子动力学模拟及扫描电镜等实验多种手段和方法测试了所选化合物在海水溶液中对铜的缓蚀性能，分析了它们对铜的缓蚀机理，从理论上探讨了缓蚀剂分子与金属表面的作用方式，归纳总结了分子结构、腐蚀粒子与缓蚀剂吸附膜相互作用与缓蚀效果之间的关系。为了拓展缓蚀剂的应用范围，利用缓蚀剂的吸附成膜特性，将缓蚀剂作为成膜分子，开发自组装体系，将缓蚀剂分子自组装到铜基材的表面，形成一层牢固、致密、排列有序的自组装膜，并通过电化学方法、原子力显微镜、拉曼光谱以及接触角测定仪对自组装膜的疏水性能及防蚀性能进行表征。
本文中涉及的两类新型杂环化合物为：噻二唑类化合物和三氮唑类化合物，研究的主要结果如下：
失重、电化学及扫描电镜实验结果表明，噻二唑类化合物和三氮唑类化合物对铜有较好的缓蚀效果和较高的缓蚀效率。实验结果表明三氮唑化合物和噻二唑化合物在100mg/L时对铜的缓蚀效率达到95%以上。结合实验现象及量子化学计算结果，推断了其吸附特点，证明噻二唑类缓蚀剂与三氮唑类缓蚀剂均符合Langmuir吸附等温模型，缓蚀剂分子的吸附机理为物理吸附和化学吸附共同作用，且化学吸附占主导。
通过分子动力学模拟三种腐蚀性粒子在缓蚀剂吸附膜间的扩散迁移作用研究缓蚀剂的缓蚀机理发现，自由体积、腐蚀性粒子与缓蚀剂分子的相互作用以及缓蚀剂分子的自扩散系数是影响离子扩散的主要因素；同种缓蚀剂膜对正负离子（H_3O~+、Cl~-）的迁移比对H_2O分子具有更强的抑制能力。
将铜基材表面用合成的2-巯基-5-苯基-1,3,4-噻二唑(MPT)、2-巯基-5-苯甲基-1,2,4-三氮唑(MBT)进行修饰，考察了组装时间，化合物浓度，超声波振荡、取代基官能团亲水性对修饰后铜的抗腐蚀性能的影响。在此基础上，研究了MPT和MBT在铜表面的成膜机理。结果表明，MPT和MBT在铜表面形成针状和球状自组装膜，使铜表面的接触角由72°上升到100°左右，达到了疏水性的要求。通过电化学测试发现，当成膜分子浓度大于3×10~(-3)M或组装时间大于2h，自组装膜将变得更加致密，粒子在缓蚀剂吸附膜间的相互扩散迁移效应逐渐消失；在组装过程中外加超声波能够在保持自组装膜足够的缓蚀性能的前提下，大大缩短组装时间。
为了提高自组装膜层的质量和稳定性，将硅烷偶联剂与MPT、MBT对铜进行复合成膜。利用电化学阻抗谱和极化曲线研究了丙基三甲氧基硅烷（PTMS）的水解溶剂，水解时间，溶液浓度，水解pH等对硅烷膜的防蚀性能，并将PTMS分别与MPT、MBT在铜表面形成复合组装膜，实验结果表明，PTMS在铜表面可能形成了三维网状结构，氮杂环化合物添加在其中，使复合组装膜的致密性提高，质量更稳定，可以起到优异的抑制腐蚀进程的作用。
Corrosion inhibitors hold the important status in the metal protection project, and they are playing more and more important role in the national economy construction. According to the present anti-corrosion of thermal energy equipments and anti-corrosion situation in other industry domain, it is an effective and economic method to use corrosion inhibitor. So, it becomes an interesting subject for chemists to study the corrosion inhibiting mechanism and develop or perfect the theory through various means and techniques.
In this paper, two series including six kinds of newly heterocyclic compounds were synthesized to be studied as corrosion inhibitors of copper in seawater using weight loss experiment, electrochemical test, scanning electron micrographs (SEM), quantum chemical calculations and molecular dynamics. And then, we studied their corrosion inhibiting mechanism on copper, discussed theoretically the function way between the corrosion inhibitors and the metal surface and summarized the relationship between the molecular structure and their inhibiting efficiency. In order to extend the usage of inhibitor, the compounds employed to assemble on the copper, forming a solid, dense self-assembled film. Then the anticorrosion property and hydrophobic were detected. The results were drawn as follows:
The triazole derivatives and thiadazole derivatives were proved to have positive inhibiting effect through weight loss experiment, electrochemical test and scanning electron micrographs. According to the experiments, the inhibit effective were more than90%when the concentration was100mg/L. Thermodynamic calculation suggests that the adsorption of the inhibitors was found to follow the Langmuir adsorption isotherm, and the adsorption of the inhibitors on copper surface involve physical as well as chemical adsorption.
Free volume, interaction between particles and membrane, and self-diffusion performance of inhibitors are the three critical factors influencing the performance for prevention of corrosion particles diffusion by inhibitor membrane. Identical inhibitor membrane has more prevention ability for cations and anions (H3O+and Cl-) than that for H2O molecules.
The MPT and MBT synthesized were assembled onto copper surface, and the effects of immersing time, concentration of inhibitors, ultrasonic irradiation and hydrophilic of the function groups are studied. The SEM shown that the morphology of the film is needle-like and globular, the contact angle is increased from72°to100°. The electrochemical tests shown that the layer become more solid after2hours treating or the concentration more than3×10-3M. Employing ultrasonic could reach the same inhibit effective in less treating time.
In order to improve the quality of the self-assembled film, PTMS silane hybrid film was successfully prepared. Using electrochemical methods studied the inhibitive effect of PTMS film with different hydrolysis solvent, hydrolysis time, solution concentration and pH value. The results shown that the PTMS form a three-dimensional structure on copper surface, and then we got a density hybrid film with MPT and MBT, which can inhibit the corrosion process and improve the adsorption of the film.
引文
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