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中国腐蚀与防护学报, 2022, 42(5): 791-797 DOI: 10.11902/1005.4537.2021.218

研究报告

卤素阴离子对离子液体缓蚀性能的影响

冯丽,1,2, 张胜涛3, 郑思远1, 胡志勇1, 朱海林1, 马雪梅1

1.中北大学化学工程与技术学院 太原 030051

2.中北大学德州研究生分院 德州 253034

3.重庆大学化学化工学院 重庆 401331

Effect of Halogen Anions on Corrosion Inhibition of Ionic Liquids

FENG Li,1,2, ZHANG Shengtao3, ZHENG Siyuan1, HU Zhiyong1, ZHU Hailin1, MA Xuemei1

1.School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, China

2.Dezhou Graduate School, North University of China, Dezhou 253034, China

3.School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 401331, China

通讯作者: 冯丽,E-mail：20200164@nuc.edu.cn,研究方向为金属的腐蚀防护

收稿日期: 2021-08-30   修回日期: 2021-09-17  

基金资助: 国家自然科学基金.  201878029

Corresponding authors: FENG Li, E-mail:20200164@nuc.edu.cn

Received: 2021-08-30   Revised: 2021-09-17  

Fund supported: National Natural Science Foundation of China.  201878029

作者简介 About authors

冯丽,女,1992年生,博士

摘要

通过电化学阻抗谱、极化曲线、扫描电镜和原子力显微镜等测试对比了不同卤素阴离子的咪唑基离子液体对X70钢在0.5 mol/L H2SO4溶液中的缓蚀性能。结果表明,它们都属于混合型缓蚀剂,均可以有效地抑制X70钢的腐蚀；且随着缓蚀剂浓度的增大,缓蚀效率逐渐增大；在浓度为5 mmol/L时,缓蚀效率达到最大。1-乙烯基-3-丁基咪唑碘盐 ([VBIM]I) 的缓蚀效率最高,其次为1-乙烯基-3-丁基咪唑氯盐 ([VBIM]Cl),而1-乙烯基-3-丁基咪唑溴盐 ([VBIM]Br) 的最低,这主要归因于I-的特异性吸附。所研究离子液体缓蚀剂的阴离子和阳离子之间存在协同缓蚀作用,即离子液体的阴离子和阳离子都参与了对金属的缓蚀。

关键词： 缓蚀剂 ; 离子液体 ; 硫酸 ; 电化学 ; X70钢 ; 形貌分析

Abstract

The corrosion inhibition performance of imidazolidyl ionic liquids with different halogen anions (such as 1-vinyl-3-butyl-imidazolium chloride salt, [VBIM]Cl, 1-vinyl-3-butylimidazolium bromide, [VBIM]Br, and 1-vinyl-3-butylimidazolium iodide, [VBIM]I) on X70 steel in 0.5 mol/L H2SO4 solution was comparatively assessed by electrochemical impedance spectroscopy, polarization curve measurement, scanning electron microscopy and atomic force microscopy. The results indicated that they were all the mixed corrosion inhibitor and could effectively inhibit the corrosion of X70 steel in 0.5 mol/L H2SO4 solution. With the increase of the concentration of corrosion inhibitors, the corrosion inhibition efficiency increases gradually. And the inhibition efficiency reached the maximum by the concentration of 5 mmol/L. The corrosion inhibition efficiency of the inhibitors may be ranked as the follows: [VBIM]I is higher than [VBIM]Cl and [VBIM]Br in turn, which is mainly due to the specific adsorption of I-. The inhibition mechanism may be described as that there is a synergistic inhibition effect between the cation and anion of the studied ionic liquid corrosion inhibitors. In other words, both the anions and cations of ionic liquid can participate in the corrosion inhibition process of metal.

Keywords： corrosion inhibitor ; Ionic liquid ; sulfuric acid ; electrochemistry ; X70 steel ; morphology analysis

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本文引用格式

冯丽, 张胜涛, 郑思远, 胡志勇, 朱海林, 马雪梅. 卤素阴离子对离子液体缓蚀性能的影响. 中国腐蚀与防护学报[J], 2022, 42(5): 791-797 DOI:10.11902/1005.4537.2021.218

FENG Li, ZHANG Shengtao, ZHENG Siyuan, HU Zhiyong, ZHU Hailin, MA Xuemei. Effect of Halogen Anions on Corrosion Inhibition of Ionic Liquids. Journal of Chinese Society for Corrosion and Protection[J], 2022, 42(5): 791-797 DOI:10.11902/1005.4537.2021.218

X70钢具有高强度、高冲击韧性、抗氢致开裂等优良性能,被广泛应用于石油、天然气等管道运输领域[1-3]。然而,它的腐蚀会造成巨大的经济和能源损失,甚至还会引发燃烧、爆炸等严重危害人民生命及财产安全的重大事故。基于金属及其合金器件很容易被氧化,其在使用之前通常都要经过酸洗工艺处理来除去表面氧化产物等污渍,进而来延长其使用期限,提高经济效益,并且有效地消除安全隐患。值得注意的是,在酸洗除锈、工艺设备酸洗及酸化采油等酸性环境中,酸溶液会对金属造成过度腐蚀,不仅给生产生活带来很多不便,而且会造成经济能源损失。因此,在酸洗过程中,常常通过添加缓蚀剂这种方法来减少或者消除对金属的过度腐蚀,进而来保护金属[4-7]。传统的高效缓蚀剂是含有N、O、S、P或共轭体系的有机物,其溶解性差、易挥发且毒性较大,对环境不友好,使其在工业应用中受到很大限制[8-13]。为满足绿色化工和生态文明建设的要求,加快酸洗环境中高效绿色缓蚀剂的开发势在必行,这对工业中酸洗工艺的提高和发展具有重大意义。

离子液体作为低温熔融盐,是完全由阴阳离子组成的化合物,可以通过改变阴离子和阳离子的组合,设计出不同的离子液体。其毒性低、溶解性好、不易挥发、稳定性好、生物相容性好,可作为潜在的绿色高效缓蚀剂[14,15]。目前,有研究证实了离子液体缓蚀剂阳离子的不同会对缓蚀效率产生显著影响[16,17]。Qiang等[1]表明咪唑溴盐离子液体对Cu在酸溶液中的腐蚀有显著的抑制作用,且取代基的链长对缓蚀效果有显著影响,这可能是由于不同的取代基其供电子效应和空间位阻效应不同造成的。Zaky等[18]合成了3种新型阳离子不同的咪唑离子液体,并表明阳离子不同的离子液体对钢的缓蚀作用是有差异的。以上这些研究都证实了阳离子不同会对缓蚀效率产生影响。然而,离子液体阴离子对缓蚀效果的影响研究较少,且其阴阳离子之间的相互作用机理尚不明确。

基于此,本文探究了含不同卤素阴离子 (I-,Cl-和Br-) 的咪唑基离子液体缓蚀剂在0.5 mol/L H2SO4溶液中对X70钢的腐蚀抑制效果以及缓蚀机制。该研究进一步加深了对咪唑基离子液体对X70钢缓蚀过程的理解,也为未来设计和开发绿色高效缓蚀剂提供了理论指导。

1 实验方法

实验使用的离子液体1-乙烯基-3-丁基咪唑氯盐 (1-vinyl-3butylimidazolium Chloride,[VBIM]Cl)、1-乙烯基-3-丁基咪唑溴盐 (1-vinyl-3butylimidazolium Bromide,[VBIM]Br) 和1-乙烯基-3-丁基咪唑碘盐 (1-vinyl-3butylimidazolium iodide,[VBIM]I),均购买自上海成捷化学公司,纯度为99 %,其结构如图1所示。实验所用的钢材其组成 (质量分数,%) 为：Mn 1.7,Si 0.45,S 0.01,P 0.02,V 0.06,Mo 0.35,Ti 0.06,Nb 0.05,余量为Fe。测试溶液为含有不同浓度离子液体缓蚀剂的0.5 mol/L H2SO4溶液,不含缓蚀剂的0.5 mol/L H2SO4溶液作为空白对照组。

图1

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图1   咪唑基离子液体缓蚀剂的化学结构

Fig.1   Chemical structures of imidazole-based ionic liquid inhibitors


电化学实验在CHI 604D电化学工作站上进行。采用三电极体系,工作电极是工作面积为1 cm2嵌入环氧树脂的X70钢,辅助电极为铂电极,参比电极为饱和甘汞电极。实验前,均用400#、600#、1500#、2000#和3000#砂纸依次打磨至镜面,再分别用蒸馏水和无水乙醇超声清洗30 s,室温干燥备用。测试前,依次进行开路电位测试、电化学阻抗谱测试和电动位极化曲线测试。其中开路测试时间为500 s,达到一个稳定的状态后,进行阻抗谱测试,测试的频率范围为105~10-2 Hz,激励信号为5 mV的正弦电压。最后进行动电位极化曲线测试,极化曲线的极化范围是基于开路电位的±250 mV,扫描速率为1 mV/s。其缓蚀效率计算为[19,20]：

η(%)=Rct-Rct,0Rct×100%
η(%)=Icorr-Icorr,0Icorr,0×100%

式中,Icorr,0和Rct,0及Icorr和Rct分别为空白硫酸溶液和添加了不同浓度离子液体缓蚀剂时的腐蚀电流密度和电荷转移电阻。

用扫描电子显微镜 (SEM,JEOL-JSM-7800F) 和原子力显微镜 (AFM,MFP-3D-BIO) 观察分析样品的表面形貌,样品尺寸分别为0.3 cm×0.5 cm×0.5 cm和1 cm×1 cm×0.1 cm。测试前,将打磨好的样品分别浸泡到不含和含离子液体缓蚀剂的0.5 mol/L H2SO4溶液中,4 h后取出样品并用蒸馏水清洗,冷风干燥后。以上所有实验均在室温 (25 ℃) 下进行,通过恒温水浴锅将温度控制在 (298±0.5) K。

2 结果与讨论

2.1 电化学阻抗谱分析

电化学阻抗谱通过ZSimpWin软件进行拟合,图2分别是拟合有感抗和没有感抗的阻抗数据采用的等效电路。图3为X70钢在空白和添加了不同浓度离子液体缓蚀剂的0.5 mol/L H2SO4溶液中的Nyquist图和Bode图,拟合参数表1。Rs为溶液电阻,Rct为电荷转移电阻,L为感抗,RL为感抗电阻,CPE为常相位角原件。CPE可用下式表示[21]：

图2

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图2   拟合含和不含感抗阻抗数据所用的等效电路

Fig.2   Equivalent circuits used to fit impedance data with (a) and without (b) inductive impedance


图3

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图3   X70钢电极在不同浓度[VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中的Nyquist和Bode图

Fig.3   Nyquist and Bode plots of X70 steel electrode in 0.5 mol/L H2SO4 solutions with different concentrations of [VBIM]Cl (a), [VBIM]Br (b) and [VBIM]I (c) at 298 K


ZCPE=1Y0(jω)n

式中,Y0为CPE的值,j为虚数,ω为角频率,n为弥散效应指数。n可反映工作电极表面的粗糙和不均一性,其值范围在-1~1之间,n值越接近1,则CPE越接近于纯电容[22]。Cdl的值可由下式计算[23]：

Cdl=Y0(ω)n-1=Y0(2πfZim-Max)

式中,fZim-Max对应的是阻抗虚部最大时的频率。

表1   X70钢电极在不同浓度[VBIM]Cl、[VBIM]Br和[VBI M]I的 0.5 mol/L H2SO4溶液中的电化学阻抗数据

Table 1  Electrochemical impedance data of X70 steel electrode in 0.5 mol/L H2SO4 solutions containing different concentrations of [VBIM]Cl, [VBIM]Br and [VBIM]I at 298 K

InhibitorC / mmol·L-1Rs / Ω·cm2Y0 / 10-5 Ω·cm2nCdl / μF·cm-2Rct / Ω·cm2L / Ω·cm2RL / Ω·cm2η / %
Blank00.9317.750.9098.523.7071.0181.0---
[VBIM]Cl0.11.1817.650.8994.529.30222.4152.019.1
0.51.2117.250.8694.354.53346.3460.456.5
11.4216.130.8587.075.16297.2395.468.5
21.0916.520.8383.181.24551.6495.170.8
51.3517.180.8080.9108.40961.5593.678.1
[VBIM]Br0.11.2217.610.8998.124.80144.1112.74.4
0.50.9316.940.9096.029.45284.8148.519.5
11.6714.710.8595.732.07105.9183.626.1
21.6813.810.9494.937.24588.0225.636.4
51.3712.440.8284.758.81176.2406.459.7
[VBIM]I0.10.7715.930.9090.849.40100.1347.052.0
0.50.7413.720.8879.8140.90155.5567.083.2
10.9010.060.8758.2285.60------90.8
20.677.330.8947.7402.20------94.1
51.025.510.9139.9669.10------96.5

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从Nyquist图中可以看出,Nyquist图是由高频区的容抗弧和低频区的感抗弧组成,高频区的容抗弧主要与电荷转移电阻和双电层电容有关,而低频区的感抗弧是由于吸附离子如 (H+)ads和 (SO42-)ads的弛豫过程引起的[24]。随着[VBIM]Cl浓度的增加,容抗弧的半径逐渐增大,这表明随缓蚀剂浓度的增大,其在电极表面的吸附增加,电荷转移电阻增大,X70钢在0.5 mol/L H2SO4溶液中的腐蚀得到了有效控制,且缓蚀效率随缓蚀剂浓度的增大而增强,并且[VBIM]I对X70钢的腐蚀抑制效果依次优于[VBIM]Cl和[VBIM]Br。在Bode图中,随着缓蚀剂浓度的增大,阻抗模值和相位角逐渐增大,也进一步说明离子液体缓蚀剂的加入有效地抑制了X70钢在0.5 mol/L H2SO4溶液中的腐蚀。

从表1的数据可以看出,随着缓蚀剂浓度的增大,电荷转移电阻 (Rct) 增大,双层电容值 (Cdl) 逐渐减小,缓蚀效率 (η) 逐渐增大。根据界面双电层的表达 式 (5)[19]：

Cdl=ε0εdS

其中,ε0为空气介电常数,ε为双电层的局部介电常数,S为工作电极面积,d为双电层的厚度。随着缓蚀剂浓度的增大,缓蚀剂逐渐取代了金属表面的水分子吸附到金属表面,且吸附厚度随浓度增大而增大。一般地,有机缓蚀剂的介电常数小于水分子的介电常数,也进一步说明,随着缓蚀剂浓度的增大,越来越多的缓蚀剂吸附到金属表面来抑制腐蚀性物质对X70钢的腐蚀。此外还可以得出,3种阴离子不同的离子液体缓蚀剂 ([VBIM]I、[VBIM]Br、[VBIM]Cl) 对X70在0.5 mol/L H2SO4中的缓蚀效率顺序为：[VBIM]I依次优于[VBIM]Cl和[VBIM]Br,这主要归因于I-优异的吸附特性。这一结果进一步揭示了所研究的3种离子液体缓蚀剂的阴阳离子之间存在协同缓蚀作用[25-27]。当阳离子相同时,阴离子为I-缓蚀剂的缓蚀效应要优于阴离子Cl-和Br-。

2.2 动电位极化曲线图

图4为X70钢分别在不同浓度[VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中的动电位极化曲线图。相应的极化数据根据Tafel直线外推法得到并列于表2中。在图4中,随着缓蚀剂浓度的增加,腐蚀电位向正方向移动,腐蚀电流密度逐渐降低,说明X70钢在0.5 mol/L H2SO4溶液中的腐蚀得到了有效的控制。电流密度的降低既体现在阳极支又体现在阴极支,说明所研究的缓蚀剂是混合型缓蚀剂[28,29]。同时可以看出,随着浓度的增加,极化曲线平行下降,线的形状并没有发生改变,表明浓度的增加并没有改变离子液体的缓蚀机理。在图4c阳极极化中,电流密度有一个骤升的拐点,这个点对应的电位为[VBIM]I缓蚀剂的脱附电位,即从脱附电位向正方向极化的过程中,缓蚀剂开始脱附,且极化过程中电流密度降低的越快,即缓蚀剂的脱附越快,腐蚀越严重。脱附电位越正,缓蚀剂越不容易脱附。而在图4a和b中,并没有观察到电流密度的骤升,说明在该极化范围下,缓蚀剂的脱附不是很严重。在离子化合物中,阴阳离子之间的作用力为库仑力,其大小与阴阳离子的电荷数量及半径有关,电荷数量相同时,离子半径越大,它们之间的作用力越小。I的半径依次大于Br和Cl,即I-与咪唑阳离子之间的作用力较Cl-和Br-更小,因此,在进行阳极极化时,[VBIM]I更容易发生脱附。此外,从表2中可以得出,添加不同浓度离子液体缓蚀剂后,其腐蚀电位相对空白的变化值均小于85 mV,进一步说明所研究的离子液体缓蚀剂均为混合型缓蚀剂[30,31]。相同体系中,[VBIM]I对X70钢的腐蚀抑制效果最好,而[VBIM]Br的最差。在酸溶液中,离子液体阴阳离子的协同作用阻碍了溶液中腐蚀性物质对金属的进攻,有效地保护X70钢免受腐蚀。极化曲线和电化学阻抗谱得出的结论是一致的。

图4

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图4   X70钢电极在含不同浓度[VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中的极化曲线图

Fig.4   Polarization curves of X70 steel electrode in 0.5 mol/L H2SO4 solutions with different concentrations of [VBIM]Cl (a), [VBIM]Br (b) and [VBIM]I (c) at 298 K


表2   X70钢电极在含不同浓度[VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中的极化曲线参数

Table 2  Polarization curve parameters of X70 steel electrode in 0.5 mol/L H2SO4 solutions with different concentrations of [VBIM]Cl, [VBIM]Br and [VBIM]I at 298 K

InhibitorC / mmol·L-1Ecorr SCE / VIcorr / mA·cm-2-βc / mV·dec-1βa / mV·dec-1η / %
Blank0-0.4771.840168.4101.6---
[VBIM]Cl0.1-0.4681.463167.0108.020.5
0.5-0.4610.588156.487.668.0
1-0.4660.374146.183.479.7
2-0.4610.363152.577.180.3
5-0.4630.286151.976.884.5
[VBIM]Br0.10.4681.738166.9114.15.5
0.5-0.4691.415164.998.423.1
1-0.4701.332167.2104.727.6
2-0.4701.227173.2114.633.3
5-0.4710.579153.992.168.5
[VBIM]I0.1-0.4780.747145.091.959.4
0.5-0.4530.249134.9102.886.5
1-0.4330.086130.2105.495.4
2-0.4260.027131.248.997.9
5-0.3990.010140.537.499.4

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2.3 SEM分析

图5为X70钢分别含和不含5 mmol/L [VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中浸泡4 h后的SEM形貌。可以看出,经过腐蚀溶液浸泡后,样品的表面均遭到不同程度的破环,空白样品的腐蚀最为严重,腐蚀痕迹更加明显。相较于空白,添加了缓蚀剂的样品,其表面状态有了明显的改善。对比高倍率下的3种缓蚀剂对应的SEM图发现,[VBIM]I比[VBIM]Cl和[VBIM]Br样品表面更加光滑平整,说明[VBIM]I的缓蚀效率比[VBIM]Cl和[VBIM]Br更好,这与电化学实验结果相吻合。

图5

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图5   X70钢电极在不含和含有 5 mmol/L [VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中浸泡4 h后的SEM形貌

Fig.5   SEM images of X70 steel electrode immersed for 4 h at 298 K in 0.5 mol/L H2SO4 solutions without (a) and with 5 mmol/L [VBIM]Cl (b), [VBIM]Br (c) and [VBIM]I (d)


2.4 AFM分析

图6为X70钢分别浸泡在含有和不含有离子液体的0.5 mol/L H2SO4溶液中4 h后的AFM 3D形貌,可以看出,空白样品表面很粗糙,有很多腐蚀坑,表面高度变化范围很大,说明其在0.5 mol/L H2SO4溶液中遭受了严重的腐蚀,致使表面变得粗糙。加了缓蚀剂以后,样品表面的腐蚀痕迹明显减弱了很多,3D图变得光滑平整,表面粗糙度明显下降,由空白的89.970 nm降低到61.034 nm ([VBIM]Br)、37.244 nm ([VBIM]Cl) 和35.250 nm ([VBIM]I),说明缓蚀剂的加入有效地抑制了X70钢的腐蚀。且粗糙度更小的[VBIM]I比[VBIM]Cl和[VBIM]Br具有更优异的腐蚀抑制效果,这与电化学得到的结果是一致的。

图6

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图6   X70钢电极在不含和含有5 mmol/L [VBIM]Cl、[VBIM]Br和[VBIM]I的0.5 mol/L H2SO4溶液中浸泡4 h后的AFM形貌

Fig.6   AFM and corresponding height images of X70 steel electrode immersed for 4 h at 298 K in 0.5 mol/L H2SO4 solutions without (a) and with 5 mmol/L [VBIM]Cl (b), [VBIM]Br (c) and [VBIM]I (d)


2.5 缓蚀机理分析

离子液体的缓蚀机理如图7所示。在0.5 mol/L H2SO4溶液中,X70钢表面带正电荷,当溶液中含有咪唑基离子液体时,卤素阴离子会通过静电作用优先吸附到X70钢表面,然后咪唑基阳离子会进一步吸附,卤素离子的“架桥”作用使得咪唑基阳离子更容易吸附。阴阳离子在金属表面有序吸附形成稳定致密的吸附保护膜,阻碍了溶液中腐蚀性物质 (如水分子和氢离子等) 对X70钢的腐蚀进攻,达到了有效的腐蚀抑制作用。阳离子相同时,I-的特异性吸附使得[VBIM]I具有较[VBIM]Cl和[VBIM]Br更优的缓蚀效果[25]。3种阴离子相比,Cl原子的半径依次小于Br和I,理论上Cl原子电性要依次大于Br和I,即Cl-更容易在带正电荷的X70表面发生吸附。然而,实验结果表明阴离子为I-时的缓蚀效率要依次大于Cl-和Br-。这主要是由于I-的半径和体积较大,原子核对外层电子的束缚能力弱,使得的I-的可极化性和变形性更强,表现出特异的吸附能力。进而使得阴离子为I-的离子液体表现出比Cl-和Br-更优的缓蚀效率。这一结论对未来离子液体缓蚀剂设计和开发具有一定的理论指导意义。

图7

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图7   离子液体缓蚀机理示意图

Fig.7   Schematic diagram of corrosion inhibition mechanism of ionic liquid inhibitors


3 结论

(1) 在0.5 mol/L的H2SO4溶液中,[VBIM]X (X=Cl、Br、I) 可以有效的抑制X70钢的腐蚀,且均属于混合型缓蚀剂,且都存在阴离子和阳离子的协同作用。

(2) 3种缓蚀剂的缓蚀效率随浓度的增大而增大,在浓度为5 mmol/L时,缓蚀效率皆达到最大。

(3) 当阳离子相同时,阴离子为I-的离子液体的缓蚀效率最高,其次为阴离子为Cl-的,而阴离子为Br-的缓蚀效率最低,这主要与I-的特异性吸附有关。

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