无患子果皮提取物的纳微米聚集体对钢的高效缓蚀

doi:10.11949/0438-1157.20200065

摘要/Abstract

摘要：

为寻求绿色、可持续与具备大规模应用潜能的天然植物提取物作为缓蚀剂，选择具有表面活性剂性质的无患子果皮提取物作为研究对象。通过简便乙醇回流萃取获得无患子果皮提取物。在室温条件下，无患子果皮提取物在DMF（N，N-二甲基甲酰胺）/HCl水溶液的混合溶液（体积比50/50，1.0 mol/L HCl 溶液）中能够发生自组装产生有序的纳微米聚集材料。傅里叶变换红外光谱（FT-IR）与X射线光电子能谱（XPS）研究表明了无患子果皮提取物聚集体能够对Q235钢表面产生化学吸附作用。利用电化学方法研究了无患子果皮提取物聚集体吸附在钢表面后，在1.0 mol/L盐酸水溶液中的缓蚀性能。结果表明无患子果皮提取物聚集体能够有效抑制钢被盐酸腐蚀，最大缓蚀效率达到90%以上。

关键词: 自聚集, 吸附, 钢, 盐酸溶液, 腐蚀

Abstract:

To seek green, sustainable and natural plant extracts with the potential for large-scale application as corrosion inhibitors, this article selects the extracts of the Sapindus mukorossi Gaertn peels with surfactant properties as the research object. Hence, this article uses Sapindus mukorossi Gaertn peel extracts (SMGPE) with surfactant properties as the study candidate. This survey presents efficient extraction of Sapindus mukorossi Gaertn peels by simply refluxing ethanol solution. It is shown that SMGPE can process orderly nano-micro meters aggregation in DMF/HCl (volume ratio: 50/50, 1.0 mol/L HCl solution) mixed solution through self-organization at the room temperature.The results show that the predominantly strong chemical adsorption of formed SMGPE aggregates on the studied Q235 steel specimens is suggested through the detection of FT-IR, Raman as well as XPS spectroscopy. This study further determines the corrosion inhibition effect of the stable SMGPE aggregates for the studied steel specimens in 1.0 mol/L HCl aqueous solution based on electrochemical method. The results suggest that the SMGPE aggregates can inhibit corrosion of the steel specimens in HCl solution efficiently, and the greatest corrosion inhibition efficiency is over 90%.

Key words: self-aggregation, adsorption, steel, HCl solution, corrosion

中图分类号:

TG 178

罗雪, 黄海军, 罗自萍, 王治永, 穆小静, 李红茹, 王新潮, 张胜涛, 高放. 无患子果皮提取物的纳微米聚集体对钢的高效缓蚀[J]. 化工学报, 2020, 71(10): 4760-4772.

Xue LUO, Haijun HUANG, Ziping LUO, Zhiyong WANG, Xiaojing MU, Hongru LI, Xinchao WANG, Shengtao ZHANG, Fang GAO. High efficient corrosion inhibition of steel by nano-micro aggregates of Sapindus mukorossi Gaertn peel extracts[J]. CIESC Journal, 2020, 71(10): 4760-4772.

图/表 20

图1 无患子果皮提取物（SMGPE）中主要化学成分的结构式

Fig.1 Chemical structures of the main molecular constituents in Sapindus mukorossi Gaertn peel extract (SMGPE)

图2 无患子果皮提取物（SMGPE）形成聚集体并在钢表面有效吸附的示意图

Fig.2 Diagrammatic drawing of the formation of SMGPE aggregates and the preparation of the stable SMGPE aggregates protection film on the studied steel specimen surface

图3 空白钢电极和吸附了不同浓度稳定SMGPE聚集体（聚集时间10 h）的钢电极在1 mol/L HCl溶液中的开路电位 (OCP)曲线

Fig.3 OCP versus time curves in 1.0 mol/L HCl solutions for the investigated unmodified steel electrodes and the stable SMGPE aggregates of different concentrations covered steel electrodes

图4 SMGPE聚集体在浓度为0.5 g/L时，在DMF/HCl（体积比50/50，1.0 mol/L HCl 溶液）混合溶液中聚集一定时间后的扫描电镜图

Fig.4 SEM images of SMGPE aggregates in DMF/HCl (vol ratio 50/50，1.0 mol/L HCl solution) mixed solution at different aggregation time

图5 SMGPE在不同浓度时，在DMF/HCl（体积比50/50，1.0 mol/L HCl 溶液）混合溶液中聚集10 h的扫描电镜图

Fig.5 SEM images of SMGPE aggregates in DMF/HCl (vol ratio 50/50，1.0 mol/L HCl solution) mixed solution with different concentrations from 0.1 to 0.6 g/L at 10 h evolution time

图6 SMGPE固体粉末的红外谱图(a)；稳定SMGPE聚集体 (聚集浓度 0.5 g/L, 聚集时间 10 h) 吸附于钢表面的全反射红外谱图(b)

Fig.6 FT-IR spectrum of original SME powder (a)； FT-IR spectrum of the stable SMGPE aggregates (aggregation concentration 0.5 g/L, aggregation time 10 h）adsorbed on the studied steel specimen surfaces (b)

图7 空白钢片在HCl水溶液中浸泡1 h，钢片表面的Fe 2p XPS能级谱图(a)；吸附稳定SMGPE聚集体 (聚集浓度 0.5 g/L, 聚集时间 10 h) 的钢片在HCl水溶液中浸泡1 h后金属表面的Fe 2p XPS能级谱图(b)

Fig.7 Fe 2p XPS spectra from the surfaces of the investigated bare steel immersed in HCl solution for 1 h (a)； Fe 2p XPS spectra from the studied steel specimens treated by the stable SMGPE aggregates (aggregation concentration 0.5 g/L, aggregation time 10 h) immersed in HCl solution for 1 h (b)

Table 1 De-convolution parameters including chemical states, binding energies and FWHMs of Fe 2p XPS spectra peaks obtained from the surfaces of the studied bare steel, the surveyed steel specimens treated by the stable SMGPE aggregates (aggregation concentration 0.5 g/L, aggregation time 10 h) immersed in 1.0 mol/LHCl solution

样品	化学状态	结合能/eV	半峰宽/eV
空白钢片	Fe₂O₃/Fe₃O₄/FeOOH	710.38	3.45
空白钢片	FeCl₃	712.47	3.5
吸附稳定SMGPE聚集体的钢片	Fe⁰	707.31	1.75
	Fe₂O₃/ Fe₃O₄	709.10	2.00
	FeOOH	710.90	2.00

图8 空白钢片在HCl水溶液（1.0 mol/L）浸泡1 h后，钢片表面的C 1s XPS图谱(a); 吸附稳定SMGPE聚集体 (聚集浓度 0.5 g/L, 聚集时间 10 h) 钢片在HCl水溶液（1.0 mol/L）浸泡1 h后钢片表面的C 1s XPS谱图 (b)表2 在HCl水溶液（1.0 mol/L）浸泡1 h后，空白钢片表面与吸附了稳定SMGPE聚集体的钢片 (聚集浓度 0.5 g/L, 聚集时间 10 h) 表面的C 1s能级分析的化学结构状态、结合能和半峰宽

Fig.8 C 1s XPS spectra from surfaces of the investigated bare steel immersed in HCl solution (1.0 mol/L HCl) for 1 h (a); C 1s XPS spectra from surfaces of the studied steel specimens treated by stable SMGPE aggregates (aggregation concentration 0.5 g/L, aggregation time 10 h) immersed in 1.0 mol/L HCl solution for 1 h (b)

Table 2 De-convolution parameters including chemical states, binding energies and FWHMs of C 1s XPS spectra peaks obtained from surfaces of the studied bare steel specimen and the studied steel specimens treated by the stable SMGPE aggregates (aggregation concentration 0.5 g/L, aggregation time 10 h) immersed in 1.0 mol/L HCl solution for 1 h

样品	化学状态	结合能/eV	半峰宽/eV
空白钢片	C—C/CC	284.90	1.62
	C—O	285.79	1.55
	CO	288.43	2.00
吸附稳定SMGPE聚集体的钢片	C—C/CC	284.98	2.06
	C—O	287.03	1.90
	CO	288.68	2.30

图9 未吸附和吸附了稳定SMGPE聚集体 (聚集浓度 0.5 g/L, 聚集时间 10 h) 的钢片在1.0 mol/L盐酸溶液中浸泡1 h后，钢片表面的O 1s XPS谱图

Fig.9 O 1s XPS spectra from surfaces of the investigated bare steel immersed in 1.0 mol/L HCl solution for 3 h; O 1s XPS spectra from surfaces of the studied steel specimens treated by stable SMGPE aggregates (aggregation concentration 0.5 g/L, aggregation time 10 h) immersed in HCl solution for 1 h

表3 空白钢片和吸附了SMGPE聚集体的钢片 (聚集浓度 0.5 g/L, 聚集时间 10 h) 在1.0 mol/L盐酸溶液中浸泡1 h后的O 1s能级分析的化学结构状态、结合能和半峰宽

Table 3 De-convolution parameters including chemical states, binding energies and FWHMs of O 1s XPS spectra peaks obtained from surfaces of the studied bare steel specimen and the studied steel specimens treated by stable SMGPE aggregates immersed in 1.0 mol/L HCl solution for 1 h (aggregation concentration, 0.5 g/L, aggregation time, 10 h)

样品	化学状态	结合能/eV	半峰宽/eV
空白钢片	Fe₂O₃/ Fe₃O₄	530.92	2.00
空白钢片	FeOOH	531.61	1.80
吸附稳定SMGPE聚集体的钢片	Fe₂O₃/ Fe₃O₄	530.24	1.90
	FeOOH	531.55	1.75
	CO/C—O	533.41	1.60

图10 钢表面的扫描电子显微镜图

Fig.10 SEM micrographs of the studied steel specimen surfaces

图11 空白钢电极和吸附了不同浓度稳定SMGPE聚集体（聚集时间10 h）的钢电极在1 mol/L HCl溶液中的动电位极化曲线

Fig.11 Potentiodynamic polarization curves in 1 mol/L HCl solutions for the investigated unmodified steel electrodes and the stable SMGPE aggregates of different concentrations (aggregation time 10 h) covered steel electrodes

表4 空白钢电极和吸附了不同浓度稳定SMGPE聚集体（聚集时间10 h）的钢电极在1 mol/L HCl溶液中的动电位极化曲线参数

Table 4 Polarization parameters for the studied unmodified and modified steel specimens by different concentrations of stable SMGPE aggregates (aggregation time 10 h) in 1.0 mol/L HCl solution

电极	极化参数
电极	C/(g/L)	E_corr (vs. SCE) /V	I_corr/(A/cm²)	β_c/(V/dec)	β_a/(V/dec)	η_j/%
空白钢电极	—	-0.480	4.387×10^-7	-0.1278	0.1068	—
稳定SMGPE聚集体吸附的钢电极	0.1	-0.447	1.004×10^-7	-0.1146	0.0585	77.11
	0.2	-0.442	4.957×10^-8	-0.1175	0.0508	88.7
	0.3	-0.437	4.549×10^-8	-0.1233	0.0515	89.63
	0.5	-0.430	2.820×10^-8	-0.1226	0.0424	93.57
	0.6	-0.440	3.767×10^-4	-0.1212	0.0524	91.41

图12 空白钢电极和吸附了不同浓度的稳定SMGPE聚集体（聚集时间10 h）的钢电极在1.0 mol/L HCl溶液中的Nyquist图(a); 空白钢电极(b)和吸附了不同浓度SMGPE聚集体的钢电极(c)在1.0 mol/L HCl溶液中的Bode图

Fig.12 Nyquist curves for the studied naked steel electrodes and SMGPE aggregates (aggregation time 10 h) of various concentrations covered steel electrodes(a)； Bode plots for the studied naked steel electrodes (b) and SMGPE aggregates (aggregation time 10 h) of various concentrations covered steel electrodes (c)

图13 本研究中在1 mol/L HCl溶液中拟合EIS实验数据的等效电路图

Fig.13 Equivalent circuit models fitting the EIS experimental data in this study

表5 空白钢电极和吸附了不同浓度稳定SMGPE聚集体（聚集时间10 h）的钢电极在1.0 mol/L HCl溶液中的交流阻抗参数

Table 5 Electrochemical impedance parameters for the studied unmodified and different concentrations of stable SMGPE aggregates (aggregation time 10 h) modified steel specimens in 1.0 mol/L HCl solution

电极	C/ (g/L)	电化学参数					χ²
电极	C/ (g/L)	R_s/ (Ω·cm²)	R_ct/ (Ω·cm²)	C_dl/ (F/cm²)	n	η_E/%	χ²
空白钢电极	—	0.6096	44.36	1.408×10^-7	0.9551	—	4.81×10³
SMGPE聚集体吸附的钢电极	0.1	0.8946	182.0	6.34×10^-8	0.8832	75.63	2.41×10³
	0.2	0.9725	315.4	5.48×10^-8	0.8829	85.94	1.52×10³
	0.3	0.9667	451.2	4.49×10^-8	0.8707	90.17	4.65×10³
	0.5	0.8991	635.0	3.98×10^-8	0.8928	93.01	1.95×10³
	0.6	1.2320	484.4	4.46×10^-8	0.8867	90.92	7.48×10³

图14 在298 K下，吸附了不同浓度稳定SMGPE聚集体的钢在1.0 mol/L HCl溶液中的Langmuir吸附等温线

Fig.14 Langmuir adsorption isotherm of stable SMGPE aggregates on the studied steel specimen surfaces in 1.0 mol/L HCl solution at 298 K (yP to Tafel curves, yE to electrochemical impedance spectroscopy)

表6 在298 K下，稳定SMGPE聚集体对钢的吸附热力学参数

Table 6 Thermodynamic parameters for the adsorption of SMGPE aggregates at 298 K

测试方法	吸附能 $Δ G a d s 0$ /(J/mol)
Polarization	-26790
EIS	-26430

表6 在298 K下，稳定SMGPE聚集体对钢的吸附热力学参数

Table 6 Thermodynamic parameters for the adsorption of SMGPE aggregates at 298 K

测试方法	吸附能 $Δ G a d s 0$ /(J/mol)
Polarization	-26790
EIS	-26430

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