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Graphene oxide modified with imidazoline quaternary ammonium salt: Water-soluble inhibitor for anticorrosion of the corrosion of carbon steel in oilfield wastewater
*Corresponding author: Email address: 254798591@qq.com (C. Xiaodong)
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Received: ,
Accepted: ,
Abstract
Graphene oxide (GO) has become a topic of interest in the field of anti-corrosion coating. However, in the field of oilfield wastewater corrosion prevention, there are few research reports on the application of GO aqueous solutions as corrosion inhibitors. This paper discovered that GO modified by acylating with imidazoline quaternary ammonium salt (IQAS) can be preferentially adsorbed on carbon steel surfaces to form a relatively dense protective layer, significantly improving the corrosion resistance of carbon steel in oilfield wastewater. N80# carbon steel was taken as the corrosion object, and oilfield wastewater as the corrosion medium to simulate the corrosion of metal equipment in oilfield wastewater during crude oil storage and transportation. The electrochemical polarization curve method, impedance spectrum method, weight loss method, corrosion morphology, and product characterization were used to understand the corrosion inhibition behavior and anti-corrosion mechanism of the GO aqueous solution. The results showed that the corrosion rate of steel sheet with 0.06% GO added at 40°C was 2.023 mm/a, which was 36.15% lower than 3.1685 mm/a in the blank control group. When 0.06% GO and 2.0% IQAS were added simultaneously, the corrosion rate was 1.6494 mm/a, which decreased by 47.94% compared with the blank control group. By weight loss method, the corrosion rate in the crude oil wastewater containing 0.06% GO and 2.0% IQAS at 40°C for 72 h was 0.0768 mm/a, which was 47.5% lower than that in the blank group. The anti-corrosion mechanism involves the inhibition being adsorbed onto the surface of the steel sheet, thereby improving the electrochemical corrosion impedance and reducing the corrosion rate. This research result will provide a novel idea for the development of corrosion and corrosion inhibitors of GO.
Keywords
Corrosion inhibition mechanism
Graphene oxide
Imidazoline quaternary ammonium salt
Modified film forming mechanism
Oilfield wastewater
1. Introduction
Safety has consistently been identified as the most critical issue in the storage and transportation of crude oil. Once corrosion of equipment and pipelines occurs, pitting corrosion, perforation, and other damages may result, leading to pipeline rupture and leakage of crude oil, which can cause major safety accidents, such as explosions and fires [1-13]. This will not only affect the safe and efficient transportation of crude oil but also pose a serious threat to the surrounding environment and people’s lives and property, resulting in significant economic losses [14-21]. In particular, the key equipment in the process of crude oil pipeline transportation, the crude oil storage tank, contains a large amount of wastewater, which often contains many corrosive media, leading to strong electrochemical corrosion and corrosion perforation, resulting in a serious decline in production efficiency and security risks [22]. To solve this problem, in addition to using reasonable coatings, corrosion inhibitors are added to crude oil wastewater to reduce pipeline corrosion, which can also play a significant anti-corrosion role in crude oil transportation [23-27].
Graphene oxide (GO) is an important derivative of graphene. Similar in structure to graphene, it has good mechanical properties, a dense structure, good physical barrier properties, a large specific surface area, and environmental friendliness. At the same time, the surface and edge of GO contain many hydroxyl, carboxyl, and epoxy functional groups [28-29], which are conducive to the formation of an anti-corrosion film on the metal surface. Because of its excellent barrier ability, it has become a research hotspot in the field of anti-corrosives [30-38]. However, at present, GO is mainly modified to enhance its dispersion and is dispersed in the coating as a filler, which can greatly enhance the corrosion resistance of the composite coating [39,40]. Researchers have also applied the prepared graphene quantum dots (GQDs) as a corrosion inhibiting component to the corrosion inhibition of carbon steel by 1 mol/L hydrochloric acid, and the optimal corrosion inhibition efficiency can reach 71%. The mechanism of corrosion inhibition is that the lone pair electrons of the O atom in GQDs and the empty orbital electrons of Fe in carbon steel can be absorbed [41]. In addition, modified GO is used as a corrosion inhibitor for carbon steel under acidification conditions in industrial oil wells, achieving a corrosion inhibition rate reaches 90.27% at 65°C and 15% HCl [42]. However, there are no reports on the corrosion inhibition behavior and application of GO aqueous solutions as corrosion inhibitors in the field of oilfield wastewater anticorrosion. The author’s research group found that a GO aqueous solution has a corrosion inhibition effect on carbon steel in oilfield wastewater; however, the optimal corrosion inhibition effect does not meet the standard requirements for oilfield corrosion prevention. It is necessary to improve its corrosion inhibition performance by modifying organic corrosion inhibitor components [43,44].
Imidazolines and their derivatives are among the most extensively utilized organic corrosion inhibitors in the field of carbon steel protection [45]. Notably, imidazolium quaternary ammonium salts (IQAS) exhibit particularly superior corrosion inhibition performance in acidic corrosive environments [46-52]. However, IQAS often does not exhibit an excellent corrosion inhibition effect in the complex corrosion system of oilfield wastewater with high salinity and high bacterial corrosion [53].
In this paper, a novel hypothesis is proposed that IQAS, an organic heterocyclic compound synthesized by the reaction of oleic acid, diethylenetriamine and benzyl alkylating agent, has the primary amine on its molecule can acylate with the carboxyl group on the GO molecule to modify GO, improve the compactness of forming anticorrosive adsorption type deposit on the surface of carbon steel, and further improve the corrosion inhibition performance. N80 carbon steel was taken as the corrosion object, and oilfield wastewater was taken as the corrosion medium, and the corrosion condition of oilfield wastewater operated by metal equipment at 30-70°C during crude oil storage and transportation was simulated. The corrosion inhibition behavior of N80 carbon steel in oil field wastewater was investigated using potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and weight loss measurements. Atomic force microscope (AFM), X-ray scanning electron microscopy (SEM), Raman spectroscopy (RS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), X-ray diffractometer (XRD), and other characterization methods were utilized to further reveal IQAS-modified GO film forming mechanism and anti-corrosion mechanism. This study should provide a new idea for the development of GO corrosion inhibitors and pave a new way for the industrial application of GO.
2. Materials and Methods
2.1. Materials
Oilfield wastewater, industrial production, Xingzichuan oil production plant of Yanchang Oilfield Company. Flake graphite, Fixed carbon content ≥95, Qingdao Tianhe Da Graphite Co., Ltd. Concentrated sulfuric acid, 98% (mass fraction), Tianjin Kemeiou Chemical Reagent Co., Ltd. Sodium nitrate, analytically pure, Taicang Shanghai Testing Reagent Co., Ltd. Potassium permanganate, analytically pure, Tianjin Kemeiou Chemical Reagent Co., Ltd. Hydrogen peroxide, 30% (mass fraction), Tianjin Kemeo Chemical Reagent Co., Ltd. Concentrated hydrochloric acid, 36% (mass fraction), Tianjin Kemeo Chemical Reagent Co., Ltd. Imidazoline quaternary ammonium salt (IQAS), 97% (mass fraction), Shaanxi Chemical Research Institute Co., LTD.
2.2. Instruments and equipment
Raman spectrometer, BX51TF, OLYMPUS Corporation, Japan. XPS, AXIS SUPRA+, Shimadzu Corporation, Japan. Fourier transform Infrared spectrometer (FTIR), Bruker Tensor27, Bruker, Germany. XRD, Bruker D8 ADVANCE, Bruker, Germany. Field emission SEM, Sigma 300 (σ300), Zeiss, Germany. Electrochemical workstation, CS350M, Wuhan Koster Test Instrument Co., Ltd. AFM, HITACHI AFM100PLUS, Hitachi High-Technologies Co., Ltd. N80 carbon steel, 50×25×2 mm, surface area of 20 cm2, Shanghai Luosong Electromechanical Equipment Co., LTD.
2.3. Specimen preparation
2.3.1. Preparation of GO aqueous solution
GO was prepared by the modified Hummers method [54]. Around 1 g of sodium nitrate (NaNO3) was mixed with 70 mL of concentrated sulfuric acid (H2SO4) in a conical flask, followed by the addition of 2 g of flake graphite. The mixture was stirred continuously under an ice bath. After 30 min, 8 g potassium permanganate (KMnO4) was added. After 35 min of reaction, the device was placed in the water bath at 35-45°C for another 4 h. Then, 120 mL of deionized water was slowly added to the reaction solution several times. After 30 min of the reaction, the temperature was heated to 95°C and maintained for 5 min. Then, 25 mL of 30% hydrogen peroxide (H2O2) was added and stirred until there were no more bubbles in the solution. Finally, 5% hydrochloric acid (HCl) and deionized water were added to centrifugally wash the reaction solution until the pH of the solid substance was neutral after adding an appropriate amount of water to the solid material, it was completely dispersed by an ultrasonic disperser to obtain an aqueous solution of GO. 10 g the aqueous solution of GO was accurately weighed and placed in an evaporation dish and was dried under vacuum at 65°C to constant weight. The solids content of the GO aqueous solution was then calculated.
2.3.2. Preparation of IQAS-modified GO samples for test
The GO aqueous solution was diluted to 0.06% by mass percentage (the highest corrosion inhibition rate) with deionized water. Then, 50 g was placed into two 100 mL glass beakers, and 0.5 g and 1 g of IQAS were added to each, and the mixtures were stirred at room temperature for 1 h using a magnetic force. Then, 10 g of each mixture was put on the clean glass surface. At the same time, 10 g of 0.06% GO was on the clean glass surface and transferred to the oven for drying at 105°C to constant weight. After removing it and allowing it to cool to room temperature, three dry samples were obtained: 0.06% GO, 0.06% GO + 1% IQAS, and 0.06% GO + 2% IQAS. Further characterization was conducted.
2.3.3. Electrochemical test
The electrochemical experimental test adopts the classic three-electrode system. N80 carbon steel was used as the working electrode, polished with 200-mesh sandpaper until shiny before measurement, washed with distilled water, rinsed with anhydrous ethanol, and dried in a dryer for use. The graphite electrode was the auxiliary electrode, the saturated calomel electrode (SCE) was the reference electrode, and the test solution was 80 mL of crude sewage solution. The polarization curve was tested under an open-circuit potential of ±100mV, with a scanning rate of 0.5 mV/s. The corrosion current, corrosion potential, and corrosion rate were obtained by the Tafel extrapolation method. The frequency range of electrochemical impedance (EIS) was 1.0×10-2 - 1.0×105 Hz, and the measured signal was a 50 mV sine wave. The experimental data were fitted and analyzed using Zview software .2.3.4. The corrosion rate was measured by the weight loss method.
N80 carbon steel sheet should be polished with sandpaper until bright and then cleaned with petroleum ether and anhydrous ethanol in turn, wiped the surface with absorbent cotton ball, dried with a hair dryer, stood in the dryer for 2 h, weighed the steel sheet with an analytical balance, and then measured the area of the test piece with a vernier caliper. Three 500 mL volumetric bottles were filled with an equal amount of oilfield wastewater, which contained the optimal amount of GO and the optimal ratio of GO and IQAS, respectively. These bottles were then placed in an oil bath at 40°C. The steel sheet was tied with a Teflon waterproof belt, with three steel sheets in each group. The three groups were suspended in three bottles, allowing the steel sheet to be completely immersed in the sewage solution. After holding and standing for 72 h, the test piece was removed, and the surface was cleaned with decontamination powder. The soft rubber was polished and then cleaned with petroleum ether and anhydrous ethanol. The surface was wiped with an absorbent cotton ball, dried with a hair dryer, and left to stand in the dryer for 2 h. After completely drying, the quality of the steel sheet was measured with an analytical balance. The corrosion rate was calculated as follows.
The corrosion rate was calculated as follow formulas Eqs. (1) and (2):
V, corrosion rate (g /m2·h), V: corrosion rate (mm/a). W, initial weight of the metal specimen (g). W1, weight of the metal specimen after removing the corrosion product (g). A, surface area of the specimen (m2). t, time of corrosion operation (h).
2.3.4. Corrosion morphology and product analysis on the steel sheet surface
The N80 carbon steel was polished until bright, cleaned with petroleum ether and anhydrous ethanol. The surface was wiped with an absorbent cotton ball, dried with a hair dryer, and left in the dryer for 2 h. Secondly, the oil field sewage, the sewage including the optimal amount of GO, and the sewage containing the optimal ratio of GO, and IQAS, were coated on the surface of the steel sheet. After parking in a closed glass container at 40°C for 72 h, the water was dried in a drying oven at constant weight. The corrosion damage and protection of the steel sheet surface were characterized by SEM. The corrosion products on the surface of the steel sheet were characterized by XRD and FTIR.
3. Results and Discussion
3.1. Mechanism of IQAS-modified GO
In the process of studying the anti-corrosion performance of GO, although GO aqueous solution has certain corrosion inhibition performance on carbon steel in oilfield wastewater, the corrosion inhibition efficiency is not sufficient to meet the anti-corrosion standard requirements of industrial production. Therefore, it is proposed to modify GO with IQAS, which has an excellent corrosion inhibition effect in acidic corrosion media. The mechanism of IQAS-modified GO is that the primary amine group of the IQAS molecule and the carboxyl group of the GO molecule are acylated to form a network structure, fill the gap of the GO lamellar layer, improve the density of the anti-corrosion adsorption film, and enhance the corrosion inhibition performance. The reaction diagram has been given in Figure 1.
To be suitable for the anti-corrosion function of carbon steel in oilfield wastewater as much as possible, when revealing the mechanism of IQAS-modified GO, the concentration of GO aqueous solution was chosen as 0.06%. The concentration that could obtain the best corrosion rate when GO was used alone. And the IQAS addition amounts were chosen as no addition, insufficient amount, and excessive amount, namely 0%, 1%, and 2%. The structure of the deposited adsorbate obtained in these three cases of addition could fully reflect the production process of modified substances in industrial applications. FTIR, RS, XPS, and SEM characterization were used to reveal the formation mechanism of IQAS-modified GO anti-corrosion films. FTIR was used to analyze the evolution of functional groups at different stages of the coating using potassium bromide tablets in the wavelength range of 400- 4000 400-4000cm-1. In the RS test, a 785 nm laser was used for excitation, and the integration time was 20 seconds.
Figure 2 shows the infrared spectra of the deposited adsorbate of 0.06% GO, 0.06%GO+1%IQAS and 0.06% GO + 2 % IQAS. It can be seen from the Infrared spectra that the characteristic peak of the deposited adsorbate of 0.06% GO is very obvious. At 1726 cm-1 is the C=O weak stretching vibration peak. The flexural vibration absorption peaks of C-OH are found at 1620 and 1645 cm−1. At 1116 cm−1 is the vibration absorption peak of C-O-C. When 1% IQAS reacts with GO, the double bending vibration absorption peak of C-OH at 1620 and 1645cm−1 disappears in the infrared image and becomes a single peak with a width of 1650cm−1, which is the C=O absorption peak on the amide group after the carboxyl group on GO reacts with the primary amine acylation on IQAS. Accordingly, C-N bond absorption peaks in the molecular structure of IQAS at 1456 and 1343 cm-1 also appeared. With the increase of IQAS to 2%, these characteristic peaks became more obvious. The results of the IR spectra showed that acylation of IQAS and GO occurred.
Figure 3 shows the Raman spectra of the deposited adsorbate of 0.06% GO, 0.06%GO+1%IQAS and 0.06% GO + 2 % IQAS. Two main characteristic peaks can be seen in all three Raman spectral curves. The first characteristic peak is the G peak at approximately 1601 cm-1, which represents the hybridization bond between the anticorrosion film and the corresponding carbon atoms in the sp2 configuration, and is the intrinsic peak of graphene [55]. The second characteristic peak is peak D, which appears at about 1326 cm-1 and is stronger than peak G. The D-peak usually means the defect site of graphene and the sp3 hybrid C atom. The D-peak is a Raman signal caused by the distortion of the graphene surface holes and oxygen-containing groups at the edge of the holes, the oxygen-containing groups at the edge of the entire GO sheet, and the two-dimensional structure. The lower G peak than D peak in this Raman spectrogram indicates that GO reaccumulates to form a multilayer structure after adsorption and deposition to form a corrosion film. When a 1% IQAS modifier was added, the membrane structure of GO was not changed despite the acylation reaction with GO. However, when IQAS is in addition to 2%, it exceeds the acylation amount relative to GO, and the excess IQAS will wrap GO, resulting in a decrease in the intensity of D and G peaks.
Figure 4 shows the XPS spectra of the deposited adsorbate of 0.06% GO, 0.06% GO + 1% IQAS, and 0.06% GO + 2 % IQAS. This information can be obtained from the full peak map of the three dry films (see Figure 4a). The XPS map was obtained after the test data was obtained and corrected with the binding energy of 284.8 eV corresponding to the polluting carbon source. The O1s peak is around 531.62 eV, 284-290eV is the C1s peak. Compared with the deposited adsorbates of 0.06% GO and IQAS modified GO, the position of O1s peak and C1s peak does not change, only the strength of O1s peak of GO is greater than that of C1s peak, and the situation is opposite after adding IQAS. The reason is that there is no oxygen atom in the IQAS molecule, and the proportion of total oxygen element in the molecular structure of the dry film decreases after acylation. According to the fitting results of C1s peaks of the three types, GO membrane has obvious C-C, C-O, and C=O bond peaks at 284.085, 286.95, and 287.96 eV [56], while the C=O bond peaks disappear after the addition of IQAS, and a new amides N-C=O bond peak appears at 286.21eV. The peak intensity increased with the increase of IQAS, adding mass (see Figure 4b). According to the fitting results of the three O1s peaks (see Figure 4c), the GO membrane has obvious O1s peaks brought by C=O and C-O at 530.76 and 532.02 eV. When IQAS is added, the peak value of the C=O bond becomes smaller than that of the C-O, which is because the -OH in the carboxyl group of the GO molecular structure will be removed by acylation reaction, resulting in a decrease in oxygen content in the membrane.
As SEM of the deposited adsorbate structure can be seen in Figure 5. When the anticorrosive deposited adsorbate formed when only GO was used as the corrosion inhibitor, the single layer of GO was re-deposited into a graphite-like multilayer film through adsorption, with large gaps, and the film was not dense (see Figure 5a). As shown in Figure 5(b), when IQAS was added, the acylation reaction occurred with GO, and GO was connected by acyl groups to eliminate large gaps and form a relatively dense anticorrosive film. As shown in Figure 5(c), the addition of excessive IQAS fills the holes and gaps of the GO+IQAS film, making the anti-corrosion film denser and improving the anti-corrosion effect. The results of SEM are consistent with those of FTIR, RS, and XPS. This shows that the film-forming theory hypothesis of IQAS modified GO proposed in this paper is true.
3.2. Corrosion polarization curve of the steel sheet in the oilfield wastewater
First, the corrosion polarization curves of the steel sheet in the oilfield wastewater at different temperatures were tested, as shown in Figure 6, and the relevant electrochemical parameters were given in Table 1. As shown in Figure 6, when the test temperature is between 30°C and 70°C, the corrosion principle of carbon steel sheet in oilfield wastewater conforms to the reaction mechanism of typical corrosion galvanic cells, and the slope of the cathode polarization curve is significantly greater than the slope of the anode polarization curve, so it belong to the electrochemical corrosion under cathode control. Table 1 shows that the corrosion rates of steel sheet are higher at 40°C and 70°C, which are 3.1685 mm/a and 3.2634 mm/a, respectively. At 40°C and 70°C, the corrosion current density of the carbon steel was higher than that of the other control groups, 366.66 µA/cm2 and 378.51 µA/cm2, respectively. However, since the actual working temperature of the crude oil settling tank in the process of crude oil storage and transportation is between 40°C and 60°C, 40°C, with a higher corrosion rate, is used as the subsequent experimental temperature.
| T (°C) | Ecorr (mV) | Icorr, (µA/cm2) | Ba (mV) | Bc (mV) | Corrosion rate (mm/a) |
|---|---|---|---|---|---|
| 30 | -900.3 | 212.38 | 3168.9 | 253.85 | 1.8479 |
| 40 | -888.05 | 366.66 | 15010 | 250.6 | 3.1685 |
| 50 | -867.63 | 338.04 | 9231.8 | 229.43 | 2.8961 |
| 60 | -830.18 | 287.20 | 50528 | 213.5 | 2.4881 |
| 70 | -817.56 | 378.51 | 3561 | 227.43 | 3.2634 |
Figure 7(a) shows the polarization curve of an aqueous solution of GO with changed contents added to oilfield wastewater at 40°C. Combined with the electrochemical parameters in Table 2, it can be concluded that as the concentration of GO changes from small to large, the corrosion rate of the carbon steel sheet by sewage decreases initially, then increases. The corrosion rate of steel sheet is the lowest when 0.06% of GO aqueous solution is added, which is 2.02 mm/a. So it can be determined that the best amount of GO is 0.06% of the mass of sewage. Figure 7(b) shows the polarization curve obtained after adding 0.06% GO to sewage and then adding different concentrations of IQAS to investigate the synergistic anti-corrosion effect of GO and IQAS.
| GO (wt%) | IQAS (wt%) | Ecorr (mV) | Icorr, (µA/cm2) | Ba (mV) | Bc (mV) | Corrosion rate (mm/a) |
|---|---|---|---|---|---|---|
| 0.02 | - | -874.94 | 299.81 | 2652.6 | 264.63 | 2.5586 |
| 0.04 | - | -847.93 | 250.77 | 11829 | 230.27 | 2.1339 |
| 0.06 | - | -898.00 | 258.48 | 4922.5 | 214.12 | 2.023 |
| 0.08 | - | -915.86 | 361.29 | 3934 | 260.60 | 3.1285 |
| 0.10 | - | -923.56 | 335.82 | 3547.9 | 257.00 | 2.6227 |
| 0.06 | 0.5 | -879.77 | 312.05 | 3352.8 | 256.88 | 2.6943 |
| 0.06 | 1.0 | -885.55 | 297.16 | 2546.2 | 263.01 | 2.5469 |
| 0.06 | 1.5 | -882.45 | 277.10 | 3016.6 | 282.27 | 2.3591 |
| 0.06 | 2.0 | -869.27 | 212.10 | 2493.2 | 249.21 | 1.6494 |
| 0.06 | 2.5 | -867.24 | 247.02 | 3883.6 | 242.42 | 1.9200 |
| 0.06 | 3.0 | -858.38 | 233.47 | 4236.4 | 244.11 | 1.8205 |
According to the polarization curve in Figure 7(b) combined with the electrochemical parameters in Table 2, it can be concluded that as the concentration of IQAS added changes from small to large, the corrosion rate of carbon steel sheet by sewage also changes from large to small and then becomes large. Therefore, the added amount of co-corrosion prevention for IQAS and GO also has an optimal value. The lowest corrosion rate is 1.6494 mm/a when 0.06% GO and 2% IQAS are added simultaneously. However, excessive addition of GO and IQAS increases the corrosion rate, so there is an optimal amount of addition. It can be seen from the parameters in Table 2 that the corrosion current density of the anode and cathode decreases significantly with the addition of GO and IQAS. The lowest corrosion current density is 212.10 µA/cm2 when 0.06% GO and 0.2% IQAS are added. The values of the slopes
Ba and Bc also varied with the amount of GO and IQAS, indicating that they control both cathode and anode reactions. For the corrosion galvanic cell reaction, the anode reaction is the oxidation reaction of the steel sheet, and the cathode reaction is the reduction reaction of hydrogen. By adding GO and IQAS, a dynamic covering film can be formed on the surface of the steel sheet, blocking the active site, reducing the dissolution of the steel sheet in the anode, slowing down the reduction of hydrogen evolution in the cathode, hindering the electron flow of the corrosion galvanic cell and reducing the corrosion current. Thus, the corrosion rate of the steel sheet is reduced.
3.3. EIS analyze of the steel sheet in the oilfield wastewater
Figure 8 shows the Nyquist diagram and Bode diagram of the corrosion process of N80 steel sheet in oilfield wastewater at different temperatures, oilfield wastewater with different concentrations of GO, oilfield wastewater with different concentrations of IQAS, and wastewater with 0.06% GO and different concentrations of IQAS. In all Nyquist plots, the arcs of capacitive reactance are shown only as a semicircle, indicating that the corrosion process of N80 steel sheet corresponds to the electron transfer restriction process, and the larger the semicircle radius, the greater the resistance, which is related to the roughness of the surface, the uneven surface electrode and the mass transfer process [57].
Under all different test conditions, the equivalent circuit diagrams of electrochemical impedance fitting for corrosion of steel sheet in sewage are the same, as shown in Figure 9. Where Rs is the solution resistance, R1 is the charge transfer resistance, and CPE is the double layer capacitor. The relevant fitting parameters are presented in Table 3. Rs decreases with the increase of temperature, while R1 and CPE change irregularly.
| Temperature | Rs (Ω) | R1 (Ω) | CPE-T | CPE-P |
|---|---|---|---|---|
| 30°C | 29.42 | 1016 | 0.00073575 | 0.68349 |
| 40°C | 21.23 | 1518 | 0.00087850 | 0.70249 |
| 50°C | 19.13 | 938.6 | 0.00072877 | 0.73842 |
| 60°C | 18.80 | 426.3 | 0.00084110 | 0.75757 |
| 70°C | 18.25 | 500.6 | 0.00150480 | 0.67511 |
As shown in Figures 8(a) and (b), the real axis intercept of the capacitive reactance arc in the low frequency region decreases with the increase of temperature, and the arc radius of the capacitive reactance in the high frequency region also shows irregular changes with temperature. This is because the sewage contains complex electrolytes and impurities. The adsorption form on the steel sheet is very chaotic under the influence of temperature, and cannot form a dense film, so that the corrosion electrode on the metal surface has dispersion and does not change regularly. When GO is added to the sewage, its impedance diagram at 40°C is shown in Figures 8(c) and (d). The change of intercept of the arc of capacitive reactance in the high frequency region of the Nyquist plot on the real axis is that the addition of GO is larger than that of the blank group, and with the increase of GO addition concentration, the intercept decreases first and then increases. The arc radius of the bulk reactance in the high frequency region is lower than that in the blank group, and it still shows irregularity with the addition concentration, as well as the Bode diagram. When 0.06% GO is added to the sewage, Rs is 28.19 Ω, which is higher than the Rs of the blank sample (21.23Ω), indicating that GO adsorbs on the surface of the carbon steel sheet to increase the resistance of the corrosion circuit, and plays a certain anti-corrosion effect. However, it is still unable to form a dense film, so that the corrosion electrode on the metal surface is dispersion. In addition, because GO has good electrical conductivity, too much addition will reduce impedance, resulting in an increase in the corrosion rate. This result is the same as that of the polarization curve method to test the corrosion rate. The impedance diagram at 40°C of different concentrations of IQAS added to the sewage is shown in Figures 8(e) and (f). When IQAS is added, the intercept of the capacitive reactance arc in the high frequency region of the Nyquist diagram first increase and then decrease on the real axis, and the radius of the capacitive reactance arc in the low frequency region is larger than that in the blank group, indicating that the addition of IQAS will change the solution resistance and increase the electron migration resistance and capacitive reactance effect. However, the arc radius of the capacitive reactance in the high frequency region does not change with the addition of concentration, indicating that its adsorption on the surface of carbon steel is controlled by thermodynamics and kinetics, and there is an optimal concentration between 1-2%. When 0.06% GO and different concentrations of IQAS are added to the sewage at the same time, the impedance diagram at 40°C is shown in Figures 8(g) and (h). The curves of the Nyquist diagram and the Bode diagram began to change regularly with the addition of IQAS concentration. The change of the intercept of the capacitive reactance arc on the real axis first increases and then decreases, while the change of the arc diameter in the high frequency region gradually increases with the increase of the concentration of IQAS. This shows that with the addition of IQAS, it acylates with GO in sewage, forming a network compound adsorbed on the surface of carbon steel, and gradually forms a relatively complete protective film, which increases the solution resistance Rs, charge transfer resistance R1, and bulk reactance effect CPE. The formation of a surface protective film has a stronger capacitance effect. However, as IQAS continues to increase, Rs began to become smaller again, reducing the anti-corrosion effect (see Table 4). This is due to the failure of the excess IQAS to react with GO, and its cationic properties increase the conductivity of the solution.
| CIQAS (wt%) | CGO (wt%) | Rs (Ω) | R1 (Ω) | CPE-T | CPE-P |
|---|---|---|---|---|---|
| 0.5 | - | 23.93 | 3877 | 0.00082703 | 0.61783 |
| 1.0 | - | 30.18 | 662.9 | 0.00134770 | 0.62601 |
| 1.5 | - | 26.52 | 1918 | 0.00787140 | 0.62408 |
| 2.0 | - | 27.56 | 2839 | 0.00065773 | 0.65764 |
| 2.5 | - | 20.55 | 1378 | 0.00152610 | 0.62492 |
| 3.0 | - | 26.90 | 1054 | 0.00071999 | 0.68608 |
| - | 0.02 | 37.41 | 924.9 | 0.00113320 | 0.61899 |
| - | 0.04 | 28.34 | 265.1 | 0.00800060 | 070221 |
| - | 0.06 | 28.19 | 532.3 | 0.00080583 | 0.66581 |
| - | 0.08 | 38.71 | 345 | 0.00140480 | 0.63278 |
| - | 0.10 | 41.5 | 542,4 | 0.00091368 | 0.60756 |
| 0.5 | 0.06 | 34.23 | 914.3 | 0.00139650 | 0.58184 |
| 1.0 | 0.06 | 39.29 | 1019 | 0.00124070 | 0.58898 |
| 1.5 | 0.06 | 36.96 | 1295 | 0.00106640 | 0.59882 |
| 2.0 | 0.06 | 34.26 | 1739 | 0.00056088 | 0.65795 |
| 2.5 | 0.06 | 29.19 | 1794 | 0.00050186 | 0.68890 |
| 3.0 | 0.06 | 30.04 | 2191 | 0.00057894 | 0.66753 |
In general, the addition of GO and IQAS does not change the equivalent circuit of the impedance, indicating that their presence does not change the corrosion mechanism of the steel sheet. When GO and IQAS are added simultaneously, the two acylates form a network protective film on the surface of carbon steel to form a more complete protective adsorption layer, resulting in increasing resistance to electrode corrosion reaction, reducing the electrochemical corrosion rate and enhancing the corrosion inhibition, proving that GO and IQAS have a synergistic effect. However, excessive addition of GO and IQAS will reduce R1 and decrease the corrosion inhibition rate. Therefore, the optimal ratios of GO and IQAS are 0.06% and 0.2%. This is in line with the conclusion obtained by the polarization curve method.
3.4. Corrosion rate by weight loss method
In order to verify the effectiveness of GO in actual industrial corrosion prevention applications, the corrosion rate of N80 carbon steel test pieces was tested in oil field wastewater, oil field wastewater containing 0.06% GO, and oil field wastewater containing 0.06% GO + 2.0% IQAS at 40°C for 72 h. The results have been presented in Table 5. When 0.06% GO is added to oilfield wastewater, the corrosion rate decreases, but it does not attain the standard corrosion rate of the industrial oilfield wastewater corrosion inhibitor. When 0.06% GO and 2.0% IQAS are added simultaneously, the corrosion rate is 0.0768mm/a, which is reduced by 47.5% compared with the blank group, and attain the requirements of industrial application, which further indicate that GO and IQAS have a synergistic anti-corrosion effect on the corrosion of oilfield wastewater.
| Sample | Oilfield wastewater | GO | GO+IQAS |
|---|---|---|---|
| Corrosion rate (g/m2·h) | 0.1310 | 0.1220 | 0.0688 |
| Corrosion rate (mm/a) | 0.1462 | 0.1361 | 0.0768 |
3.5. Anti-corrosion mechanism analysis
To explore the corrosion inhibition mechanism of GO and IQAS on steel sheet, the morphology and composition of corrosion products on the surface of carbon steel were characterized and analyzed by AFM, SEM, XRD, and FTIR. The AFM and SEM of GO added during the test have been shown in Figure 10. GO is a two-dimensional monolayer with a thickness of 0.55 nm.
Figure 11(a) shows the SEM image of corrosion products on the surface of the steel sheet after corrosion by oilfield wastewater without adding any anti-corrosion materials. The surface is the subject with crystals of organic and inorganic substances and salts in the sewage, but no dense passivation film is formed. When 0.06% GO is added to the wastewater, the SEM morphology of corrosion products on the surface of the steel sheet is shown in Figure 11(b). The salt crystals on the surface are significantly reduced, and a less dense anticorrosive film is formed, which hinders the corrosion process to a certain extent. Figure 11(c) shows the SEM of the corrosion products on the surface of the steel sheet from the sewage when 0.06% GO and 2.0% IQAS are added together. GO and IQAS react to form a network anticorrosive film. This relatively condensed film blocks the electrolytes of water and inorganic salts well outside the metal surface and has an anti-corrosion effect.
Figure 12(a) shows the XRD pattern with Cu-Kα radiation (λ=0.15418 nm) of the corrosion products on the steel plate surface in sewage. In the figure, the sample has characteristic peaks at 14.58°, 31.70°, 45.44°, and 66.17o. These characteristic peaks are in the same position as the diffraction peaks of rock salt crystals, and the corresponding crystal faces are respectively (200), (400), and (420), indicating that a large number of rock debris and inorganic salt deposits are deposited when the steel sheet is corroded in sewage, which is consistent with the SEM topography. Figure 12(b) depicts the XRD pattern of corrosion products in wastewater with 0.06% wt GO added to the surface of the steel sheet. Characteristic peaks appear at 27.35o, 31.70°, 45.48° and 66.23o. These characteristic peaks are in the same position as the diffraction peaks of rock salt crystals, and the corresponding crystal faces are (200) and (220), respectively. This shows that after adding a small amount of GO in the sewage, GO is preferentially deposited on the surface of the steel sheet, blocking the electrolyte rock salt corrosion medium in the sewage outside the metal surface, and deposited on the GO. Therefore, the XRD pattern and Figure 12(a) show little change, and only have a wide peak at 2θ less than 15o, which is characteristic of graphene. Figure 12(c) shows the XRD pattern of corrosion products on the surface of the steel sheet in the sewage with 0.06%wt GO and 2.0%wt IQAS added. Different from Figure 12(b), the diffraction characteristic peaks of graphene appear at 15.66° and 26.65°. In addition, 42.93o is the characteristic peak of calcite. The corrosion products of sewage +GO+IQAS on steel sheet contain CaCO3 crystals. Characteristic peaks appear at 31.84°, 45.54°, and 66.58o. These characteristic peaks are in the same position as the diffraction peaks of rock salt crystals, and the corresponding crystal faces are (220) and (222), indicating that rock salt crystals are still contained in the corrosion products at this time, and GO+ IQAS could enrich inorganic salts outside the anti-corrosion film after coordination. IQAS forms corrosion products with high resistance, reducing the corrosion current and ultimately the corrosion rate.
Figure 13(a) depicts the FTIR spectrum of the corrosion products on the surface of the steel sheet in the sewage. Figure 13(b) depicts the FTIR spectrum of the corrosion products on the surface of the steel sheet in the sewage with 0.06% GO and 2.0% IQAS added. Figure 13(c) shows the FTIR spectrum of the corrosion products on the surface of the steel sheet in the sewage with 0.06% GO and 2.0% IQAS added. The positions of these infrared characteristic peaks in the three cases are essentially the same. Due to the complex impurities in the sewage, it is speculated that the wide peaks at the wavelength of 3600 cm-1 to 2700 cm-1 are the peaks of the -OH antisymmetric stretching vibration on the structural water or GO molecules. The absorption peak near 1630 cm-1 is the C=C double bond on the aromatic hydrocarbon or the weak absorption peak of C=O stretching vibration on the amide, and the absorption peak near 1400 cm-1 is the stretching vibration peak of aromatics or ammonium salts. These are the contributions of N-H functional groups in IQAS and organic sediments, such as demulsifier, high polymer of drilling fluid, and crude oil that may exist in sewage. In Figures 13(b) and (c), the position, width, and peak intensity of the broad peak at 3600 cm-1 to 2700 cm-1 and the absorption peaks at 1630 cm-1 and 1400 cm-1 are basically the same. The only difference between Figure13 (a) and the first two.
The figure displays the broad peaks at 3600 cm-1 to 2700 cm-1 narrowed. The peak strength of the absorption peak at 1400 cm-1 becomes stronger. This phenomenon shows that GO added to the sewage is adsorbed on the metal surface, followed by the attachment of various impurities and inorganic salts in the sewage to it. The molecules are mainly aromatic rings, so it does not cause changes in the infrared spectrum. When GO and IQAS are added, GO forms a network structure after the acylation reaction. The infrared spectrum changes, preventing the adsorption of amino and amide groups of organic impurities in sewage on the surface of carbon steel, resulting in a weakening of the peak strength of the absorption peak at 1400 cm-1.
By polarization curve, EIS, XRD, and FTIR characterization, the anti-corrosion mechanism is that the carboxyl group on graphite oxide is used to amidase the amino group in IQAS. In the acylation reaction, IQAS modified GO and formed a dense mesh adsorption film. The reaction product can be uniformly dispersed in aqueous solution and can be selectively adsorbed on the carbon steel surface after contact with the carbon steel surface to form a relatively dense anti-corrosion film. The impedance of the corrosion galvanic cell increases, and the corrosion current intensity and corrosion rate decrease. A schematic diagram has been shown in Figure 14.
4. Conclusions
In this paper, a theoretical hypothesis is proposed that GO can be modified by acylation of IQAS to enhance the densification and corrosion inhibition of the adsorption film. The study results are consistent with the theoretical hypothesis of anticorrosive film formation. N80 carbon steel was used to simulate the corrosion of crude oil storage tanks in oilfield wastewater, and the influence of different concentrations of GO aqueous solution on the corrosion rate was investigated. By corrosion polarization curve, GO with 0.06% was added had the best corrosion inhibition effect, and the corrosion rate of the steel sheet was 2.023 mm/a, which decreased by 36.15% compared with 3.1685mm/a in the blank control group. At the same time, when 0.06% GO and 2.0% IQAS were added, the corrosion inhibition rate reached 1.6494mm/a, which decreased by 47.94% compared with the blank control group. The test results of the weightlessness method showed that the corrosion rate of oil field wastewater containing 0.06% GO and 2.0% IQAS was 0.0768 mm/a after standing at 40°C for 72h, which was 47.5% lower than that of the blank group. The anti-corrosion mechanism is that GO and IQAS have the acylation reaction, forming a relatively dense protective layer on the surface of the steel sheet, improving the electrochemical corrosion impedance, impeding the electron flow of the corrosion galvanic cell, and reducing the corrosion current density, reduce corrosion rate. The research results provide a new idea for the development of anticorrosion function and corrosion inhibitors of GO. It provides a new method to prevent the corrosion of steel equipment and pipelines caused by oil field sewage.
Acknowledgement
This work was supported by the National Natural Science Foundation of China (Grant 22268046), Yulin Science and Technology Bureau (Grant CXY-2021-106-01).
CRediT authorship contribution statement
Xiaodong Chen: Conceptualization, Funding acquisition, Supervision, Writing – review & editing. Mihui Xie: Investigation, Formal analysis, Writing – original draft. Jiannan Ai: Investigation. Yanli Gao: Investigation. Yonglin Yang: Writing – review & editing. Bo Zhang: Investigation. Ming Li: Investigation.
Declaration of competing interest
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Declaration of generative AI and AI-assisted technologies in the writing process
The authors confirm that there was no use of AI-assisted technology for assisting in the writing of the manuscript and no images were manipulated using AI.
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