CN113073330A - Compound corrosion inhibitor suitable for low alloy steel and preparation and application thereof - Google Patents
Compound corrosion inhibitor suitable for low alloy steel and preparation and application thereof Download PDFInfo
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- CN113073330A CN113073330A CN202110269767.4A CN202110269767A CN113073330A CN 113073330 A CN113073330 A CN 113073330A CN 202110269767 A CN202110269767 A CN 202110269767A CN 113073330 A CN113073330 A CN 113073330A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
Abstract
The invention relates to an environment-friendly compound corrosion inhibitor, in particular to a compound corrosion inhibitor suitable for low alloy steel, preparation thereof and application thereof as a compound corrosion inhibitor in natural seawater. The effective components of the corrosion inhibitor are polyaspartic acid and sodium tungstate, and the mass concentration ratio is that the polyaspartic acid: sodium tungstate 10: (1-4). Compared with a single PASP corrosion inhibitor, the polyaspartic acid compound sodium tungstate corrosion inhibitor has the advantages that the film forming speed on the metal surface is high, the corresponding corrosion inhibition rate is relatively stable, the generation of corrosion products on the surface of low alloy steel is inhibited, the corrosion of the low alloy steel and the like in natural seawater can be effectively protected, and the corrosion inhibition effect is better.
Description
Technical Field
The invention relates to an environment-friendly compound corrosion inhibitor, in particular to a compound corrosion inhibitor suitable for low alloy steel, preparation thereof and application thereof as a compound corrosion inhibitor in natural seawater.
Background
The low alloy steel has high strength, good fatigue resistance, high toughness, low brittle transition temperature, good cold forming performance and welding performance, better corrosion resistance and certain wear resistance, and is suitable for large-scale steel structures such as electric power iron towers, wharfs, bridges, offshore oil platforms and the like. In the application process of the low alloy steel in the marine environment, the low alloy steel is influenced by the severe marine corrosion environment, so that corrosion safety accidents are easy to happen, the safety production is seriously threatened, and effective corrosion protection measures must be taken.
At present, corrosion inhibitor research has achieved some research results, but the research results mainly focus on heterocyclic compounds and heavy metal salts, and although these substances have a certain protection effect on corrosion, the application of these substances is limited to a great extent due to the problems of high cost, high toxicity and the like. Therefore, in the present day that environmental protection is more and more important, the development of environment-friendly corrosion inhibitors has become one of the hot spots for corrosion inhibitor research. In the field of corrosion inhibitors, tungstate is an environment-friendly substance because of no harm to human bodies and the environment, and scientists have studied a great deal of tungstate. However, research results show that tungstate is an anode type corrosion inhibitor with weak oxidizability, and when 100mg/L of sodium tungstate is added, a test piece is seriously corroded, and the surface is rough and has multiple plaques; when 600mg/L sodium tungstate is added, the hanging piece is bright, a small amount of plaque exists on the edge, the pitting is slightly corroded, and when the adding amount of the sodium tungstate is increased to 1200mg/L, the hanging piece is bright and clean, and the edge plaque disappears. When the amount of the sodium tungstate is small, the corrosion inhibition efficiency is not high when the sodium tungstate is used as a seawater corrosion inhibitor alone, and in order to achieve a better corrosion inhibition effect, the addition amount of the sodium tungstate needs to be higher, and in order to reduce the use amount of the sodium tungstate and better inhibit pitting corrosion, the sodium tungstate can be compounded with other corrosion inhibitors and realized by a synergistic effect, so that the research on the compounding effect of the sodium tungstate and other corrosion inhibitors is widely concerned by people.
Disclosure of Invention
The invention aims to provide a compound corrosion inhibitor suitable for low alloy steel, a preparation method thereof and application of the compound corrosion inhibitor in natural seawater.
In order to achieve the purpose, the invention adopts the technical scheme that:
a compound corrosion inhibitor suitable for low alloy steel comprises the following effective components of polyaspartic acid and sodium tungstate, wherein the mass concentration ratio of the polyaspartic acid: sodium tungstate 10: (1-4).
The effective components of the corrosion inhibitor are polyaspartic acid and sodium tungstate, and the mass concentration ratio is that the polyaspartic acid: sodium tungstate 10: 3.
the polyaspartic acid is prepared by using L-aspartic acid as a raw material () and adding a catalyst H3PO4Under the action of 200-3PO4The mass ratio is more than 1; during hydrolysis, the concentration of alkali influences the hydrolysis process of polyaspartic anhydride, and alkali is added until the pH value of a system is 3-8, wherein the alkali is sodium hydroxide generally.
The corrosion inhibitor is prepared by adding effective components into natural seawater; wherein the mass concentration of the polyaspartic acid is 500mg/L, and the mass concentration of the sodium tungstate is 50-200 mg/L.
The corrosion inhibitor is suitable for application of a low alloy steel compound corrosion inhibitor, and is applied to the low alloy steel compound corrosion inhibitor in a marine environment.
The low alloy steel refers to alloy steel with the total amount of alloy elements less than 5%, and is relative to carbon steel, on the basis of the carbon steel, one or more alloy elements are intentionally added into the steel in order to improve the performance of the steel, and the low alloy steel is widely applied to the manufacturing of engineering machinery, wharfs, ships, bridges and high-rise buildings.
The method for testing the electrochemical performance of the polyaspartic acid compound sodium tungstate corrosion inhibitor comprises the following steps: the test temperature is 303K by using a Gamry 3000 electrochemical system connected with a computer for detection. The test solutions with and without the addition of corrosion inhibitors were placed in 500m L glass beakers and the experiments were performed with a three-electrode system. In the three-electrode system, a saturated calomel electrode was used as a reference electrode, a platinum sheet electrode was used as an auxiliary electrode (counter electrode), and a working electrode was a low alloy steel sample having a size of 10mm × 10mm × 10 mm. Experiments were conducted with electrochemical alternating current impedance spectroscopy (EIS) at open circuit potential, setting the frequency range to 10 mhz to 100 khz, and the peak-to-peak amplitude of the alternating signal to 10 mV. The scan rate during the polarization curve test was 1m Vs-1, with a scan potential ranging from-250 mV to +250mV relative to the Open Circuit Potential (OCP) when the working electrode was at steady state (the floating range of open circuit potential was within 5 mV). The experiment was repeated three times for each experimental condition.
The surface analysis method of the polyaspartic acid compound sodium tungstate corrosion inhibitor comprises the following steps: soaking a sample in an experimental solution for 5 days, and detecting the surface of the sample by using an S-3400N Scanning Electron Microscope (SEM) and an Atomic Force Microscope (AFM); the surface of the stainless steel sample is characterized by Fourier infrared spectroscopy (FTIR) which adopts a Bruker Vertex 70FTIR detector and has the resolution of 2cm-1。
The basic principle of the invention is as follows:
compared with other preparation methods, the heat condensation method using L-aspartic acid as the raw material is easier to control and has good repeatability in the reaction process, the conversion rate can reach 94 percent, and low chroma and relative score can be preparedA high molecular weight polymer. Polyaspartic acid is an amphoteric substance which forms PASPH in solution+Positive ions, PASPH+The poly-aspartic acid contains a large amount of amino and hydroxyl, and contains nitrogen atoms and oxygen atoms with lone pair electrons in molecules, so that the poly-aspartic acid can be effectively adsorbed on the surface of the low alloy steel. At this time, PASPH+So as to be adsorbed on the metal surface or on the active sites of electrochemical reaction with high coverage rate, thereby improving the corrosion inhibition efficiency of the polyaspartic acid.
The invention has the advantages that:
the invention adopts the polyaspartic acid compounded sodium tungstate as the corrosion inhibitor for the specific substrate under the environment, and the mode not only can effectively improve the corrosion inhibition efficiency of the polyaspartic acid on the low alloy steel, but also has no harm to human bodies and the environment, thereby being an effective environment-friendly compounded corrosion inhibitor. The method specifically comprises the following steps:
1. the corrosion inhibition efficiency of the low alloy steel is improved. When the sodium tungstate is used alone as a seawater corrosion inhibitor with a small amount, the corrosion inhibition efficiency is not high, the addition amount of the sodium tungstate needs to be higher to achieve a better corrosion inhibition effect, and in order to reduce the use amount of the sodium tungstate and better inhibit pitting corrosion, the sodium tungstate and the polyaspartic acid can be compounded, and the corrosion inhibition efficiency is improved by virtue of a synergistic effect. The slow release effect of the compound corrosion inhibitor on the low alloy steel in the natural seawater is better.
2. Green and environmental protection without pollution. The polyaspartic acid is non-toxic and environment-friendly, has biodegradability and scale inhibition, and has simple and easy-to-operate synthesis process. The other component of the corrosion inhibitor is sodium tungstate, which is harmless to human bodies and the environment.
3. The water solubility is good. The corrosion inhibitor is polyaspartic acid compounded sodium tungstate, the two components have good water solubility, and organic solvent dissolution is not needed in the application process, so that the cost is saved, the environmental problem after use does not exist, the corrosion inhibitor is nontoxic and harmless to the environment and organisms, and the development trend of the corrosion inhibitor is met.
In conclusion, the corrosion inhibitor prepared by compounding polyaspartic acid with sodium tungstate achieves a good corrosion inhibition effect on low alloy steel, and is an excellent environment-friendly compound corrosion inhibitor.
Drawings
FIG. 1 is a scanning electron microscope image of a low alloy steel bare chip before corrosion (A), a low alloy steel bare chip after corrosion (B), and a low alloy steel test piece after corrosion (C) with corrosion inhibitor added (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 150 mg/L).
FIG. 2 is an atomic force microscope image of a low alloy steel bare chip before corrosion (A), a low alloy steel bare chip after corrosion (B), and a low alloy steel test piece after corrosion (C) with a corrosion inhibitor added (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 150 mg/L).
FIG. 3 is an infrared spectrum of a low alloy steel directly soaked in natural seawater (A), and a low alloy steel added with polyaspartic acid compounded sodium tungstate corrosion inhibitor (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 150mg/L) and then soaked in natural seawater (B).
FIG. 4 is a polarization curve of a low alloy steel test piece in natural seawater without corrosion inhibitor and with a compound corrosion inhibitor (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 50-200 mg/L).
FIG. 5 is an impedance spectrum of a low alloy steel test piece in natural seawater without corrosion inhibitor and with a compound corrosion inhibitor (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 50-200 mg/L).
Detailed Description
The invention is further illustrated with reference to the following examples and figures, without thereby restricting the content of the invention.
Example 1
The preparation method of the polyaspartic acid compound sodium tungstate corrosion inhibitor specifically comprises the following steps:
(1) preparation of polyaspartic acid:
synthesis of polyaspartic anhydride: taking a certain amount of L-dayAspartic acid in a muffle furnace in a catalyst H3PO4Thermally polycondensing into polyaspartic anhydride (L-aspartic acid and catalyst H) under the action of3PO4The mass ratio of (2) is more than 1), the reaction time is 2h, the polymerization temperature is 240 ℃, the relative molecular mass of the polymer can be improved by using the catalyst in the reaction process, the color of the product is lightened, but great difficulty is caused to the separation and purification of the product, the production cost is also increased, and therefore, the dosage of the catalyst phosphoric acid needs to be properly controlled in the reaction process.
Synthesis of polyaspartic acid: using excessive sodium hydroxide to depolymerize aspartic anhydride to obtain a sodium polyaspartate solution; adjusting pH to 5 with hydrochloric acid, adding ethanol solution, and precipitating; and (5) carrying out suction filtration and drying to obtain a pure product of the polyaspartic acid.
(2) 1000ml of natural seawater is taken, 500mg of polyaspartic acid is added, sodium tungstate with different contents (namely 50mg/L, 100mg/L, 150mg/L and 200mg/L) is added into the solution, and the polyaspartic acid and the sodium tungstate are mixed and stirred uniformly to form corrosion inhibitor solutions with different mass concentrations.
Application example 1
The corrosion inhibition test of the polyaspartic acid compound sodium tungstate corrosion inhibitor obtained in example 1 is as follows:
(1) pretreatment of low alloy steel test pieces: the specification of the working electrode of the electrochemical experiment is 10mm multiplied by 10mm, the low alloy steel test piece is sealed by epoxy resin, and the exposed working area is 10mm multiplied by 10 mm. And (3) polishing the test piece by using No. 400-1200 abrasive paper, then washing the test piece by using deionized water, then ultrasonically cleaning the test piece by using absolute ethyl alcohol for 5min, then drying the test piece by using nitrogen, and finally storing the test piece in a dryer for later use.
(2) And soaking the treated electrode sample in solutions with different amounts of sodium tungstate added to form corrosion inhibitors and in blank solutions for 5 days or 8 days at the temperature of 303K for later use. Wherein the corrosion inhibition solution is prepared from natural seawater polyaspartic acid with a mass concentration of 500mg/L, and sodium tungstate with a mass concentration of 50mg/L, 100mg/L, 150mg/L and 200 mg/L.
After the corrosion inhibition treatment is carried out on the obtained low alloy steel test piece, surface analysis and electrochemical performance test are carried out, and the method specifically comprises the following steps:
1) the surface analysis method of the low alloy steel test piece comprises the following steps:
the treated low alloy steel (70mm multiplied by 20mm multiplied by 3mm) is immersed in natural seawater solution and natural seawater added with the compound corrosion inhibitor of polyaspartic acid and sodium tungstate for 1 h. The surface of the sample was examined by a Scanning Electron Microscope (SEM) model S-3400N (see FIGS. 1-3).
Fig. 1(a) is a scanning electron microscope picture of a low alloy steel bare chip before corrosion, and it can be seen that the surface is very flat, and the processing scratches are clear and complete. Fig. 1(B) is a scanning electron microscope image of the low alloy steel after being soaked in natural seawater for 8 days, and it can be seen from the image that the corrosion products on the surface are cluster-shaped, contain a part of micro-flower hierarchical structure, and are uneven. Fig. 1(C) is a scanning electron microscope picture of low alloy steel after being soaked in natural seawater added with polyaspartic acid and sodium tungstate compound corrosion inhibitor (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 150mg/L) for 8 days. Compared with the graph 1(B), the graph 1(C) can clearly see that a layer of granular or needle-shaped protective film uniformly covers the surface of the sample, so that the surface of the sample is still flat and is not corroded by corrosive particles, and the compound corrosion inhibitor plays a good protection role. The surface of the sample is detected by an Atomic Force Microscope (AFM), fig. 2(a) is an atomic force microscope picture of the low alloy steel bare chip before corrosion, fig. 2(B) is an atomic force microscope picture of the low alloy steel after being soaked in natural seawater for 8 days, and fig. 2 (C) is an atomic force microscope picture of the low alloy steel after being soaked in natural seawater added with a polyaspartic acid and sodium tungstate compounded corrosion inhibitor (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 150mg/L) for 8 days. The AFM topography shows that the surface roughness and the microstructure surface of the low alloy steel after being soaked in natural seawater for 8 days are deformed, have air holes and cracks and are relatively obviously changed, and the surface roughness and the microstructure change of the low alloy steel after being soaked in natural seawater added with a polyaspartic acid and sodium tungstate compound corrosion inhibitor (the mass concentration of the polyaspartic acid is 500mg/L and the mass concentration of the sodium tungstate is 150mg/L) for 8 days are relatively moreAnd small, the compound corrosion inhibitor of polyaspartic acid and sodium tungstate is proved to have good slow release effect. The sample surface was then further characterized by Fourier Infrared Spectroscopy (FTIR) using a Bruker Vertex 70FTIR detector with a resolution of 2cm-1. FIG. 3(A) is an IR spectrum of a low alloy steel after immersion in natural seawater for 8 days. FIG. 3B is an infrared spectrum of a low alloy steel soaked in polyaspartic acid-sodium tungstate corrosion inhibitor (the mass concentration of polyaspartic acid is 500mg/L, and the mass concentration of sodium tungstate is 150mg/L) in natural seawater for 8 days.
2) And (3) electrochemical performance testing: the test temperature is 303K by using a Gamry 3000 electrochemical system connected with a computer for detection. The test solutions with and without the addition of corrosion inhibitors were placed in 500m L glass beakers and the experiments were performed with a three-electrode system. In the three-electrode system, a saturated calomel electrode was used as a reference electrode, a platinum sheet electrode was used as an auxiliary electrode (counter electrode), and a working electrode was a low alloy steel sample having a size of 10mm × 10mm × 10 mm. Experiments were conducted with electrochemical alternating current impedance spectroscopy (EIS) at open circuit potential, setting the frequency range to 10 mhz to 100 khz, and the peak-to-peak amplitude of the alternating signal to 10 mV. The scan rate during the polarization curve test was 1m Vs-1, with a scan potential ranging from-250 mV to +250mV relative to the Open Circuit Potential (OCP) when the working electrode was at steady state (the floating range of open circuit potential was within 5 mV). The experiment was repeated three times for each experimental condition (see fig. 4 and 5).
FIG. 4 shows the polarization curve of low alloy steel after soaking in natural seawater for 8 days when the corrosion inhibitor contains polyaspartic acid and sodium tungstate at different mass concentration ratios. As can also be seen from the polarization curve in FIG. 4, the cathodic polarization and anodic polarization of the compounded polyaspartic acid and sodium tungstate are both inhibited, which indicates that the action mechanism of the compounded corrosion inhibitor on low alloy steel is a mixed corrosion inhibitor. Wherein sodium tungstate is a cathode corrosion inhibitor. Polyaspartic acid is an anode type corrosion inhibitor.
As can be seen from FIG. 4, when the polyaspartic acid and sodium tungstate compound corrosion inhibitor is added into the experimental solution, the anode current is reduced, which indicates that the corrosion inhibitor molecules can alleviate the corrosion of the sample and the anode reaction is betterThis behavior is due to the adsorption of corrosion inhibitor molecules to the active sites on the metal surface. When the corrosion inhibitor is 500mg/L PASP +150mg/L Na2WO4When the mass concentration of (i.e. PASP and Na) is proportioned2WO4The mass concentration ratio is 10: 3), and the corrosion current density reaches the lowest value. As can be seen, the corrosion inhibitors PASP and Na2WO4The compounding under the proper concentration proportion can generate 'synergistic effect', so that the corrosion inhibition effect is better than that of single use. The combination of organic adsorption corrosion inhibitor and inorganic oxidation corrosion inhibitor can generate better 'synergistic effect', and the combination of PASP and Na2WO4 belongs to the situation.
From the nyquist plot of the stainless steel after 8 days immersion in fig. 5, it can be seen that the impedance spectrum shows a squashed half-arc, and that the parameters of the half-arc increase as the corrosion inhibitor concentration increases. All impedance spectra show a single capacitive arc, which indicates that the charge transfer resistance controls the corrosion of stainless steel at corrosion potential, revealing the corrosion inhibition effect of the corrosion inhibitor during the corrosion of metal materials. When the corrosion inhibitor is PASP + Na2WO4When the corrosion inhibitor is mixed according to different mass concentrations, the impedance of each curve is higher than that of the curve without the corrosion inhibitor, so that the corrosion inhibitor plays a certain corrosion inhibition role on the low alloy steel, or the corrosion resistance of the low alloy steel is improved; increase Na2WO4When the concentration of the corrosion inhibitor reaches 150mg/L, the corresponding impedance value also obviously rises and reaches the maximum, which shows that the corrosion inhibition effect is the best at the moment, and the corrosion resistance of the low alloy steel is the best; continuously increase Na2WO4When the concentration is 200mg/L, the impedance value is reduced; i.e., the corrosion resistance of the low alloy steel, which may be caused by the concentration limit phenomenon of the corrosion inhibitor.
The polyaspartic acid compound sodium tungstate corrosion inhibitor is low in preparation cost, green and pollution-free, can be quickly adsorbed on the surface of low alloy steel so as to weaken corrosion and oxygen absorption reaction on the surface of the material, has an obvious corrosion inhibition effect on corrosion of the low alloy steel in natural seawater, and provides a direction for protecting metal materials by an environment-friendly corrosion inhibitor.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (5)
1. A compound corrosion inhibitor suitable for low alloy steel is characterized in that: the effective components of the corrosion inhibitor are polyaspartic acid and sodium tungstate, and the mass concentration ratio is that the polyaspartic acid: sodium tungstate 10: (1-4).
2. The environment-friendly compound corrosion inhibitor as claimed in claim 1, characterized in that: the effective components of the corrosion inhibitor are polyaspartic acid and sodium tungstate, and the mass concentration ratio is that the polyaspartic acid: sodium tungstate 10: 3.
3. the environment-friendly compound corrosion inhibitor as claimed in claim 1 or 2, which is characterized in that: the polyaspartic acid is prepared from L-aspartic acid as a raw material by reacting the L-aspartic acid with a catalyst H3PO4Under the action of the reaction, the mixture is thermally shrunk and reacted for 2 to 3 hours at the temperature of 200-260 ℃ to generate Polysuccinimide (PSI), and then the polysuccinimide is hydrolyzed under the alkaline condition to obtain the polyaspartic acid.
4. The environment-friendly compound corrosion inhibitor as claimed in claim 1 or 2, which is characterized in that: the corrosion inhibitor is prepared by adding effective components into natural seawater; wherein the mass concentration of the polyaspartic acid is 500mg/L, and the mass concentration of the sodium tungstate is 50-200 mg/L.
5. The use of the compound corrosion inhibitor for low alloy steel according to claim 1, wherein the corrosion inhibitor comprises the following components in percentage by weight: the corrosion inhibitor is applied to low alloy steel compound corrosion inhibitors in marine environment.
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