CN115125540A - Carbon steel pickling inhibitor based on 5-hydroxymethylfurfural modified chitosan - Google Patents
Carbon steel pickling inhibitor based on 5-hydroxymethylfurfural modified chitosan Download PDFInfo
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- 239000010962 carbon steel Substances 0.000 title claims abstract description 44
- 238000005554 pickling Methods 0.000 title claims abstract description 30
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 title claims abstract description 23
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
- C23G1/068—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors compounds containing a C=C bond
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
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Abstract
The invention relates to the field of corrosion inhibitors, in particular to a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural modified chitosan. The invention discloses a carbon steel pickling inhibitor of 5-hydroxymethylfurfural modified chitosan, the optimal dosage of which is 400mg/L, and the corrosion resistance of the carbon steel pickling inhibitor is tested by an electrochemical method and a weight loss method. The raw materials of the corrosion inhibitor are simple and easy to obtain, the price is low, compared with the organic corrosion inhibitor, the corrosion inhibitor is low in toxicity and harmless, and the development trend of the environment-friendly corrosion inhibitor is met. The chitosan Schiff base corrosion inhibitor has strong continuous action capability and good corrosion inhibition performance, can meet the requirement of carbon steel corrosion inhibition in 1mol/L hydrochloric acid solution, can avoid the problem of environmental pollution caused by the existing organic corrosion inhibitor, and has wide market application prospect.
Description
Technical Field
The invention relates to the field of corrosion inhibitors, in particular to a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural modified chitosan.
Background
Carbon steel is the most widely used metal material in industrial and agricultural production and human life (Zhang, W., et al. carbohydrate Polymers 2020,238,116216; Obot, I.B., et al. journal of Molecular Liquids 2109,277,749). However, in the related chemical industrial processes of acid cleaning and descaling, oil well acidification, seawater desalination and the like, carbon steel can be in contact with aggressive media to generate serious corrosion, so that huge economic loss and resource waste are caused, and even the life safety of people is endangered. Therefore, the corrosion protection work is well done, and the social and economic problems of protecting the environment, saving resources, implementing the strategy of sustainable development and the like are concerned. The corrosion inhibitor added in various corrosion prevention means has the advantages of convenient operation, low investment, strong practicability and the like, and is widely applied in the field of metal corrosion protection. In particular, organic corrosion inhibitors containing N, O, S and other heteroatoms and pi-bonds provide lone pair electrons to the metal surface, and thus have good corrosion resistance (Sareni, M., et al Corroson Science 2006,48, 1404; Gao, Y., et al desalinization 2015,365,220; Wang, C., et al. journal of Cleaner Production 2019,238,117823), but are gradually prohibited from use due to their toxic properties to the environment and organisms. Based on the requirements of strategy of environmental protection and sustainable development, the preparation of high-efficiency, cheap and environment-friendly corrosion inhibitors becomes a urgent priority.
Natural Polymers are matched with natural ecosystems, have wide sources and low cost, can be directly discharged without polluting the environment, and become a hotspot of research on green corrosion inhibitors (Zhang, W., et al. carbohydrate Polymers 2021,260,117842; Solomon, M.M.et al. ACS Applied Materials)&Interfaces 2018,10, 28112). Chitosan and its derivatives can be regarded as an attractive alternative to organic corrosion inhibitors, which can be formed by-OH and-NH groups on the chitosan chain 2 The groups are chelated with metal ions, so that the metal ions are more easily adsorbed on the metal surface, and active corrosion sites are inhibited. However, at present, the corrosion inhibition mechanism of the chitosan polymer as carbon steel in an acidic medium is rarely researched, and the influence of the formation of the expanded chitosan schiff base and the description of reaction parameters (such as the change of the molar ratio of reactants) on corrosion application is hardly expanded. In view of the above, the invention uses chitosan and 5-hydroxymethylfurfural as monomers, and realizes the regulation of the number of adsorption sites on a molecular level by changing the degree of substitution, thereby synthesizing the efficient and environment-friendly 5-hydroxymethylfurfural-chitosan schiff base corrosion inhibitor.
The invention is helpful for better understanding the molecular influence controlled by the structural unit and provides a new idea for the design of the novel chitosan Schiff base carbon steel pickling corrosion inhibitor.
Disclosure of Invention
1. Object of the invention
The invention provides a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan Schiff base, which can effectively reduce the corrosion of carbon steel in an acid solution. Meanwhile, the problems of high toxicity, complex process, easy secondary pollution to the environment and the like of the existing corrosion inhibitor are solved.
2. The technical scheme adopted by the invention
The technical principle of the invention is as follows: according to the invention, chitosan (preferably purified chitosan) and 5-hydroxymethylfurfural are used as monomers, 5-hydroxymethylfurfural-chitosan Schiff bases with different degrees of substitution are prepared by adding 5-hydroxymethylfurfural with different molar ratios, and the structure of the 5-hydroxymethylfurfural-chitosan Schiff base is shown in figure 1.
Preferably, the 5-hydroxymethylfurfural-chitosan with different substitution degrees is prepared by mixing chitosan and 5-hydroxymethylfurfural according to a molar ratio of 1: 1-1: 3, more preferably 1:1, 1:2 or 1:3, most preferably 1: 3.
Preferably, the concentration of the 5-hydroxymethylfurfural-chitosan Schiff base in the carbon steel pickling corrosion inhibitor is 100mg/L-400mg/L, and more preferably 300-400 mg/L.
Preferably, the pickling solution in the carbon steel pickling corrosion inhibitor is 1mol/L HCl aqueous solution.
Preferably, the carbon steel pickling corrosion inhibitor is used as a corrosion inhibitor in a medium-high temperature acidic medium, wherein the medium-high temperature is 20-55 ℃, and the further preferable temperature is 20-35 ℃.
Preferably, the 5-hydroxymethylfurfural-chitosan schiff base is prepared by the following method:
(1) preparation: purified chitosan (mw ═ 50,000-. Then, 5-hydroxymethylfurfural (Chi-Cn1 is 0.73 mL; 2.19mL is used for Chi-Cn3) dissolved in ethanol at different molar ratios is poured into the chitosan solution and kept for 6h at 50 ℃; formation of a dark yellow gel was observed confirming the formation of the chitosan polymer.
(2) And (3) post-treatment: and precipitating the obtained product by using a 5 wt% sodium hydroxide aqueous solution, filtering, and washing by using distilled water and ethanol to remove unreacted 5-hydroxymethylfurfural to obtain the 5-hydroxymethylfurfural-chitosan Schiff base.
According to another aspect of the invention, the invention provides a method for evaluating the corrosion inhibition performance of a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan schiff base, which comprises the following steps:
(1) 5-hydroxymethylfurfural with different molar ratios reacts with Mannich base of chitosan to obtain the 5-hydroxymethylfurfural-chitosan Schiff base corrosion inhibitor with different degrees of substitution.
(2) And (2) weighing 10-40 mg of the chitosan Schiff base corrosion inhibitor obtained in the step (1), fully dissolving the chitosan Schiff base corrosion inhibitor in the pickling solution, and then diluting to 100mL to obtain the test solution.
(3) At room temperature, a carbon steel sample with an exposed surface area of 0.5cm2 is used as a working electrode, Tafel polarization curves and alternating current impedance data of the carbon steel electrode in hydrochloric acid solution before and after the corrosion inhibitor is added are measured, and the corrosion inhibition performance of the chitosan Schiff base corrosion inhibitor with different degrees of substitution is evaluated;
(4) performing a weight loss coupon experiment in the corrosion solution prepared in the step (2) at the temperature of 20-55 ℃ to evaluate corrosion inhibition performance;
preferably, the acid wash solution is 1mol/L aqueous HCl.
Further, the temperature is room temperature (30 ℃), and a weight loss and electrochemical experiment is carried out by adopting a static method.
According to a third aspect of the invention, the invention provides an application method of a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan Schiff base, which is used for inhibiting corrosion of a hydrochloric acid pickling solution at a certain temperature.
Preferably, the certain temperature is 20 to 55 ℃, and more preferably 25 to 35 ℃.
Compared with the prior art, the invention has the following positive beneficial effects
(1) The invention selects natural polysaccharide as the green corrosion inhibitor, designs a one-step chemical modification route, realizes the regulation and control of the number of adsorption sites on a molecular level, meets the economic synthesis concept of steps, and provides a feasible new method for preparing the efficient green corrosion inhibitor.
(2) The corrosion inhibitor is used for cleaning carbon steel and products thereof, can effectively inhibit harmful corrosion of a metal matrix in acid and excessive consumption of acid liquor, has the outstanding advantages of low consumption, environmental protection and strong continuous action capability compared with the current common corrosion inhibitor, and can be repeatedly used.
Drawings
Fig. 1 is a scheme diagram of synthesis of 5-hydroxymethylfurfural-chitosan schiff base.
FIG. 2 is a plot of Tafel polarization curves for carbon steel in example 2 in 1M HCl solution without and with added corrosion inhibitor.
FIG. 3 is a Nyquist impedance plot of carbon steel in example 2 in 1M HCl solution without and with the addition of a corrosion inhibitor.
Detailed Description
5-hydroxymethylfurfural-chitosan schiff base with different degrees of substitution is prepared according to the following method:
(1) preparation: purified chitosan (mw: 50,000-190,000; 85% deacetylation) was mixed in 50ml of 2V% acetic acid aqueous solution, and stirred at 30 ℃ for 6h to obtain a transparent, homogeneous viscous solution. Then, 5-hydroxymethylfurfural dissolved in ethanol in different molar ratios is poured into the chitosan solution and kept at 50 ℃ for 6 hours; formation of a dark yellow gel was observed confirming the formation of the chitosan polymer.
(2) And (3) post-treatment: and precipitating the obtained product by using a 5 wt% sodium hydroxide aqueous solution, filtering, and washing by using distilled water and ethanol to remove unreacted 5-hydroxymethylfurfural to obtain the 5-hydroxymethylfurfural-chitosan Schiff base.
Example 1
(1) Chitosan schiff base corrosion inhibitor test solutions with different substitution degrees and the concentrations of 100mg/L, 200mg/L, 300mg/L and 400mg/L are respectively prepared by using 1M HCl aqueous solution.
(2) The exposed area is 0.5cm 2 The carbon steel bar is used as a working electrode, the saturated calomel electrode is used as a reference electrode, the platinum sheet electrode is used as a counter electrode, and a CHI760e electrochemical workstation is used for measuring Tafel polarization curves of carbon steel electrodes containing corrosion inhibitors with different concentrations in 1M HCl aqueous solution: the scanning speed is 1mV/s, and the scanning interval is-750 mV to-250 mV.
FIG. 2 is a plot of Tafel polarization curves for carbon steel in example 1 in 1M HCl solution with no corrosion inhibitor added. As can be seen from the electrochemical corrosion characteristic study in FIG. 2, the corrosion inhibition efficiency increases with the increase of the concentration of the corrosion inhibitor, and after the concentration exceeds 300mg/L, the corrosion inhibition efficiency does not increase obviously, and the concentration is not suitable to be increased. In addition, the larger the polymerization degree of the chitosan Schiff base corrosion inhibitor is, the stronger the corrosion inhibition capability is.
Wherein Chi-Cn1 means that the molar ratio of chitosan to 5-hydroxymethylfurfural is 1:1, obtaining the chitosan Schiff base corrosion inhibitor; Chi-Cn3 means that the molar ratio of chitosan to 5-hydroxymethylfurfural is 1:3, obtaining the chitosan Schiff base corrosion inhibitor.
Example 2
(1) Test solutions were prepared with 1M HCl at concentrations of 100mg/L, 200mg/L, 300mg/L, and 400mg/L, respectively.
(2) The exposed area is 0.5cm 2 The carbon steel bar is used as a working electrode, the saturated calomel electrode is used as a reference electrode, the platinum sheet electrode is used as a counter electrode, and an electrochemical impedance spectrum of the carbon steel electrode containing corrosion inhibitors with different concentrations in 1M HCl is measured by using a CHI760e electrochemical workstation: the frequency range is 100000Hz-0.05Hz and the amplitude is 5 mV.
FIG. 3 is a graph of the electrochemical impedance of carbon steel in example 2 in 1M HCl solution without and with the addition of corrosion inhibitors. It can be seen from fig. 3 that after the corrosion inhibitor is added, the diameter of the impedance arc is obviously larger than that of the blank HCl solution, and the molar ratio of chitosan to 5-hydroxymethylfurfural is 1:3 the larger the impedance arc diameter of the obtained chitosan schiff base. The corrosion inhibition efficiency obtained by the impedance method is 97.13 percent, is consistent with the corrosion inhibition efficiency (96.94 percent) obtained by a polarization curve, and both prove the good corrosion inhibition capability of the chitosan Schiff base corrosion inhibitor.
Example 3
(1) 100mL of Chi-Cn3 test solution with a concentration of 400mg/L was prepared with 1M aqueous HCl. Fixing a 5cm x 5cm carbon steel sheet on a hanging piece instrument at the temperature of 25-55 ℃, completely immersing the steel sheet in an experimental solution, rotating at the rotating speed of 75rpm for 48 hours, and recording the weight of the test piece before and after the experiment.
(2) According to the formula: v ═ w 1 -w 2 ) /(s × t) calculating the corrosion efficiency, where w 1 And w 2 (mg) is the weight loss of the sample before and after soaking, s (cm) -2 ) Is the area of the steel sample, and t (h) is the soaking time; eta w ＝(v 0 -v)/v 0 Calculating the efficiency of corrosion inhibition, wherein v and v 0 The corrosion rates without and with corrosion inhibitor, respectively.
The corrosion inhibition efficiency of the corrosion inhibitor obtained by the weight loss method in example 3 at different temperatures is shown in table 1.
TABLE 1.400 mg/L results of corrosion inhibition efficiency of Chi-Cn3 at various temperatures
| T(K) | v HCl (mg cm -2 h -1 ) | v Chi-Cn3 (mg cm -2 h -1 ) | η z (％) |
| 25℃ | 11.62 | 0.46 | 96.04 |
| 35℃ | 15.28 | 1.02 | 93.32 |
| 45℃ | 21.95 | 2.31 | 89.48 |
| 55℃ | 31.39 | 4.57 | 85.44 |
In table 1, the v-values for carbon steel in both the non-inhibiting and inhibiting solutions increased with increasing temperature. This may be due to the fact that, at higher temperatures, the molecules of the corrosion inhibitor desorb at a rate greater than the adsorption rate in the corrosive medium and do not readily adhere to the steel surface. Namely, the chitosan Schiff base is a temperature-dependent corrosion inhibitor and can be used as a corrosion inhibitor of a medium-temperature HCl medium.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan Schiff base is characterized in that: the 5-hydroxymethylfurfural-chitosan Schiff base is prepared by the following method: the 5-hydroxymethylfurfural-chitosan Schiff base with different degrees of substitution is prepared by taking chitosan and 5-hydroxymethylfurfural as monomers and adding 5-hydroxymethylfurfural with different molar ratios.
2. The carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan schiff base of claim 1, characterized in that: the 5-hydroxymethylfurfural-chitosan with different substitution degrees is prepared by respectively mixing chitosan and 5-hydroxymethylfurfural according to the molar ratio of 1: 1-1: 3 is obtained by Mannich base reaction.
3. The carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan schiff base of claim 2, characterized in that: the 5-hydroxymethylfurfural-chitosan is prepared by respectively mixing chitosan and 5-hydroxymethylfurfural according to a molar ratio of 1:3 is obtained by Mannich base reaction.
4. The carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan schiff base as claimed in any one of claims 1 to 3, wherein: the concentration of the 5-hydroxymethylfurfural-chitosan Schiff base in the carbon steel pickling corrosion inhibitor is 100mg/L-400mg/L, and more preferably 300-400 mg/L.
5. The carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan schiff base as claimed in any one of claims 1 to 3, wherein: the pickling solution in the carbon steel pickling corrosion inhibitor is 1mol/L HCl aqueous solution.
6. The carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan schiff base as claimed in any one of claims 1 to 3, wherein: the carbon steel pickling corrosion inhibitor is used as a corrosion inhibitor in a medium-high temperature acid medium, wherein the medium-high temperature is 20-55 ℃, and the preferable temperature is 20-35 ℃.
7. A method for evaluating the corrosion inhibition performance of a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan Schiff base comprises the following steps:
(1) reacting 5-hydroxymethylfurfural with different molar ratios with Mannich base of chitosan to obtain 5-hydroxymethylfurfural-chitosan Schiff base corrosion inhibitors with different degrees of substitution;
(2) weighing 10-40 mg of the chitosan Schiff base corrosion inhibitor obtained in the step (1), fully dissolving the chitosan Schiff base corrosion inhibitor in a pickling solution, and then performing constant volume treatment to 100mL to obtain a test solution;
(3) at room temperature, with an exposed surface area of0.5cm 2 The carbon steel sample is used as a working electrode, Tafel polarization curve and alternating current impedance data of the carbon steel electrode in hydrochloric acid solution before and after the corrosion inhibitor is added are measured, and the corrosion inhibition performance of the chitosan Schiff base corrosion inhibitor with different degrees of substitution is evaluated;
(4) and (3) performing a weight loss coupon experiment in the corrosion solution prepared in the step (2) at the temperature of 20-55 ℃ to evaluate corrosion inhibition performance.
8. The method of claim 7, wherein: the acid washing solution is 1mol/L HCl aqueous solution.
9. The method of claim 7, wherein: the temperature is room temperature (30 ℃), and a weight loss and electrochemical experiment is carried out by adopting a static method.
10. An application method of a carbon steel pickling corrosion inhibitor based on 5-hydroxymethylfurfural-chitosan Schiff base is used for inhibiting corrosion of a hydrochloric acid pickling solution at a certain temperature; the 5-hydroxymethylfurfural-chitosan is prepared by respectively mixing chitosan and 5-hydroxymethylfurfural according to the molar ratio of 1:3, performing Mannich base reaction to obtain the product; the certain temperature is 25-35 ℃.
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| CN112915103A (en) * | 2021-01-27 | 2021-06-08 | 仲恺农业工程学院 | Vanillin modified chitosan Schiff base chelated zinc sustained release agent as well as preparation method and application thereof |
| CN113549922A (en) * | 2021-07-21 | 2021-10-26 | 曲阜师范大学 | Carbon steel pickling corrosion inhibitor based on resveratrol |
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| CN112915103A (en) * | 2021-01-27 | 2021-06-08 | 仲恺农业工程学院 | Vanillin modified chitosan Schiff base chelated zinc sustained release agent as well as preparation method and application thereof |
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