CN113804613A - Test method for simulating corrosion of iron bacteria in water environment - Google Patents
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Abstract
A test method for simulating the corrosion of iron bacteria in a water environment comprises the following steps: 1) preparing a simulated microbial film by taking a natural high polymer material as a film forming matter, wherein the simulated microbial film is divided into two layers, one layer is a composite high polymer film and contains a corrosion product mimic, and the composite high polymer film is coated on the surface of a steel matrix; the other layer is a pure polymer film without a compound and is coated on the surface of the compound polymer film; the simulated microbial film prevents the escape of corrosion product mimics into an aqueous environment, while its porosity ensures the transport of oxygen within the film. 2) The sample coated with the simulated microbial film is placed in a container containing a soluble ferric salt and H2O2In the test solution of (1), Fe3+And H2O2The pure polymer film and the composite polymer film are diffused to the steel matrix to form an oxidizing environment, so that the corrosion process of the steel matrix is promoted. The method can accurately control various corrosion factors in the iron bacteria (IOB) corrosion process without complicated and time-consuming microbial culture process.
Description
Technical Field
The invention relates to the field of corrosivity, in particular to a test method for carrying out laboratory simulation on a corrosion process of iron bacteria in a water environment.
Background
Microbial corrosion (MIC) is a corrosion process occurring with the participation of microbial life activities, and the process widely exists in the fields of petroleum industry, marine equipment, fluid transportation, water treatment and the like, and the problem of corrosion failure caused by the process is increasingly emphasized in the fields of engineering and research. Because factors influencing the microbial corrosion process in the actual environment are complex and changeable and are difficult to control and quantitatively describe, the experimental method for simulating the biological environment has important significance for evaluating the biological factors in the seawater corrosion of the material and revealing the rule of the biological corrosion.
Among various microorganisms associated with corrosion, iron bacteria (IOB) is an important one. Previous studies have shown that IOB gains energy by oxidizing ferrous iron to ferric iron, which is usually present as an insoluble compound. The IOB corrosion process works over a large area of oxygen concentration and small anodic spots on metal surfaces as well as over a large area of cathodic sites. At present, the conventional method for simulating the microbial corrosion process is to culture selected microorganisms to form a specific microbial corrosion environment, and then place the sample in the environment for corrosion simulation. The method of soaking the sample in the liquid culture medium containing bacteria can be used for measuring and calculating the corrosion rate and electrochemical research (YaoRong, Zusanli, Qinqing, etc., corrosion and protection 2016, 37 (3): 206-. However, the above method is not applicable when in situ observation of the etching process is required. Patent CN 2844899Y reports an experimental device for simulating the generation of microorganism/macromolecular membrane, which is provided with a sealable flow cell with a circulating liquid inlet and outlet for simulating the microbial corrosion environment, and can make microorganisms form microorganism membranes in different forms such as 'conditioned membrane', 'monolayer membrane', 'mature membrane' and the like on the surface of a sample by controlling the flow rate of the simulating liquid; the flow cell sealed bin is covered with a probe and a scanning measurement system for real-time image pickup and online microscopic observation. Patent CN 101226136B discloses a microbial corrosion method of magnesium alloy based on solid culture medium, which relates to the simulation of bacterial corrosion process. The method comprises the specific steps of sample processing and sterilization, solid culture medium preparation and sterilization, bacteria culture and activation, and constant temperature corrosion on the surface of the sample by using a bacteria-carrying culture medium. The method overcomes the defect that the microbial corrosion process is difficult to observe in situ in the liquid corrosion medium soaking method, is relatively simple in implementation process, has low requirement on sample surface treatment, and is convenient for in situ observation of the corrosion process. However, neither the method using a liquid culture medium nor the method using a solid culture medium can achieve accelerated simulation of the microbial corrosion process, and thus cannot be used for rapid evaluation of the microbial corrosion resistance of a material, because the amount of nutrients for growth of microorganisms in the culture medium or the culture solution is fixed, and therefore the number of microorganisms contained in the culture medium or the culture solution is constant, and as the nutrients are consumed, the number of microorganisms inevitably undergoes a process from increase to decay, and the metabolic process inevitably undergoes a process from vigorous to stagnant, which means that the concentrations of metabolites and corrosion products at the surface of a sample are uncontrollable and cannot be maintained at high levels all times, and thus the corrosion process cannot be accelerated simulation from the viewpoint of the corrosion mechanism of the metabolites and the corrosion mechanism of the corrosion products. In addition, sterilization, biochemical culture equipment and various auxiliary devices are required to be arranged for culturing the microorganisms in the laboratory, and the process is complicated and takes long time. Because factors influencing the microbial corrosion process in the real marine environment are complex and changeable, and the microbial culture process in a laboratory is tedious and time-consuming, a method for simulating a microbial film is adopted in some microbial corrosion researches. For example, sodium alginate gel is deposited on the surface of a metal material to form a simulated microbial film, and the electrochemical behavior of the metal material is researched in simulated seawater (Wang Qingfei, Suizhi, Wan Xiao shan et al, journal of chemical engineering 2001, 52 (9): 814-. However, this method cannot simulate the influence of corrosion products and metabolites, and does not take into account the influence of the microbial membrane ocean environment.
Disclosure of Invention
The invention aims to provide a test method for simulating iron bacteria corrosion in a water environment, which can accurately control various corrosion factors in the iron bacteria (IOB) corrosion process without performing a complicated and time-consuming microbial culture process.
A test method for simulating the corrosion of iron bacteria in a water environment comprises the following steps:
1) preparing a simulated microbial film by taking a natural high polymer material as a film forming matter, wherein the simulated microbial film is divided into two layers, one layer is a composite high polymer film and contains a corrosion product mimic, and the composite high polymer film is coated on the surface of a steel matrix; the other layer is a pure polymer film without a compound and is coated on the surface of the compound polymer film; the simulated microbial film prevents the escape of corrosion product mimics into an aqueous environment, while its porosity ensures the transport of oxygen within the film.
2) The sample coated with the simulated microbial film is placed in a container containing a soluble ferric salt and H2O2In the test solution of (1), Fe3+And H2O2The pure polymer film and the composite polymer film are diffused to the steel matrix to form an oxidizing environment, so that the corrosion process of the steel matrix is promoted.
The natural polymer material is Sodium Alginate (SA). When SA is used as a film forming material, SA is prepared into a water solution with a certain concentration, the SA solution is spread to form a film, and then a calcium chloride water solution is used as a gelling agent to gel an SA liquid film to prepare the SA gel film. The concentration of the SA solution and the concentration of calcium chloride in the gelling agent are the main factors determining the performance of the SA gel membrane. If the concentration of SA and calcium chloride is too low, the strength and water resistance of the gel film are poor, and if the concentration is too high, the toughness of the gel film is poor.
The preparation method of the pure polymer film comprises the following steps: firstly, preparing sodium alginate into aqueous solution, extending the aqueous solution of sodium alginate into a film, and then using the aqueous solution of calcium chloride as a gelling agent to gelatinize the liquid film of sodium alginate to prepare the sodium alginate gel film.
The concentration of the sodium alginate aqueous solution is 3 to 6 weight percent; the concentration of calcium chloride in the gel is 4-8 wt%.
The corrosion product mimic is Fe (OH)3。Fe(OH)3Is the reaction of IOB with Fe2+Oxidation to Fe3+The latter main product.
The preparation method of the composite polymer film comprises the following steps: mixing Fe (OH)3Mixing with sodium alginate aqueous solution to obtain mixed solution, coating the mixed solution on the surface of steel substrate to obtain wet film, and gelatinizing the wet film with gelling agent to obtain the final product containing Fe (OH)3The composite sodium alginate gel membrane (composite polymer membrane) of (1).
Fe (OH) in the mixed solution3The content of (A) is 0.1 mol/L-0.5 mol/L; the concentration of the sodium alginate aqueous solution is 3 to 6 weight percent; the gelling agent is calcium chloride aqueous solution with the concentration of 4-8 wt%.
The test solution is an aqueous solution containing soluble ferric iron salt and H2O2。
The soluble ferric salt in the test solution is selected from ferric chloride or ferric sulfate.
Fe in test solution3+The concentration is 0.02 mol/L-0.1 mol/L, H2O2The concentration is 0.05 mmol/L-0.8 mmol/L.
Preparing a pure SA gel film (a pure polymer film) on the composite SA gel film (a composite polymer film), and sequentially preparing two gel films on the surface of the steel substrate to enrich the corrosion product mimic Fe (OH)3The purpose of (1). Fe ionized from soluble ferric salts3+And H2O2Decomposed O2The sodium alginate gel film is diffused to the surface of the steel matrix to form an oxidizing environment, so that the corrosion of the steel matrix is promoted.
Compared with the prior art, the invention has the beneficial effects that:
the traditional microbial corrosion research method needs microbial culture with a complicated process, and cannot control the concentration values of microbial metabolites and corrosion products, so that the microbial corrosion process cannot be accelerated and simulated, and the method cannot be effectively used for deep research on the microbial corrosion mechanism.
The test method of the invention does not need to carry out a tedious and time-consuming microbial culture process. Therefore, the test method can simply and conveniently realize the simulation of the IOB corrosion process under the action of multiple factors in the water environment and the rapid evaluation of the IOB corrosion resistance of the metal material, and the use time can be shortened from 14 days of the traditional method to 1 day. In addition, the test method can accurately control various corrosion factors in the corrosion process of iron bacteria (IOB), thereby facilitating the realization of in-situ observation of the corrosion process.
Drawings
FIG. 1 is a schematic diagram of the experimental method of the present invention for simulating the corrosion of iron bacteria in an aqueous environment.
In the figure: 1-a steel matrix; 2-is a composite SA gel film; 3-is a pure SA gel film; 4-is the test solution.
Detailed Description
The following examples are intended to illustrate the invention in detail, and are intended to be a general description of the invention, and not to limit the invention.
In the case of no particular requirements on the specimen geometry, the specimen dimensions are preferably 50mm by 25mm by 5mm, with a hole of 5mm diameter drilled at the tip for suspending the specimen. When weightlessness corrosion test is carried out, at least 3 parallel samples should be used for each group of samples. Degreasing the surface of the sample by using an organic solvent such as a metal degreasing agent or acetone; the degreased and rinsed sample was immediately poured into absolute ethanol, taken out, blown dry and placed in a desiccator for use. Before the test sample is used, the mass is weighed and the size is measured, the mass is accurate to 0.001g, and the size is accurate to 0.1 mm.
The test solution is an aqueous solution simulating the service environment of the material. The amount of test solution should be greater than 20ml/cm2(sample surface area). The simulation of the temperature and the flow rate of the test solution is realized by a rotary coupon corrosion tester which is provided with a water bath heating tank, a sample is suspended on a sample rack with adjustable rotating speed, and the simulation is carried outThe flow speed of the seawater is 0-6 m/s.
The preparation method of the pure SA solution comprises the steps of adding SA into deionized water at 60 ℃, stirring to dissolve the SA, standing to remove bubbles for later use. Composite SA solution composed of Fe (OH)3Powder and SA solution. The preparation method of the composite SA solution comprises the following steps: mixing Fe (OH)3Adding the powder into SA solution, dispersing for 15min with high-speed dispersing homogenizer, treating for 5min in ultrasonic cleaning machine for 6 cycles.
The preparation method of the simulated microbial membrane comprises the following steps: a wire rod coater or a film coater which meets the national standard GB/T1727 is adopted to coat a composite SA solution film with the thickness of 200 mu m on the surface of a sample, a gelling agent is sprayed on the surface of the liquid film to enable the composite SA solution film to gel, and a plurality of layers of composite SA gel films can be prepared on the gelled composite SA film by adopting the same method according to the research requirement. On the surface of the composite SA gel film, several layers of pure SA gel films were prepared using the method described above. The pure SA gel film and the composite SA gel film jointly form a simulated microbial film.
Example 1:
weightlessness-method-based evaluation of IOB corrosion resistance of steel material
The SA solution concentration was 3 wt%. Fe (OH) in composite SA solution3The addition amount of (A) is 0.5 mol/L; when the simulated microbial film is prepared, CaCl in the gel2The concentration was 8 wt%. Preparing 3 layers of composite sodium alginate gel films on a steel matrix, and preparing 5 layers of pure sodium alginate gel films on the surfaces of the composite sodium alginate gel films.
The test solution was a 3.5 wt% NaCl aqueous solution to which ferric chloride and H were added2O2，Fe3+Concentration of 0.2mol/L, H2O2The concentration is 0.05 mmol/L; the flow velocity of the simulated seawater is 5m/s, and the temperature is 25 ℃.
Fe in the test solution after immersion of the test specimen in the test solution3+And H2O2Decomposed O2The pure SA gel film and the composite SA gel film are diffused to the steel matrix and participate in the corrosion process of the steel matrix together.
The samples were soaked in simulated seawater for 72h (simulated seawater was changed every 24 h). After the test is finished, the surface corrosion product and the morphology of the sample can be researched, the surface corrosion product of the sample can also be cleaned according to the national standard GB/T16545-.
Example 2:
electrochemical research on corrosion process of iron and steel material IOB
The SA solution concentration was 3 wt%. Fe (OH) in composite SA solution3The amount of (B) was 0.3 mol/L. When the simulated microbial film is prepared, CaCl in the gel2The concentration was 6 wt%. Preparing 2 layers of composite sodium alginate gel films on a steel matrix, and preparing 3 layers of pure sodium alginate gel films on the surfaces of the composite sodium alginate gel films.
The test solution was deionized water to which ferric sulfate and H were added2O2，Fe3+Concentration of 0.1mol/L, H2O2The concentration was 0.4 mmol/L. And taking the sample as a working electrode and the test solution as electrolyte, and performing electrochemical impedance test by adopting an electrochemical workstation. The test temperature was 25 ℃ and the sweep range was 10-2-105Hz, sine wave potential amplitude of 20 mV.
Although the present invention has been specifically described with reference to the parameters such as reagent concentration, test conditions, etc., the present invention is not limited to the above embodiments, which are not intended to be limiting, and those skilled in the art can make various modifications without departing from the spirit and scope of the present invention, which should not be excluded from the scope of the present invention.
Claims (10)
1. A test method for simulating the corrosion of iron bacteria in a water environment is characterized by comprising the following steps:
1) preparing a simulated microbial film by taking a natural high polymer material as a film forming matter, wherein the simulated microbial film is divided into two layers, one layer is a composite high polymer film and contains a corrosion product mimic, and the composite high polymer film is coated on the surface of a steel matrix; the other layer is a pure polymer film coated on the surface of the composite polymer film;
2) the sample coated with the simulated microbial film is placed in a container containing a soluble ferric salt and H2O2In the test solution of (1), Fe3+And H2O2The pure polymer film and the composite polymer film are diffused to the steel matrix to form an oxidizing environment, so that the corrosion process of the steel matrix is promoted.
2. The test method for simulating the corrosion of iron bacteria in an aqueous environment according to claim 1, wherein the natural polymer material is sodium alginate.
3. The test method for simulating the corrosion of iron bacteria in the water environment according to claim 1 or 2, wherein the pure polymer film is prepared by the following steps: firstly, preparing sodium alginate into aqueous solution, extending the aqueous solution of sodium alginate into a film, and then using the aqueous solution of calcium chloride as a gelling agent to gelatinize the liquid film of sodium alginate to prepare the sodium alginate gel film.
4. The test method for simulating the corrosion of iron bacteria in the water environment according to claim 3, wherein the concentration of the sodium alginate aqueous solution is 3-6 wt%; the concentration of calcium chloride in the gel is 4-8 wt%.
5. The assay of claim 1, wherein the corrosion product mimic is Fe (OH)3。
6. The test method for simulating the corrosion of iron bacteria in the water environment according to claim 1, wherein the preparation method of the composite polymer film comprises the following steps: mixing Fe (OH)3Mixing with sodium alginate aqueous solution to obtain mixed solution, coating the mixed solution on the surface of steel substrate to obtain wet film, and gelatinizing the wet film with gelling agent to obtain the final product containing Fe (OH)3The composite sodium alginate gel film.
7. The method of claim 6, wherein the mixture contains Fe (OH)3The content of (A) is 0.1 mol/L-0.5 mol/L; the concentration of the sodium alginate aqueous solution is 3 to 6 weight percent; the gelling agent is calcium chloride aqueous solution with the concentration of 4-8 wt%.
8. The method as claimed in claim 1, wherein the test solution is an aqueous solution.
9. The test method for simulating the corrosion of iron bacteria in the water environment according to claim 1 or 8, wherein the soluble ferric salt in the test solution is selected from one of ferric chloride and ferric sulfate.
10. The method as claimed in claim 9, wherein the test solution contains Fe3+The concentration is 0.02 mol/L-0.1 mol/L, H2O2The concentration is 0.05 mmol/L-0.8 mmol/L.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002221483A (en) * | 2001-01-25 | 2002-08-09 | Nippon Steel Corp | Testing liquid and method for evaluating corrosion resistance of stainless steel |
| CN108535173A (en) * | 2018-03-30 | 2018-09-14 | 鞍钢股份有限公司 | A kind of method of steel material surface bacterial biof iotalm in simulation water environment |
| CN108956441A (en) * | 2018-09-04 | 2018-12-07 | 鞍钢股份有限公司 | The test method of sulfate reducing bacteria corrosion in a kind of simulating ocean environment |
| CN109374518A (en) * | 2018-10-09 | 2019-02-22 | 中国科学院海洋研究所 | A kind of test device and method of the corrosion of simulation nuclear waste storage tank gas-liquid interface |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002221483A (en) * | 2001-01-25 | 2002-08-09 | Nippon Steel Corp | Testing liquid and method for evaluating corrosion resistance of stainless steel |
| CN108535173A (en) * | 2018-03-30 | 2018-09-14 | 鞍钢股份有限公司 | A kind of method of steel material surface bacterial biof iotalm in simulation water environment |
| CN108956441A (en) * | 2018-09-04 | 2018-12-07 | 鞍钢股份有限公司 | The test method of sulfate reducing bacteria corrosion in a kind of simulating ocean environment |
| CN109374518A (en) * | 2018-10-09 | 2019-02-22 | 中国科学院海洋研究所 | A kind of test device and method of the corrosion of simulation nuclear waste storage tank gas-liquid interface |
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