CN117347211A - Experimental device and experimental method for coupling corrosive wear under high pressure condition - Google Patents
Experimental device and experimental method for coupling corrosive wear under high pressure condition Download PDFInfo
- Publication number
- CN117347211A CN117347211A CN202311341957.8A CN202311341957A CN117347211A CN 117347211 A CN117347211 A CN 117347211A CN 202311341957 A CN202311341957 A CN 202311341957A CN 117347211 A CN117347211 A CN 117347211A
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- pressure reaction
- pressure
- experimental
- working electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002474 experimental method Methods 0.000 title claims abstract description 35
- 230000008878 coupling Effects 0.000 title claims abstract description 28
- 238000010168 coupling process Methods 0.000 title claims abstract description 28
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 71
- 238000003756 stirring Methods 0.000 claims abstract description 52
- 238000005260 corrosion Methods 0.000 claims abstract description 32
- 230000007797 corrosion Effects 0.000 claims abstract description 32
- 238000005299 abrasion Methods 0.000 claims abstract description 25
- 238000012360 testing method Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000013461 design Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000110 cooling liquid Substances 0.000 claims description 37
- 230000001105 regulatory effect Effects 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 9
- 230000006399 behavior Effects 0.000 claims description 7
- 238000000840 electrochemical analysis Methods 0.000 claims description 6
- 230000001808 coupling effect Effects 0.000 claims description 5
- 230000010287 polarization Effects 0.000 claims description 5
- 238000001453 impedance spectrum Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000012935 Averaging Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 13
- 230000007246 mechanism Effects 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 239000008151 electrolyte solution Substances 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000003245 coal Substances 0.000 description 14
- 150000002500 ions Chemical class 0.000 description 6
- 238000011160 research Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000010866 blackwater Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000009991 scouring Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003250 coal slurry Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/56—Investigating resistance to wear or abrasion
- G01N3/565—Investigating resistance to wear or abrasion of granular or particulate material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/56—Investigating resistance to wear or abrasion
- G01N3/567—Investigating resistance to wear or abrasion by submitting the specimen to the action of a fluid or of a fluidised material, e.g. cavitation, jet abrasion
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses an experimental device and an experimental method for corrosion and abrasion coupling under high pressure conditions, wherein the experimental device comprises a high-pressure reaction kettle, a variable-frequency stirring device, an electrochemical workstation and a circulating cooling device; the high-pressure reaction kettle comprises a high-pressure reaction kettle body, a high-pressure reaction kettle cover and a controller, wherein the high-pressure reaction kettle body is internally provided with an experimental medium; the electrochemical workstation is a Prlington multichannel electrochemical workstation, is connected with a working electrode, a reference electrode and an auxiliary electrode by virtue of external copper wires, is placed on one side of the high-pressure reaction kettle, is completed by providing an in-situ electrochemical and corrosion testing device and method for electrolyte solution in a high-pressure environment and matching the electrochemical workstation through a three-electrode structural design, provides an experimental method for researching a mechanism of corrosion abrasion coupling failure more fitting an actual working condition and a matched experimental device, and has great significance for improving the problem of corrosion abrasion coupling failure in the chemical industry field.
Description
Technical Field
The invention belongs to the technical field of coal chemical industry, and particularly relates to an experimental device and an experimental method for corrosion and abrasion coupling under high pressure.
Background
The energy is an important material foundation for stable development of national economy and permanent security of civil society, and has important strategic position in the national economy. The world is now in an unprecedented major bureau with a severe energy crisis. Based on the energy structure characteristics of rich coal, lean oil and less gas in China, the overseas dependence of oil and gas resources is high, and the energy structure is mainly made of coal. The advanced performance of the coal gasification technology as a tap technology of the coal chemical industry influences the efficiency, cost and development of the whole technology of the coal chemical industry, and the system working condition of equipment has the characteristics of high pressure, high temperature, extremely high hardness of media (coal slag and coal slurry), high flow rate, strong flushing, severe flash evaporation cavitation and the like, and the failure problem is frequent. For example, due to the characteristics of high temperature, high pressure difference, high flow rate and the like, the black water treatment system in the coal chemical industry has serious abrasion to valves, pipelines and equipment internals, meanwhile, acidic substances such as HCl, HCOOH, HCN and the like can be generated in the coal gasification reaction, and corrosion effects can be generated on the equipment and the pipelines to a certain extent, so that the pipe valve device of the black water system has double risks of erosion and abrasion and scouring corrosion (abbreviated as abrasion). The problem of failure caused by the coupling action of corrosion and abrasion frequently occurs in various large coal chemical enterprises, and the problem of failure severely restricts the long-period and stable operation of the device.
For the failure prevention and control problem of coal chemical equipment, the control optimization and longer period operation of the equipment are achieved mainly through measures such as corrosion inhibitor, metal coating research, substrate surface hardening treatment, fluid medium analysis, equipment structure optimization and the like, and technical support is provided for guaranteeing the equipment to operate stably and for a long period. Most of the existing researches are single-factor influence researches, and the action mechanism of the corrosion abrasion coupling damage process of the multiphase flow medium is not clear. However, in practical conditions, the surface of the metal material is subjected to abrasion and simultaneously reacts with surrounding corrosive media chemically or electrochemically, so that the material on the surface is accelerated to be lost, and the phenomenon is called corrosive abrasion coupling. The corrosive wear is the result of mechanical scouring and electrochemical corrosion interactions that result in a metal material loss greater than the sum of the two effects alone.
The invention mainly researches the corrosion and abrasion coupling characteristics and failure mechanisms of materials of the coal chemical industry device under variable working conditions such as different fluid flow rates, different temperatures, different pressures, different particle sizes, different particle mass fractions, different corrosive medium environments and the like by means of the corrosion and abrasion coupling experimental device of the high-pressure reaction kettle. The reaction kettle is one of the most commonly used reaction vessels in the coal chemical industry and plays an important role in ensuring the quality of products. At present, a high-pressure reaction kettle experimental device capable of meeting reasonable coal chemical industry demonstration devices and meeting analysis accuracy requirements is yet to be developed.
Disclosure of Invention
The invention provides an experimental device and an experimental method for corrosion and abrasion coupling under high pressure condition, which are completed through the design of a three-electrode structure and cooperation with an electrochemical workstation; the technical problem to be solved by the invention is to provide an experimental method and a matched experimental device for researching the mechanism of the corrosion and abrasion coupling effect failure, which are more fit for the actual working condition, and the experimental method and the matched experimental device have great significance for improving the problem of the corrosion and abrasion coupling effect failure in the chemical industry field.
In order to achieve the above purpose, the present invention provides the following technical solutions: an experimental device for corrosion and abrasion coupling under high pressure condition comprises a high-pressure reaction kettle, a variable-frequency stirring device, an electrochemical workstation and a circulating cooling device;
the high-pressure reaction kettle comprises a high-pressure reaction kettle body, a high-pressure reaction kettle cover and a controller, wherein the controller is arranged on the high-pressure reaction kettle body and can regulate and control the pressure and the temperature of the internal environment of the kettle, and an experimental medium is arranged in the high-pressure reaction kettle body;
the variable-frequency stirring device comprises a variable-frequency driving motor, a frame, a coupler, a stirring shaft and a stirring paddle; the variable frequency driving motor is fixed above the high-pressure reaction kettle cover through the rack; the stirring shaft penetrates through the high-pressure reaction kettle cover, is connected with the variable-frequency driving motor through the shaft coupling and is sealed by adopting mechanical sealing, the upper end of the stirring shaft penetrates through the high-pressure reaction kettle cover, and the stirring paddle is fixed at the bottom end of the stirring shaft;
the electrochemical workstation is a Prlington multichannel electrochemical workstation, is connected with a working electrode, a reference electrode and an auxiliary electrode by means of an external copper wire, and is arranged at one side of the high-pressure reaction kettle;
the circulating cooling device comprises a cooling liquid circulating pump and a pipe valve component, wherein the pipe valve component comprises a pipeline and a regulating valve arranged on the pipeline, a cooling liquid inlet and a cooling liquid outlet are arranged above two sides of the high-pressure reaction kettle body, a cooling clamping cavity is arranged in the wall of the high-pressure reaction kettle body and is communicated with the cooling liquid inlet and the cooling liquid outlet, and the cooling liquid circulating pump is communicated with the cooling liquid inlet and the cooling liquid outlet through the pipe valve component.
Preferably, the volume of the high-pressure reaction kettle is 2L, the design pressure is 10MPa, and the controller is a pressure-temperature body surface.
Preferably, the working electrode, the reference electrode and the auxiliary electrode are fully contacted with the experimental medium, are spaced from the stirring paddles, and are not contacted with the inner wall of the high-pressure reaction kettle body.
Preferably, the lower edge of the stirring paddle is positioned at the middle position of the experimental medium and is kept 3-5 mm lower than the working electrode.
An experimental method based on any one of the experimental devices for corrosive wear coupling under high pressure conditions, comprising the following steps:
s1, preparing 1L of experimental medium with required ion concentration and particle concentration, adding the experimental medium into a high-pressure reaction kettle body, and closing a regulating valve;
s2, fully soaking a working electrode, a reference electrode and an auxiliary electrode in an experimental medium through a fixing device, and simultaneously connecting an external copper wire with an electrochemical workstation;
s3, after the stirring shaft passes through the high-pressure reaction kettle cover to be fixed, sealing the high-pressure reaction kettle cover, and connecting the stirring shaft with a rotating shaft of the variable-frequency driving motor through a coupler;
s4, starting a variable frequency driving motor to drive a stirring paddle to stir an experimental medium in the high-pressure reaction kettle; opening a regulating valve, simultaneously opening a cooling liquid circulating pump, setting target pressure and temperature values in the kettle through a control instrument, and recording pressure and temperature data acquired in real time;
s5, when the pressure and the temperature are regulated to preset values of a single group of experiments, opening an electrochemical workstation, and testing the corrosion and abrasion coupling behavior of the working electrode through an impedance spectrum test or a polarization curve of an electrochemical test system;
s6, before the experiment starts, cleaning the surfaces of the working electrode, the reference electrode and the auxiliary electrode, removing surface impurities by adopting an ultrasonic cleaner, removing surface greasy dirt and redundant moisture by adopting a dryer, completing weighing measurement of the working electrode by adopting an electronic analytical balance, and weighing for multiple times to obtain the initial weight of the working electrode; after the experiment is finished, carrying out ultrasonic cleaning and drying on the working electrode, weighing the working electrode for a plurality of times to obtain the mass of the working electrode, calculating the mass loss, and obtaining the corrosion rate of the test piece through a weightlessness method; the calculation formula is as follows:wherein W is 1 Is the corrosion wear rate of the working electrode; m is m 0 The mass of the working electrode before the experiment; m is m 1 The mass of the working electrode after the experiment; s is the working area of the working electrode; t is the time of experiment; ρ is the density of the working electrode;
s7, according to the experimental flow from the step S1 to the step S6, experimental media with different ion concentrations and particle concentrations are configured, the rotating speed of the variable frequency driving motor is regulated, and the pressure temperature set value of the high-pressure reaction kettle controller is changed, so that corrosion and abrasion coupling action behaviors of the to-be-tested piece are tested.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides an in-situ electrochemical and corrosion testing device and method for electrolyte solution in a high-pressure environment, which are completed by matching a three-electrode structure design with an electrochemical workstation, and provides an experimental method for researching a mechanism of corrosion and wear coupling failure, which is more fit with actual working conditions, and a matched experimental device, and have great significance for improving the problem of corrosion and wear coupling failure in the chemical industry field.
Drawings
FIG. 1 is a schematic diagram of a front view of the present invention;
FIG. 2 is a schematic illustration of the experimental procedure of the present invention.
In the figure: 1. a variable frequency drive motor; 2. a pressure temperature body surface; 3. a high-pressure reaction kettle cover; 4. a cooling liquid inlet; 5. a stirring shaft; 6. a high-pressure reaction kettle body; 7. stirring paddles; 8. an experimental medium; 9. a cooling liquid circulation pump; 10. a frame; 11. a coupling; 12. mechanical sealing; 13. a working electrode; 14. a reference electrode; 15. an auxiliary electrode; 16. a cooling liquid outlet; 17. externally connecting copper wires; 18. an electrochemical workstation; 19. and (3) regulating the valve.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the invention provides an experimental device for coupling corrosive wear under high pressure condition, which comprises a high-pressure reaction kettle, a variable-frequency stirring device, an electrochemical workstation 18 and a circulating cooling device; the high-pressure reaction kettle comprises a high-pressure reaction kettle body 6, a high-pressure reaction kettle cover 3 and a controller, wherein the controller is arranged on the high-pressure reaction kettle body 6 and can regulate and control the pressure and the temperature of the internal environment of the kettle, an experiment medium 8 is arranged in the high-pressure reaction kettle body 6, and the experiment medium 8 is provided with different ion concentrations and particle concentrations according to experiment targets; the variable-frequency stirring device comprises a variable-frequency driving motor 1, a frame 10, a coupler 11, a stirring shaft 5 and stirring paddles 7; the stirring shaft 5 and the stirring paddle 7 are made of polytetrafluoroethylene, and the variable-frequency driving motor 1 is fixed above the high-pressure reaction kettle cover 3 through the frame 10; the stirring shaft 5 penetrates through the high-pressure reaction kettle cover 3, is connected with the rotating shaft of the variable-frequency driving motor 1 through the coupler 11 and is sealed by adopting a mechanical seal 12, so that the air tightness of the high-pressure reaction kettle is ensured, the upper end of the stirring shaft 5 penetrates through the high-pressure reaction kettle cover 3, the stirring paddle 7 is fixed at the bottom end of the stirring shaft 5, the variable-frequency driving motor 1 is fixed above the frame 10 through a nut, and the stirring shaft 5 and the stirring paddle 7 are driven to rotate through the coupler 11, so that different rotating speed values are provided for the experimental medium 8; the electrochemical workstation 18 is a prinston multichannel electrochemical workstation, is connected with the working electrode 13, the reference electrode 14 and the auxiliary electrode 15 by means of external copper wires 17, is placed on one side of the high-pressure reaction kettle, is convenient for analyzing experimental phenomena, controls experimental variables to group and perform experiments, such as temperature, pressure, ions of an experimental medium, concentration of solid particles and the like, and tests the coupling behavior of corrosion and abrasion of the working electrode through an impedance spectrum test or polarization curve of an electrochemical test system after the experimental medium 8 runs stably; the circulating cooling device comprises a cooling liquid circulating pump 9 and a pipe valve component, wherein the pipe valve component comprises a pipeline and a regulating valve 19 arranged on the pipeline, a cooling liquid inlet 4 and a cooling liquid outlet 16 are arranged above two sides of the high-pressure reaction kettle body 6, a cooling clamping cavity is arranged in the wall of the high-pressure reaction kettle body 6 and is communicated with the cooling liquid inlet 4 and the cooling liquid outlet 16, and the cooling liquid circulating pump 9 is communicated with the cooling liquid inlet 4 and the cooling liquid outlet 16 through the pipe valve component; r410a is selected as cooling liquid in the cooling liquid circulating pump 9, the cooling liquid enters the high-pressure reaction kettle body 6 through the cooling liquid inlet 4 to cool the clamping cavity, the temperature of the experimental medium 8 is controlled in a water bath mode, and then the cooling liquid flows out from the cooling liquid outlet 16 to the cooling liquid circulating pump 9 to realize circulation.
Referring to fig. 1, the volume of the high-pressure reaction kettle is 2L, the design pressure is 10MPa, and the controller is a pressure-temperature body surface 2; in the embodiment, the volume of the high-pressure reaction kettle is 2L, the design pressure is 10MPa, which is the experimental preferred design value of the invention, and the pressure and temperature are conveniently and synchronously observed by the body surface 2.
Referring to fig. 1, the working electrode 13, the reference electrode 14, and the auxiliary electrode 15 all fully touch the experimental medium 8, are spaced from the stirring paddle 7, and do not contact the inner wall of the autoclave body 6; in this embodiment, the working electrode 13, the reference electrode 14 and the auxiliary electrode 15 are made to fully contact and react with the experimental medium 8, and the stirring paddle 7 is rotated without being interfered by the electrode and the autoclave body 6.
Referring to fig. 1, the lower edge of the stirring paddle 7 is located at the middle position of the experimental medium 8 and is kept lower than the working electrode 133-5 mm; in the present embodiment, the stirring paddle 7 is made to sufficiently stir the experimental medium 8 without interfering with the working electrode 13.
Referring to fig. 2, the present invention provides an experimental method based on the experimental device for corrosive wear coupling under high pressure conditions, comprising the following steps:
s1, preparing an experimental medium 8 with the required ion concentration and particle concentration of 1L, adding the experimental medium into a high-pressure reaction kettle body 6, and closing a regulating valve 19;
s2, fully soaking a working electrode 13, a reference electrode 14 and an auxiliary electrode 15 in an experimental medium 8 through a fixing device, and simultaneously connecting an external copper wire 17 with an electrochemical workstation 18;
s3, after the stirring shaft 5 passes through the high-pressure reaction kettle cover 3 to be fixed, the high-pressure reaction kettle cover 3 is sealed, and the stirring shaft 5 is connected with a rotating shaft of the variable-frequency driving motor 1 through a coupler 11;
s4, starting the variable frequency driving motor 1 to drive the stirring paddle 7 to stir the experimental medium 8 in the high-pressure reaction kettle; opening a regulating valve 19, simultaneously opening a cooling liquid circulating pump 9, setting target pressure and temperature values in the kettle through a control instrument, and recording pressure and temperature data acquired in real time;
s5, when the pressure and the temperature are regulated to preset values of a single group of experiments, opening an electrochemical workstation 18, testing the corrosion and abrasion coupling behaviors of a working electrode 13 through an impedance spectrum test or a polarization curve of an electrochemical test system, and performing all electrochemical tests by adopting the Prlington electrochemical workstation, wherein the test system is a standard three-electrode system; prior to each electrochemical test, the surface of the working electrode was sanded to 1000#, to expose a fresh surface, and Open Circuit Potential (OCP) monitoring was first performed for 30 minutes to stabilize the electrochemical system to quasi-steady state; then, applying sinusoidal potential disturbance with the frequency of 100 kHz-10 mHz and the amplitude of 10mV under OCP to carry out EIS measurement; the potential scanning range of the potentiodynamic polarization curve test is-300 mVvs. OCP-500 mVvs. SCE, and the potential scanning rate is 0.333mV/s;
s6, before the experiment starts, cleaning the surfaces of the working electrode 13, the reference electrode 14 and the auxiliary electrode 15, removing surface impurities by adopting an ultrasonic cleaner, removing surface greasy dirt and redundant moisture by adopting a dryer, completing weighing measurement of the working electrode 13 by adopting an electronic analytical balance, and weighing for multiple times to obtain the initial weight of the working electrode 13; after the experiment is finished, carrying out ultrasonic cleaning and drying on the working electrode 13, weighing the working electrode 13 for a plurality of times to obtain the mass of the working electrode, calculating the mass loss, and obtaining the corrosion rate of the test piece through a weightlessness method; the calculation formula is as follows:wherein W is 1 Is the erosion rate of the working electrode 13; m is m 0 The mass of the working electrode 13 before the experiment; m is m 1 The mass of the working electrode 13 after the experiment; s is the working area of the working electrode 13; t is the time of experiment; ρ is the density of the working electrode 13;
s7, according to the experimental flow of the steps S1-S6, experimental mediums 8 with different ion concentrations and particle concentrations are configured, the rotating speed of the variable frequency driving motor 1 is regulated, and the pressure temperature set value of the high-pressure reaction kettle controller is changed, so that corrosion and abrasion synergistic action behaviors of the to-be-tested piece are tested.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The experimental device for corrosion and abrasion coupling under high pressure conditions is characterized by comprising a high-pressure reaction kettle, a variable-frequency stirring device, an electrochemical workstation (18) and a circulating cooling device;
the high-pressure reaction kettle comprises a high-pressure reaction kettle body (6), a high-pressure reaction kettle cover (3) and a control instrument, wherein the control instrument is arranged on the high-pressure reaction kettle body (6) and can regulate and control the pressure and the temperature of the internal environment of the kettle, and an experimental medium (8) is arranged in the high-pressure reaction kettle body (6);
the variable-frequency stirring device comprises a variable-frequency driving motor (1), a frame (10), a coupler (11), a stirring shaft (5) and stirring paddles (7); the variable-frequency driving motor (1) is fixed above the high-pressure reaction kettle cover (3) through the rack (10); the stirring shaft (5) penetrates through the high-pressure reaction kettle cover (3) to be connected with the rotating shaft of the variable-frequency driving motor (1) through the coupler (11) and is sealed by adopting a mechanical seal (12), the upper end of the stirring shaft (5) penetrates through the high-pressure reaction kettle cover (3), and the stirring paddle (7) is fixed at the bottom end of the stirring shaft (5);
the electrochemical workstation (18) is a Prlington multichannel electrochemical workstation, is connected with the working electrode (13), the reference electrode (14) and the auxiliary electrode (15) by means of an external copper wire (17), and is arranged at one side of the high-pressure reaction kettle;
the circulating cooling device comprises a cooling liquid circulating pump (9) and a pipe valve component, wherein the pipe valve component comprises a pipeline and a regulating valve (19) arranged on the pipeline, a cooling liquid inlet (4) and a cooling liquid outlet (16) are formed in the upper parts of two sides of a high-pressure reaction kettle body (6), a cooling clamping cavity is formed in the wall of the high-pressure reaction kettle body (6), the cooling liquid inlet (4) is communicated with the cooling liquid outlet (16), and the cooling liquid circulating pump (9) is communicated with the cooling liquid inlet (4) and the cooling liquid outlet (16) through the pipe valve component.
2. The experimental device for coupling of corrosive wear under high pressure according to claim 1, wherein the volume of the high-pressure reaction kettle is 2L, the design pressure is 10MPa, and the controller is a pressure-temperature integrated body (2).
3. The experimental device for coupling of corrosive wear under high pressure according to claim 1, wherein the working electrode (13), the reference electrode (14) and the auxiliary electrode (15) are in full contact with the experimental medium (8), are spaced from the stirring paddles (7), and are not in contact with the inner wall of the autoclave body (6).
4. An experimental device for coupling of corrosive wear under high pressure conditions according to claim 1, characterized in that the lower edge of the stirring paddle (7) is located in the middle of the experimental medium (8) and kept 3-5 mm below the working electrode (13).
5. An experimental method based on the experimental device for corrosive wear coupling under high pressure conditions according to any one of claims 1 to 4, comprising the steps of:
s1, preparing 1L of experimental medium with required ion concentration and particle concentration, adding the experimental medium into a high-pressure reaction kettle body, and closing a regulating valve;
s2, fully soaking a working electrode, a reference electrode and an auxiliary electrode in an experimental medium through a fixing device, and simultaneously connecting an external copper wire with an electrochemical workstation;
s3, after the stirring shaft passes through the high-pressure reaction kettle cover to be fixed, sealing the high-pressure reaction kettle cover, and connecting the stirring shaft with a rotating shaft of the variable-frequency driving motor through a coupler;
s4, starting a variable frequency driving motor to drive a stirring paddle to stir an experimental medium in the high-pressure reaction kettle; opening a regulating valve, simultaneously opening a cooling liquid circulating pump, setting target pressure and temperature values in the kettle through a control instrument, and recording pressure and temperature data acquired in real time;
s5, when the pressure and the temperature are regulated to preset values of a single group of experiments, opening an electrochemical workstation, and testing the corrosion and abrasion coupling behavior of the working electrode through an impedance spectrum test or a polarization curve of an electrochemical test system;
s6, before the experiment starts, cleaning the surfaces of the working electrode, the reference electrode and the auxiliary electrode, removing surface impurities by adopting an ultrasonic cleaner, removing oil stains and redundant moisture on the surface by adopting a dryer, and adopting electronic analysisThe balance completes weighing measurement of the working electrode, and the initial weight of the working electrode is obtained by weighing and averaging for a plurality of times; after the experiment is finished, carrying out ultrasonic cleaning and drying on the working electrode, weighing the working electrode for a plurality of times to obtain the mass of the working electrode, calculating the mass loss, and obtaining the corrosion rate of the test piece through a weightlessness method; the calculation formula is as follows:wherein W is 1 Is the corrosion wear rate of the working electrode; m is m 0 The mass of the working electrode before the experiment; m is m 1 The mass of the working electrode after the experiment; s is the working area of the working electrode; t is the time of experiment; ρ is the density of the working electrode;
s7, according to the experimental flow from the step S1 to the step S6, experimental media with different ion concentrations and particle concentrations are configured, the rotating speed of the variable frequency driving motor is regulated, and the pressure temperature set value of the high-pressure reaction kettle controller is changed, so that corrosion and abrasion coupling action behaviors of the to-be-tested piece are tested.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311341957.8A CN117347211A (en) | 2023-10-17 | 2023-10-17 | Experimental device and experimental method for coupling corrosive wear under high pressure condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311341957.8A CN117347211A (en) | 2023-10-17 | 2023-10-17 | Experimental device and experimental method for coupling corrosive wear under high pressure condition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117347211A true CN117347211A (en) | 2024-01-05 |
Family
ID=89355448
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311341957.8A Pending CN117347211A (en) | 2023-10-17 | 2023-10-17 | Experimental device and experimental method for coupling corrosive wear under high pressure condition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117347211A (en) |
-
2023
- 2023-10-17 CN CN202311341957.8A patent/CN117347211A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN201594066U (en) | Simulated petrochemical pipeline erosion-corrosion monitoring test device | |
| CN109856036A (en) | A kind of high temperature and pressure gas, liquid, solid three-phase erosion corrosion test device and method | |
| CN105866018A (en) | Test device and method for evaluating scouring corrosion of oil-gas pipeline under high flow rate | |
| CN109269966A (en) | Dynamic Corrosion performance test methods | |
| Rashid et al. | 3-Methoxypropyl-amine as corrosion inhibitor for X80 steel in simulated saline water | |
| CN202974789U (en) | Loop test device for simulating natural gas gas-phase erosion-corrosion | |
| Qin et al. | Main control factors and prediction model of flow-accelerated CO2/H2S synergistic corrosion for X65 steel | |
| CN109187676A (en) | A kind of reaction under high pressure kettle device and its application method for simulated deep-sea environment | |
| Jing et al. | Effect of flow velocity on corrosion behavior of AZ91D magnesium alloy at elbow of loop system | |
| Zhang et al. | Corrosion behavior of X65 steel at different depths of pitting defects under local flow conditions | |
| Sivokon et al. | Laboratory assessment of the efficiency of corrosion inhibitors at oilfield pipelines of the West Siberia region I. Objective setting | |
| CN117347211A (en) | Experimental device and experimental method for coupling corrosive wear under high pressure condition | |
| CN117288668A (en) | Device and method for testing corrosion resistance of metal material | |
| CN202854022U (en) | Comparison simulation testing device for carbon dioxide corrosion resistance of steel products | |
| CN114965231A (en) | Experimental device suitable for metal tubular column material corrodes | |
| CN106525708A (en) | Chanel type dynamic medium electrochemical test apparatus and method | |
| Zhang et al. | Effect of HCO3− concentration on CO2 corrosion in oil and gas fields | |
| Nor | The Effect of Turbulent Flow on Corrosion of Mild Steel in High Partial CO 2 Environments | |
| Galvan-Martinez et al. | Study of the mass transport on corrosion of low carbon steel immersed in sour solution under turbulent flow conditions | |
| Ma et al. | Comparative investigation on high-pressure flow accelerated corrosion at gradual contraction and gradual expansion pipes | |
| CN114578030A (en) | Multi-medium coupling variable-temperature pressure corrosion test device and test method | |
| Papavinasam et al. | Inhibitor Selection for Internal Corrosion Control of Pipelines: Comparison of Rates of General Corrosion and Pitting Corrosion Under Gassy-Oil Pipeline Conditions in the Laboratory and in the Field | |
| Andresen | Corrosion fatigue testing | |
| KR20100137845A (en) | Apparatus and method for continuous corrosion monitoring and determination of end point in chemical cleaning process of power plant boilers by hydrogen gas | |
| WO2023179084A1 (en) | Pin-on-disc frictive-corrosive multi-environment coupling test apparatus, and method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |