CN106198374B - Electrode for high-temperature high-pressure galvanic corrosion electrochemical test and application thereof - Google Patents
Electrode for high-temperature high-pressure galvanic corrosion electrochemical test and application thereof Download PDFInfo
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- CN106198374B CN106198374B CN201610475848.9A CN201610475848A CN106198374B CN 106198374 B CN106198374 B CN 106198374B CN 201610475848 A CN201610475848 A CN 201610475848A CN 106198374 B CN106198374 B CN 106198374B
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- 238000005260 corrosion Methods 0.000 title claims abstract description 70
- 230000007797 corrosion Effects 0.000 title claims abstract description 69
- 238000000840 electrochemical analysis Methods 0.000 title abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 78
- 229910052751 metal Inorganic materials 0.000 claims abstract description 78
- 238000012360 testing method Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 239000000565 sealant Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 238000004382 potting Methods 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 150000002739 metals Chemical class 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910000856 hastalloy Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001342 Bakelite® Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000004637 bakelite Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
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- 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
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- 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
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Abstract
The invention discloses an electrode for high-temperature and high-pressure galvanic corrosion electrochemical test, which comprises an insulating support, a high-temperature autoclave and a reference electrode, wherein the upper part of the insulating support is in threaded connection with a high-temperature and high-pressure autoclave cover of the high-temperature autoclave, a lead is arranged in the insulating support, one end of the lead is led out of the high-temperature autoclave and is connected with a galvanic corrosion meter, the other end of the lead is connected with a metal sample, one end of the reference electrode extends into the high-temperature autoclave, and the other end of the reference electrode is connected with the galvanic corrosion meter. The invention can research the contact corrosion behavior of dissimilar metals in a high-temperature high-pressure liquid phase medium or a multiphase medium containing a liquid phase, is suitable for a galvanic couple electrode for electrochemical test in a high-temperature high-pressure closed environment, and utilizes the electrode to perform the electrochemical test of galvanic couple corrosion by virtue of a high-temperature high-pressure autoclave.
Description
Technical Field
The invention relates to an electrode for high-temperature and high-pressure galvanic corrosion electrochemical test and application thereof, in particular to preparation of the electrode for the galvanic corrosion electrochemical test in a high-temperature and high-pressure closed environment, an electrochemical test system formed by the electrode, a high-temperature autoclave and a reference electrode, and online electrochemical test of galvanic corrosion caused by dissimilar metal contact.
Background
With the continuous development of industry, the corrosion environment is more and more demanding, wherein a high-temperature and high-pressure sealed environment is one of the most common corrosion environments in the petroleum industry and the chemical industry, and the high temperature and high pressure put higher requirements on corrosion electrochemical tests, therefore, most of the corrosion electrochemical tests are carried out under normal pressure, and the results of the tests are necessarily greatly different from the actual environments.
Galvanic corrosion refers to the phenomenon that different metal materials are selected for equipment to prepare parts, the parts are mutually contacted, and in an electrolyte, metal with lower electrode potential becomes an anode of a corrosion primary battery, so that the accelerated corrosion is caused. The petroleum industry and chemical industry are complex in equipment structure, different metal materials are often selected, so galvanic corrosion is very common, and the galvanic corrosion becomes important content of research.
For galvanic corrosion, people mainly use a galvanic corrosion meter to test the respective self-corrosion potential, galvanic potential and galvanic current change conditions of two metals constituting a galvanic couple, thereby discussing the influence factors of galvanic corrosion, the mechanism of galvanic corrosion and the method for controlling galvanic corrosion.
At present, a galvanic couple electrode system in a high-temperature and high-pressure environment is lacked, so that corresponding research is deficient, corresponding corrosion data accumulation is lacked, and particularly, the detailed change rule of galvanic couple corrosion along with time cannot be monitored.
Disclosure of Invention
In order to solve the technical problem, the invention provides an electrode for high-temperature and high-pressure galvanic corrosion electrochemical test, which comprises an insulating support, a high-temperature and high-pressure autoclave and a reference electrode, wherein the upper part of the insulating support is in threaded connection with a high-temperature and high-pressure autoclave cover of the high-temperature and high-pressure autoclave, a lead is arranged in the insulating support, one end of the lead is led out of the high-temperature autoclave and is connected with a galvanic corrosion meter, the other end of the lead is connected with a metal sample, one end of the reference electrode extends into the high-temperature autoclave, and the other end of the reference electrode.
Furthermore, the insulating support also comprises a support shell, the support shell is a hastelloy shell, and a high-temperature-resistant and high-pressure-bearing insulating filling material is arranged in the support shell.
Furthermore, a pouring sealant and a sealing insulating gasket are arranged at the contact position of the metal sample and the support shell.
Furthermore, the upper portion of support shell is provided with the fixed shim, the fixed shim is drawn forth to the one end of wire, the other end of wire 4 is connected with the metal connecting piece.
Furthermore, the number of the metal samples is two, namely a metal sample A and a metal sample B.
Further, the top of metal sample is provided with the external screw thread, metal connection piece is provided with the internal thread, metal sample and metal connection piece threaded connection.
The invention also provides an application of the electrode for the high-temperature and high-pressure galvanic corrosion electrochemical test, which comprises the following steps: screwing the bracket shell with the high-temperature high-pressure kettle cover; step two: inserting a reference electrode into a high-temperature high-pressure kettle through a high-temperature high-pressure kettle cover; step three: respectively connecting the reference electrode, the metal sample A and the metal sample B with three binding posts of a galvanic corrosion meter; step four: and designing experimental corrosion medium, temperature and pressure conditions according to the required simulated field working condition conditions, and starting a galvanic corrosion meter to test corresponding galvanic corrosion electrochemical parameters.
The invention can research the contact corrosion behavior of dissimilar metals in a high-temperature high-pressure liquid phase medium or a multiphase medium containing a liquid phase, is suitable for a galvanic couple electrode for electrochemical test in a high-temperature high-pressure closed environment, and utilizes the electrode to perform the electrochemical test of galvanic couple corrosion by virtue of a high-temperature high-pressure autoclave.
Drawings
FIG. 1 is a schematic diagram of the electrode structure for high-temperature high-pressure galvanic corrosion electrochemical test according to the present invention;
FIG. 2 is a diagram of a galvanic couple electrode of the present invention connected to a reference electrode, high temperature autoclave;
FIG. 3 is a graph of galvanic potential and galvanic current for a galvanic corrosion test when the present invention is applied.
In the figure, 1, a support shell, 2, a fixing gasket, 3, an insulating filling material, 4, a wire, 5, a metal connecting sheet, 6, pouring sealant, 7, a sealing insulating gasket, 8, metal samples A and 9, metal samples B and 10, an insulating sealing gasket, 11, a reference electrode, 12, a high-temperature high-pressure kettle cover, 13 and a high-temperature high-pressure kettle.
Detailed Description
The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Referring to fig. 1 to 3, the electrode for high-temperature and high-pressure galvanic corrosion electrochemical testing in the invention comprises an insulating support, a high-temperature high-pressure autoclave 13 and a reference electrode 11, wherein the insulating support comprises a support shell 1, in this embodiment, the support shell 1 is a hastelloy shell, a fixed gasket 2 is arranged at the upper part of the support shell 1, a high-temperature-resistant and high-pressure-bearing insulating filling material 3, a lead 4 and a metal connecting sheet 5 are further arranged inside the support shell 1, the fixed gasket 2 is led out from one end of the lead 4, and the other end of the lead 4 is connected with the metal connecting sheet 5.
The lower part of metal connecting piece 5 is connected with the metal sample, and the metal sample contains two in this embodiment, is metal sample A8 and metal sample B9 respectively, the top of metal sample is provided with the external screw thread, metal connecting piece 5 is provided with the internal thread, metal sample and metal connecting piece 5 threaded connection.
The contact position of the metal sample and the bracket shell 1 is provided with pouring sealant 6 and a sealing insulating gasket 7, in the embodiment, the bracket shell 1 plays a role in fixing and supporting, and is in threaded connection with a high-temperature high-pressure kettle cover 12 of a high-temperature high-pressure kettle 13 through threads at the upper end of the bracket shell, so that the high-temperature high-pressure corrosion resistance effect is achieved; the lead 4 and the metal connecting sheet 5 play a role in conducting electricity for connecting the two metal samples, and transmit electrochemical signals on the surfaces of the metal samples to an external galvanic corrosion meter; the lead 4 is led out of the fixed gasket 2 to play a role of fixing the lead and prevent the insulating filling material 3 from overflowing; the insulating filling material 3, the pouring sealant 6 and the sealing insulating gasket 7 play a role in isolating the conductive channels of the two metal samples and play a role in resisting high temperature and high pressure.
In this embodiment, the high temperature resistant insulating filler is bakelite powder, the metal connecting sheet is a copper sheet, the wire is a copper wire, and the fixing gasket is polytetrafluoroethylene.
Referring to fig. 2, the electrode for electrochemical testing of high-temperature high-pressure galvanic corrosion according to the present invention is screwed to the lid 12 of the autoclave through the external thread at the upper end of the housing 1 of the support, and the insulating gasket 10 is disposed at the contact position to enhance the sealing effect, and the reference electrode 11 is inserted into the autoclave 13 through the lid 12 of the autoclave to form a high-temperature high-pressure galvanic corrosion electrochemical testing system.
The specific preparation process of the insulating bracket is as follows:
processing a circular shell, wherein the interior of the shell is hollow, external threads are processed on the outer surface of the upper section, and the rest surfaces are smooth surfaces;
leading the lead 4 out of the fixed gasket 2, so that the upper end of the lead 4 is arranged outside the bracket shell 1, the lower end of the lead 4 is arranged inside the bracket shell 1, and welding the metal connecting sheet 5 at the lower end of the lead 4;
step three, filling the high-temperature-resistant and high-pressure-bearing insulating filling material 3 into the bracket shell 1, extruding and compacting, heating to melt the high-temperature-resistant insulating filling material, and pressing and fastening under isostatic pressure;
and fourthly, two step holes are formed in the lower end of the support shell 1 in a split mode, holes are drilled in the centers of the step holes until the metal connecting sheets 5 are drilled through, and then internal threads are machined.
The steps of connecting the metal sample and the insulating bracket are as follows:
processing two metal samples (a metal sample A8 and a metal sample B9), wherein the upper end of the metal sample is processed into a cylinder with external threads, and the lower end of the metal sample can be processed into different shapes and different surface area ratios according to requirements;
and step two, sleeving a polytetrafluoroethylene sealing insulating gasket 7 on the metal sample, screwing the metal sample into a hole at the lower end of the support shell 1 to be further screwed with the metal connecting sheet 5, and pouring high-temperature-resistant epoxy pouring sealant 6 in the screwing process.
The invention provides an electrode for high-temperature and high-pressure galvanic corrosion electrochemical test, which comprises the following test application processes:
(A) determining the components, temperature, total pressure and gas partial pressure of the corrosion solution according to the on-site working condition;
(B) installing a metal sample and a reference electrode 11 for high-temperature and high-pressure galvanic corrosion electrochemical test;
(C) introducing a proper amount of corrosive solution into the high-temperature high-pressure kettle 13 to ensure that the reference electrode 11 is completely soaked in the corrosive solution, covering the high-temperature high-pressure kettle cover 12, introducing corrosive gas according to the requirements of partial pressure and total pressure, and heating to a set temperature;
(D) connecting the wires of the metal sample for the high-temperature and high-pressure galvanic corrosion electrochemical test and the reference electrode 11 with a galvanic corrosion meter, starting the galvanic corrosion meter to test the electrochemical parameters of the galvanic corrosion such as galvanic potential and galvanic current, analyzing the electrochemical test result, and discussing the galvanic corrosion behaviors of the metal sample A8 and the metal sample B9 in the high-temperature and high-pressure corrosion environment.
In the specific embodiment, the galvanic potential and galvanic current of high-temperature and high-pressure galvanic corrosion are tested:
according to the electrode for the high-temperature high-pressure galvanic corrosion electrochemical test, the galvanic current and the galvanic potential of 20-L stainless steel and 316-L stainless steel are tested under the test condition of H2S partial pressure of 1MPa and CO24MPa partial pressure and 60 ℃ in 3.5 percent NaCl solution.
The test result is shown in figure 3, the tested couple current and couple potential curve is stable, and the test result is reliable. The galvanic potential is gradually increased and the galvanic current is gradually reduced along with the prolonging of the corrosion time, and the galvanic current tends to be stable after 28 hours, which shows that the galvanic effect is larger at the beginning and is reduced at the later stage, and the corrosion product on the surface of the anode 20 steel generates resistance after corrosion, so that the galvanic corrosion rate is reduced.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (6)
1. An electrode for high-temperature and high-pressure galvanic corrosion electrochemical testing is characterized by comprising an insulating support, a high-temperature and high-pressure autoclave and a reference electrode, wherein the upper part of the insulating support is in threaded connection with a high-temperature and high-pressure autoclave cover of the high-temperature and high-pressure autoclave, the outer part of the insulating support is a circular support shell, the inner part of the insulating support is of a hollow structure, the outer surface of the upper section of the insulating support is provided with external threads and is in threaded connection with the high-temperature and high-pressure autoclave cover, the upper part of the insulating support is provided with a fixed gasket, one end of the wire penetrates through the fixed gasket and is led out of the high-temperature autoclave and is connected with a galvanic corrosion meter, one end of the reference electrode extends into the high-temperature and high-pressure autoclave, the other end of the reference electrode is connected with the galvanic corrosion meter, the support shell, the other end of the wire is arranged in the support shell, the other end of the wire is connected with a metal connecting sheet, the lower portion of the metal connecting sheet is connected with a metal sample, the center of the metal connecting sheet is of an internal thread structure, two step holes are formed in the lower end of the support shell in a split mode, the top end of the metal sample is of a cylindrical structure with an external thread, the metal sample is in threaded connection with the metal connecting sheet through the step holes, and a sealing insulating gasket is arranged between the metal sample and the bottom of the support shell.
2. The electrode for high-temperature high-pressure galvanic corrosion electrochemical testing according to claim 1, wherein a potting adhesive is further disposed at a contact position of the metal sample and the support housing.
3. The electrode for high-temperature high-pressure galvanic corrosion electrochemical testing according to claim 1, wherein the number of the metal samples is two, namely a metal sample A and a metal sample B.
4. The electrode for high-temperature high-pressure galvanic corrosion electrochemical testing according to claim 1, wherein the insulating support is prepared by the following specific steps:
processing a circular shell, wherein the interior of the shell is hollow, external threads are processed on the outer surface of the upper section, and the rest surfaces are smooth surfaces;
leading out the lead from the fixed gasket, so that the upper end of the lead is arranged outside the bracket shell, the lower end of the lead is arranged inside the bracket shell, and welding the metal connecting sheet at the lower end of the lead;
step three, filling the high-temperature-resistant and high-pressure-bearing insulating filling material into the bracket shell, extruding and compacting, heating to melt the high-temperature-resistant insulating filling material, and pressing and fastening under isostatic pressure;
and fourthly, two step holes are formed in the lower end of the support shell in a split mode, holes are drilled in the centers of the step holes until the metal connecting sheets are drilled through quickly, and then internal threads are machined.
5. The electrode for high temperature and high pressure galvanic corrosion electrochemical testing of claim 1, wherein the metal sample and the insulating support are connected by the following steps:
processing a metal sample A and a metal sample B, wherein the upper end of the metal sample A and the upper end of the metal sample B are processed into a cylinder with external threads, and the lower end of the metal sample B is processed into different shapes and different surface area ratios according to requirements;
and step two, sleeving a polytetrafluoroethylene sealing insulating gasket on the metal sample, screwing the metal sample into a hole at the lower end of the support shell so as to be in threaded connection with the metal connecting sheet, and pouring high-temperature-resistant epoxy pouring sealant in the screwing process.
6. The application of the electrode for high-temperature and high-pressure galvanic corrosion electrochemical testing according to claim 1, wherein the first step is: screwing the bracket shell with the high-temperature high-pressure kettle cover; step two: inserting a reference electrode into a high-temperature high-pressure kettle through a high-temperature high-pressure kettle cover; step three: respectively connecting the reference electrode, the metal sample A and the metal sample B with three binding posts of a galvanic corrosion meter; step four: and designing experimental corrosion medium, temperature and pressure conditions according to the required simulated field working condition, and starting a galvanic corrosion meter to test corresponding galvanic corrosion electrochemical parameters.
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| CN201610475848.9A CN106198374B (en) | 2016-06-24 | 2016-06-24 | Electrode for high-temperature high-pressure galvanic corrosion electrochemical test and application thereof |
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| CN201610475848.9A CN106198374B (en) | 2016-06-24 | 2016-06-24 | Electrode for high-temperature high-pressure galvanic corrosion electrochemical test and application thereof |
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| CN106198374B true CN106198374B (en) | 2020-03-24 |
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| CN106706511B (en) * | 2017-02-16 | 2023-08-11 | 天津大学 | Electrochemical reaction kettle with two open sides and application method thereof |
| CN106940277A (en) * | 2017-05-25 | 2017-07-11 | 河南科技大学 | Dissimilar metal friction is with secondary corrosion wear characteristic method of testing and test device |
| CN107884334A (en) * | 2017-11-21 | 2018-04-06 | 北京市燃气集团有限责任公司 | A kind of galvanic corrosion test system and its method of testing |
| CN108519300A (en) * | 2018-03-08 | 2018-09-11 | 中国科学院金属研究所 | A kind of galvanic corrosion weightless test method under the conditions of realization high hydrostatic pressure |
| CN108918402A (en) * | 2018-06-12 | 2018-11-30 | 中国船舶重工集团公司第七二五研究所 | A kind of high temperature and pressure galvanic corrosion experimental rig |
| CN109060925B (en) * | 2018-09-05 | 2024-02-27 | 安科工程技术研究院（北京）有限公司 | Couple corrosion test device used in high-temperature high-pressure environment |
| CN110940628B (en) * | 2019-12-18 | 2022-08-16 | 苏州热工研究院有限公司 | Electrochemical in-situ micro-vibration wear test system and use method thereof |
| CN111220532B (en) * | 2020-01-18 | 2020-12-18 | 温州新国余机械科技有限公司 | Testing arrangement of electrode high temperature corrosivity for glass electric melting furnace |
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