CN108680491A - Method for testing using dynamic electrochemical device - Google Patents
Method for testing using dynamic electrochemical device Download PDFInfo
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Abstract
The invention discloses a method for testing by utilizing a dynamic electrochemical device, which comprises the following steps of firstly, filling corrosive liquid into a high-pressure kettle body through a feeding auxiliary device and a feeding hole; introducing inert gas into the corrosive liquid in the high-pressure kettle body through the gas inlet pipe; introducing experimental gas into the corrosive liquid in the high-pressure kettle body through an air inlet pipe; starting a heating and heat-preserving device through an external control box, heating the corrosive liquid in the high-pressure kettle to a set experimental temperature and preserving heat, adjusting the control box, and changing the rotating speed of a rotating shaft to enable the rotating speed to reach a preset rotating speed; and the external electrochemical workstation is respectively connected with the working electrode, the auxiliary electrode and the reference electrode, receives signals and starts to perform experimental tests. The technical scheme of the invention is suitable for detecting the corrosion in-situ electrochemical signal of the metal material under the dynamic working condition of the high-temperature high-pressure corrosion medium so as to carry out high-temperature high-pressure dynamic corrosion behavior and mechanism research, and solves the problem that the electrochemical signal measurement of the simulation solution under the high-temperature high-pressure condition cannot be carried out in the past.
Description
The present patent application is the division of parent application " high temperature and pressure dynamic electro-chemical test experimental provision and test method "
The applying date of application, parent application is on May 16th, 2016, and application No. is 2016103221363.
Technical field
The present invention relates to electro-chemical test experimental provision, especially high temperature and pressure dynamic electro-chemical test experimental provisions and survey
Method for testing.
Background technology
Occur to destroy or go bad caused by chemistry or electrochemical action between metal material and ambient enviroment (medium) to claim
For corrosion, metal erosion spreads the every field of industrial and agricultural production and national defense construction, and harm is very serious.And high temperature pressure corrosion
It is a kind of to lead to a kind of phenomenon of material failure because electrochemical corrosion acts on.Such as during oil and gas development, in associated gas
Often contain H2S and CO2, various pipelines or structure is caused to fail in the form of high temperature pressure corrosion.Carry out high temperature pressure corrosion process
Simulated experiment is defeated oil/gas material screening and evaluation, the screening of sustained release agent and evaluation and research material corrosion resistance and etching machine
The important means of reason.But due under high-temperature and high-pressure conditions, to working electrode, reference electrode and the isostructural resistance to height of auxiliary electrode
Mild high voltage performance has very high requirement, is not easy to realize the output of electrochemical signals.Meanwhile related forming currently on the market
The price of product is all higher, affects the extensive research to high temperature pressure corrosion behavior and mechanism.
Invention content
The present invention overcomes the disadvantages of the prior art, provides high temperature and pressure dynamic electro-chemical test experimental provision and surveys
Method for testing.The device is suitable for high temperature pressure corrosion medium under the conditions of dynamic operation condition, to metallic material corrosion electrochemical in-situ
Signal is detected, and to carry out the behavior of high temperature and pressure Dynamic Corrosion and mechanism study, solving in the past cannot be to simulated solution
The problem of electrochemical signals measurement is carried out under high-temperature and high-pressure conditions.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions：
High temperature and pressure dynamic electrochemical testing device, including high-temperature high-pressure reaction kettle, three-electrode system, external control cabinet,
External air supply system, external electrochemical workstation and computer；
High-temperature high-pressure reaction kettle include autoclave body, high pressure kettle cover, air inlet pipe, escape pipe, rotation axis, pressure sensor,
Pressure gauge, temperature sensor, heating device and heat preservation heat insulation layer, autoclave body is cylindrical container, in the outside of autoclave body
Heating device is set, thermal insulating warm-keeping layer is set in the outside of heating device, high pressure kettle cover is set in the upper surface of autoclave body, tightly
Fixing bolt passes through fixed mounting hole, is connected with autoclave body interconnecting piece, so that kettle cover is tightened to an entirety with autoclave body, and realizes
It seals, is diametrically disposed on high pressure kettle cover circular surface：Air inlet pipe hole, temperature sensor hole, working electrode hole,
Rotational axis hole, charging aperture, pressure sensor hole and outlet pore, wherein rotational axis hole are located at circle centre position, are arranged in rotational axis hole
Rotation axis, rotation axis connection control motor, and rotation axis top half is located on high pressure kettle cover, and rotation axis lower half portion is located at height
It presses in autoclave body, the lower end of rotation axis is provided with mixing component, is respectively arranged with above and below working electrode hole is adjacent
Auxiliary electrode hole and reference electrode hole, are provided with working electrode column on working electrode hole, and auxiliary is arranged on auxiliary electrode hole
Reference electrode is arranged on reference electrode hole, air inlet pipe is arranged in air inlet pipe hole, outlet is arranged in outlet pore for electrode column
Pipe, setting charging auxiliary device, pressure sensor and pressure gauge are provided on pressure sensor hole on charging aperture；
In the above-mentioned technical solutions, the lower half portion length in autoclave body that is located at of the rotation axis accounts for autoclave body height
, the mixing component is agitating paddle or stirring disk；
In the above-mentioned technical solutions, the air inlet pipe gos deep into the bottom of autoclave body, and escape pipe is located in autoclave body
It is more than liquid surface；
In the above-mentioned technical solutions, temperature sensor is connected with temperature controller, and temperature controller is connected with heating device；
In above-mentioned technical proposal, when three electrodes is arranged in three electrode holes, electrode is with the structure at high pressure kettle cover sealing,
Setting of casing, upper casing and plug are set gradually from bottom to top；
Three-electrode system includes reference electrode, working electrode column, auxiliary electrode column, working electrode stabilising arrangement and electrode
Folder, wherein reference electrode are an integral structure Ag/AgCl electrodes, and working electrode column and auxiliary electrode column have identical structure, i.e.,
Cylindrical structure is arranged metallic channel directed downwardly in the lower section of cylinder, sheet metal is arranged in metallic channel, along cylindrical center's setting
The bottom end of portion's conducting wire, inner lead is in contact with the sheet metal in metallic channel, the side setting fastening spiral shell button in the position that is in contact,
Fasten the connection that spiral shell button is used for fixing internal conducting wire and sheet metal；In order to make working electrode and reference in autoclave body under stirring
Stabilizing distance is kept, therefore working electrode auxiliary stabilizing device is set, which includes first clamping plate, second clamping plate and third clamping plate
And telescopic device, telescopic device connect into an entirety across three pieces of clamping plates, first clamping plate and third clamping plate can be along telescopic devices
It carries out, close to the activity with separate second clamping plate, secure component (not marking in figure) being arranged in first clamping plate and third clamping plate,
For strap and telescopic device, electrode holder includes stable disk, conducting wire and sheet metal, and working electrode groove is arranged in stable disk,
Working electrode sample is set in working electrode groove, and stable disk is connected by conducting wire with sheet metal, and reference electrode is fixed on the first folder
Between plate and second clamping plate, the stable disk of electrode holder is fixed between second clamping plate and third clamping plate, keeps working electrode sample flat
It is hollow structure between clamping plate facing towards reference electrode, makes to be full of experimental solutions between working electrode sample and reference electrode, gold
Belong to piece and be connected with working electrode by being inserted into the metallic channel below working electrode column, is set in the lower-lying metal slot of auxiliary electrode column
Set platinum plate electrode；
In the above-mentioned technical solutions, the working electrode is the test button of epoxy encapsulation,
In the above-mentioned technical solutions, the auxiliary electrode is the platinum plate electrode of 13 × 10 × 0.2mm, unilateral exposed surface
Product is 10 × 10mm,
In the above-mentioned technical solutions, the working electrode surface is away from reference electrode 2-5mm；
In the above-mentioned technical solutions, the working electrode auxiliary stabilizing device and electrode holder are maximum temperature 260
DEG C, maximum pressure is the polytetrafluoroethylene (PTFE) of 10Mpa；
In the above-mentioned technical solutions, the reference electrode is 310 DEG C of maximum temperature, and maximum pressure is the high temperature of 10Mpa
High pressure Ag/AgCl electrodes；
External control cabinet is connected with heating and heat-insulating device and rotation axis, and heating and thermal insulation dress can be adjusted by external control cabinet
The rotating speed of the temperature and rotation axis set；
External air supply system is connected with the air inlet pipe of device, for providing corrosive gas；
External electrochemical workstation is connected with the terminals of auxiliary electrode, reference electrode and working electrode, auxiliary for acquiring
The electrochemical signals of electrode, reference electrode and working electrode, computer are helped to be connected with external electrochemical workstation, for external
The data of electrochemical workstation acquisition are recorded, analyzing processing and output.
The test method of high temperature and pressure dynamic electrochemical testing device is as follows：
Step 1, corrosive liquid is packed into autoclave body by charging auxiliary device and charging aperture, and covers high pressure kettle cover and gives
With fixation；
Step 2, it is passed through inert gas in the corrosive liquid by air inlet pipe into autoclave body, to remove in autoclave body
Oxygen；
In step 2, inert gas is nitrogen, helium or argon gas；
In step 2, the time for being passed through inert gas is 12-24 hours, preferably 15-20 hours；
Step 3, it is passed through experimental gas in the corrosive liquid by air inlet pipe into autoclave body, so that experimental gas is filled in
Autoclave body inner space；
In step 3, the time for being passed through experimental gas is 22-24 hours, experimental gas CO2Or H2S gases；
Step 4, heating and heat-insulating device is started by external control cabinet, autoclave internal corrosion liquid is heated to setting experiment temperature
It spends and keeps the temperature, adjusting control case changes rotation rotating speed, reaches preset rotation speed；
Step 5, external electrochemical workstation is connected with working electrode, auxiliary electrode and reference electrode respectively, and receives letter
Number, proceed by experiment test.
In actual use, pressure setting, during excluding oxygen, high pressure are carried out by pressure sensor and pressure gauge
When pressure reaches preset value in kettle, it can generally assert that oxygroup originally drains；Similarly, when pressure reaches preset value in autoclave, one
As can assert that experimental gas has been filled with space in autoclave.
Compared with prior art, the beneficial effects of the invention are as follows：Using high temperature and pressure Ag/AgCl reference electrodes, reach
The requirement of test environment leakproofness and heat-resisting quantity, while also ensuring the accuracy of test result, it is assisted using working electrode
Stabilising arrangement makes working electrode keep relative distance to fix with reference electrode, and autoclave body meets the requirement of leakproofness and heat-resisting quantity,
The device provides the test environments of high temperature and pressure can be used for dynamic high temperature high pressure corrosion behavior and mechanism study.
Description of the drawings
Fig. 1 is the autoclave superstructure schematic diagram of the present invention.
Fig. 2 is the whole kettle side structure schematic view of A-A sections in Fig. 1.
Fig. 3 is that autoclave covers component connection sealing means schematic diagram.
Fig. 4 is working electrode column/reference electrode rod structure schematic diagram.
Fig. 5 is electrode holder structural schematic diagram.
Fig. 6 is working electrode auxiliary stabilizing device overlooking structure diagram.
Fig. 7 is working electrode auxiliary stabilizing device side structure schematic view.
Fig. 8 is temperature 60 C, CO2Divide 0.03Mpa, under 0m/s and 0.3m/s rotating speeds, the electrochemical corrosion of carbon steel A106B
Polarization curve.
Fig. 9 is 90 DEG C of temperature, CO2Divide 0.1Mpa, under 0m/s and 0.3m/s rotating speeds, the electrochemical corrosion of carbon steel A106B
Polarization curve.
Figure 10 is 90 DEG C of temperature, CO2Divide 0.2Mpa, under 0m/s and 0.5m/s rotating speeds, the electrochemical corrosion of carbon steel A106B
Polarization curve.
Figure 11 is 90 DEG C of temperature, CO2Divide 0.5Mpa, under 0m/s and 1m/s rotating speeds, the electrochemical corrosion pole of carbon steel A106B
Change curve.
In 1-7：1 is autoclave body, and 2 be heating device, and 3 be heat preservation heat insulation layer, and 4 be nut, and 5 be mixing component, and 6 are
Escape pipe, 7 be pressure sensor, and 8 be pressure gauge, and 9 be charge door, and 10 be rotation axis, and 11 be auxiliary electrode column, and 12 be reference electricity
Pole, 13 be working electrode column, and 14 be temperature sensor, and 15 be air inlet pipe, and 16 be fastening bolt, and 17 be high pressure kettle cover, and 18 be work
Make electrode, 19 be auxiliary electrode, and 20 be autoclave outer wall, and 21 be outlet pore, and 22 be pressure sensor hole, and 23 be charging aperture,
24 be rotational axis hole, and 25 be auxiliary electrode hole, and 26 be working electrode hole, and 27 be temperature sensor hole, and 28 be air inlet pipe hole, 29
It is inner lead for reference electrode hole, 30,31 be plug, and 32 be upper casing, and 33 be setting of casing, and 34 be fastening spiral shell button, and 35 be gold
Belong to slot, 36 be stable disk, and 37 be working electrode groove, and 38 be conducting wire, and 39 be sheet metal, and 40 be first clamping plate, and 41 be the second folder
Plate, 42 be third clamping plate, and 43 be telescopic device, and 44 be fixed mounting hole, and 45 motors in order to control, 46 be autoclave body interconnecting piece.
In 8-11,1 is static lower test, and 2 indicate the lower test of dynamic.
Specific implementation mode
Present invention is further described in detail with specific embodiment below in conjunction with the accompanying drawings：
High temperature and pressure dynamic electrochemical testing device, including high-temperature high-pressure reaction kettle, three-electrode system, external control cabinet,
External air supply system, external electrochemical workstation and computer；
High-temperature high-pressure reaction kettle include autoclave body, high pressure kettle cover, air inlet pipe, escape pipe, rotation axis, pressure sensor,
Pressure gauge, temperature sensor, heating device and heat preservation heat insulation layer, autoclave body is cylindrical container, in the outside of autoclave body
Heating device is set, thermal insulating warm-keeping layer is set in the outside of heating device, high pressure kettle cover is set in the upper surface of autoclave body, tightly
Fixing bolt passes through fixed mounting hole, is connected with autoclave body interconnecting piece, so that kettle cover is tightened to an entirety with autoclave body, and realizes
It seals, is diametrically disposed on high pressure kettle cover circular surface：Air inlet pipe hole, temperature sensor hole, working electrode hole,
Rotational axis hole, charging aperture, pressure sensor hole and outlet pore, wherein rotational axis hole are located at circle centre position, are arranged in rotational axis hole
Rotation axis, rotation axis connection control motor, and rotation axis top half is located on high pressure kettle cover, and rotation axis lower half portion is located at height
It presses in autoclave body, the lower end of rotation axis is provided with mixing component, is respectively arranged with above and below working electrode hole is adjacent
Auxiliary electrode hole and reference electrode hole, are provided with working electrode column on working electrode hole, and auxiliary is arranged on auxiliary electrode hole
Reference electrode is arranged on reference electrode hole, air inlet pipe is arranged in air inlet pipe hole, outlet is arranged in outlet pore for electrode column
Pipe, setting charging auxiliary device, pressure sensor and pressure gauge are provided on pressure sensor hole on charging aperture；
In the above-mentioned technical solutions, the lower half portion length in autoclave body that is located at of the rotation axis accounts for autoclave body height
, the mixing component is agitating paddle or stirring disk；
In the above-mentioned technical solutions, the air inlet pipe gos deep into the bottom of autoclave body, and escape pipe is located in autoclave body
It is more than liquid surface；
In the above-mentioned technical solutions, temperature sensor is connected with temperature controller, and temperature controller is connected with heating device；
In above-mentioned technical proposal, when three electrodes is arranged in three electrode holes, electrode is with the structure at high pressure kettle cover sealing,
Setting of casing, upper casing and plug are set gradually from bottom to top；
Three-electrode system includes reference electrode, working electrode column, auxiliary electrode column, working electrode stabilising arrangement and electrode
Folder, wherein reference electrode are an integral structure Ag/AgCl electrodes, and working electrode column and auxiliary electrode column have identical structure, i.e.,
Cylindrical structure is arranged metallic channel directed downwardly in the lower section of cylinder, sheet metal is arranged in metallic channel, along cylindrical center's setting
The bottom end of portion's conducting wire, inner lead is in contact with the sheet metal in metallic channel, the side setting fastening spiral shell button in the position that is in contact,
Fasten the connection that spiral shell button is used for fixing internal conducting wire and sheet metal；In order to make working electrode and reference in autoclave body under stirring
Stabilizing distance is kept, therefore working electrode auxiliary stabilizing device is set, which includes first clamping plate, second clamping plate and third clamping plate
And telescopic device, telescopic device connect into an entirety across three pieces of clamping plates, first clamping plate and third clamping plate can be along telescopic devices
It carries out, close to the activity with separate second clamping plate, secure component (not marking in figure) being arranged in first clamping plate and third clamping plate,
For strap and telescopic device, electrode holder includes stable disk, conducting wire and sheet metal, and working electrode groove is arranged in stable disk,
Working electrode sample is set in working electrode groove, and stable disk is connected by conducting wire with sheet metal, and reference electrode is fixed on the first folder
Between plate and second clamping plate, the stable disk of electrode holder is fixed between second clamping plate and third clamping plate, keeps working electrode sample flat
It is hollow structure between clamping plate facing towards reference electrode, makes to be full of experimental solutions between working electrode sample and reference electrode, gold
Belong to piece and be connected with working electrode by being inserted into the metallic channel below working electrode column, is set in the lower-lying metal slot of auxiliary electrode column
Set platinum plate electrode；
In the above-mentioned technical solutions, the working electrode is the test button of epoxy encapsulation,
In the above-mentioned technical solutions, the auxiliary electrode is the platinum plate electrode of 13 × 10 × 0.2mm, unilateral exposed surface
Product is 10 × 10mm,
In the above-mentioned technical solutions, the working electrode surface is away from reference electrode 2-5mm；
In the above-mentioned technical solutions, the working electrode auxiliary stabilizing device and electrode holder are maximum temperature 260
DEG C, maximum pressure is the polytetrafluoroethylene (PTFE) of 10Mpa；
In the above-mentioned technical solutions, the reference electrode is 310 DEG C of maximum temperature, and maximum pressure is the high temperature of 10Mpa
High pressure Ag/AgCl electrodes；
External control cabinet is connected with heating and heat-insulating device and rotation axis, and heating and thermal insulation dress can be adjusted by external control cabinet
The rotating speed of the temperature and rotation axis set；
External air supply system is connected with the air inlet pipe of device, for providing corrosive gas；
External electrochemical workstation is connected with the terminals of auxiliary electrode, reference electrode and working electrode, auxiliary for acquiring
The electrochemical signals of electrode, reference electrode and working electrode, computer are helped to be connected with external electrochemical workstation, for external
The data of electrochemical workstation acquisition are recorded, analyzing processing and output.
The test method of high temperature and pressure dynamic electrochemical testing device is as follows：
Step 1, corrosive liquid is packed into autoclave body by charging auxiliary device and charging aperture, and covers high pressure kettle cover and gives
With fixation；
Step 2, it is passed through inert gas in the corrosive liquid by air inlet pipe into autoclave body, to remove in autoclave body
Oxygen；
In step 2, inert gas is nitrogen, helium or argon gas；
In step 2, the time for being passed through inert gas is 12-24 hours, preferably 15-20 hours；
Step 3, it is passed through experimental gas in the corrosive liquid by air inlet pipe into autoclave body, so that experimental gas is filled in
Autoclave body inner space；
In step 3, the time for being passed through experimental gas is 22-24 hours, experimental gas CO2Or H2S gases；
Step 4, heating and heat-insulating device is started by external control cabinet, autoclave internal corrosion liquid is heated to setting experiment temperature
It spends and keeps the temperature, adjusting control case changes rotation rotating speed, reaches preset rotation speed；
Step 5, external electrochemical workstation is connected with working electrode, auxiliary electrode and reference electrode respectively, and receives letter
Number, proceed by experiment test.
In actual use, pressure setting, during excluding oxygen, high pressure are carried out by pressure sensor and pressure gauge
When pressure reaches preset value in kettle, it can generally assert that oxygroup originally drains；Similarly, when pressure reaches preset value in autoclave, one
As can assert that experimental gas has been filled with space in autoclave.
With the present apparatus under different rotating speeds, temperature and air pressure conditions to the electrochemical corrosion polarization curve of carbon steel A106B into
Row test, sample impregnates before testing continues 1 hour in the solution, until specimen surface system reaches dynamic stability, test result
As shown below.1 indicates static lower test in figure, and 2 indicate the lower test of dynamic.Fig. 8 is temperature 60 C, CO20.03Mpa is divided,
Polarization curve under 0m/s and 0.3m/s rotating speeds.Due to CO2Relatively low and Acclimation temperature is divided, the anode of polarization curve is propped up with activity
Based on dissolving.Meanwhile rotating speed reduces polarization curve cathode in such a way that diffusion polarization controls.Fig. 9 is 90 DEG C of temperature, CO2Point
Press 0.1Mpa, the polarization curve under 0m/s and 0.3m/s rotating speeds.Due to CO2The raising of partial pressure, the anode branch and Fig. 8 of polarization curve
It compares, slight deactivation phenomenon occurs, this is because raising and the CO of temperature2The raising of partial pressure accelerates specimen surface corrosive film
Formation, it can be seen that the passivation phenomenon of the lower specimen surface of static state becomes apparent from.The raising and dynamic test of temperature are so that polarization is bent
Line cathode is no longer carried out with polarization curve cathode.Figure 10 is 90 DEG C of temperature, and CO2 divides 0.2Mpa, under 0m/s and 0.5m/s rotating speeds
Polarization curve.Test result and Fig. 9 are close under this condition, are that anode surface slight deactivation occurs, cathode turns to electrochemistry
Polarizing control.Figure 11 is 90 DEG C of temperature, CO2Divide 0.5Mpa, the polarization curve under 0m/s and 1m/s rotating speeds.Due to CO2Partial pressure carries
Height, anode branch passivation phenomenon is apparent, and cathode is carried out with activation polarization control mode.
It describes the invention in detail, but content is only the preferred embodiment of the present invention, cannot be recognized above
For the practical range for limiting the present invention.Any changes and modifications in accordance with the scope of the present application should all still return
Belong within the patent covering scope of the present invention.
Claims (8)
1. the method tested using dynamic electrochemical appliance, which is characterized in that dynamic electrochemical appliance includes high temperature and pressure
Reaction kettle, three-electrode system, external control cabinet, external air supply system, external electrochemical workstation and computer；High temperature high pressure reverse
Answer kettle include autoclave body, high pressure kettle cover, air inlet pipe, escape pipe, rotation axis, pressure sensor, pressure gauge, temperature sensor,
Heating device and heat preservation heat insulation layer, autoclave body is cylindrical container, and heating device is arranged in the outside of autoclave body, is heating
Thermal insulating warm-keeping layer is arranged in the outside of device, high pressure kettle cover is arranged in the upper surface of autoclave body, fastening bolt, which passes through, to be fixedly mounted
Hole is connected with autoclave body interconnecting piece, so that kettle cover is tightened to an entirety with autoclave body, and realizes sealing, and high pressure kettle cover is round
It is diametrically disposed on surface：Air inlet pipe hole, temperature sensor hole, working electrode hole, rotational axis hole, charging aperture,
Pressure sensor hole and outlet pore, wherein rotational axis hole are located at circle centre position, and rotation axis is arranged in rotational axis hole, rotates axis connection
Motor is controlled, rotation axis top half is located on high pressure kettle cover, and rotation axis lower half portion is located in autoclave body, in rotation axis
Lower end be provided with mixing component, be respectively arranged with above and below working electrode hole is adjacent auxiliary electrode hole and reference electricity
Pole hole is provided with working electrode column on working electrode hole, auxiliary electrode column is arranged on auxiliary electrode hole, in reference electrode hole
Upper setting reference electrode, air inlet pipe hole is interior to be arranged air inlet pipe, escape pipe is arranged in outlet pore, tracheae gos deep into autoclave body
Bottom, escape pipe are located in autoclave body more than liquid surface, the setting charging auxiliary device on charging aperture, in pressure sensor
Pressure sensor and pressure gauge are provided on hole, temperature sensor is connected with temperature controller, temperature controller and heating device
It is connected；
Three-electrode system includes reference electrode, working electrode column, auxiliary electrode column, working electrode stabilising arrangement and electrode holder,
Middle reference electrode is an integral structure Ag/AgCl electrodes, and working electrode column and auxiliary electrode column have identical structure, i.e. cylinder
Structure is arranged metallic channel directed downwardly in the lower section of cylinder, sheet metal is arranged in metallic channel, is led along cylindrical center's setting inside
The bottom end of line, inner lead is in contact with the sheet metal in metallic channel, the side setting fastening spiral shell button in the position that is in contact, fastening
Spiral shell button is used for the connection of fixing internal conducting wire and sheet metal；In order to make working electrode be kept under stirring in autoclave body with reference
Stabilizing distance, therefore working electrode auxiliary stabilizing device is set, which includes first clamping plate, second clamping plate and third clamping plate and stretches
Compression apparatus, telescopic device connect into an entirety across three pieces of clamping plates, and first clamping plate and third clamping plate can be carried out along telescopic device
Close to far from second clamping plate activity, secure component is set in first clamping plate and third clamping plate, for strap with stretch
Compression apparatus, electrode holder include stable disk, conducting wire and sheet metal, and working electrode groove is arranged in stable disk, is arranged in working electrode groove
Working electrode sample, stable disk are connected by conducting wire with sheet metal, and reference electrode is fixed between first clamping plate and second clamping plate,
The stable disk of electrode holder is fixed between second clamping plate and third clamping plate, makes working electrode sample plane towards reference electrode, folder
It is hollow structure between plate, makes to be full of experimental solutions between working electrode sample and reference electrode, sheet metal is by being inserted into work
Metallic channel below electrode column is connected with working electrode, and platinum plate electrode is arranged in the lower-lying metal slot of auxiliary electrode column；
External control cabinet is connected with heating and heat-insulating device and rotation axis, and heating and heat-insulating device can be adjusted by external control cabinet
The rotating speed of temperature and rotation axis；
External air supply system is connected with the air inlet pipe of device, for providing corrosive gas；
External electrochemical workstation is connected with the terminals of auxiliary electrode, reference electrode and working electrode, for acquiring auxiliary electricity
Pole, reference electrode and working electrode electrochemical signals, computer is connected with external electrochemical workstation, for external electrification
The data for learning workstation collection are recorded, analyzing processing and output；It is being tested, is being carried out as steps described below：
Step 1, corrosive liquid is packed into autoclave body by charging auxiliary device and charging aperture, and covers high pressure kettle cover and is consolidated
It is fixed；
Step 2, it is passed through inert gas in the corrosive liquid by air inlet pipe into autoclave body, to remove the oxygen in autoclave body；
Step 3, it is passed through experimental gas in the corrosive liquid by air inlet pipe into autoclave body, so that experimental gas is filled in high pressure
Autoclave body inner space；
Step 4, heating and heat-insulating device is started by external control cabinet, autoclave internal corrosion liquid is heated to setting experimental temperature simultaneously
Heat preservation, adjusting control case change rotation rotating speed, reach preset rotation speed；
Step 5, external electrochemical workstation is connected with working electrode, auxiliary electrode and reference electrode respectively, and receives signal, opens
Begin to carry out experiment test.
2. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that in step 2
In, the inert gas is nitrogen, helium or argon gas, and the time for being passed through inert gas is 12-24 hours, preferably 15-20
Hour.
3. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that in step 3
In, the experimental gas is CO2Or H2S gases, the time for being passed through experimental gas are 22-24 hours.
4. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that described turns
The lower half portion length in autoclave body that is located at of moving axis accounts for the 1/3-1/2 of autoclave body height, the mixing component be agitating paddle or
Stir disk.
5. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that the work
Make electrode surface away from reference electrode 2-5mm.
6. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that described is auxiliary
It is the platinum plate electrode of 13 × 10 × 0.2mm to help electrode, and unilateral bare area is 10 × 10mm.
7. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that the ginseng
It is 310 DEG C of maximum temperature than electrode, maximum pressure is the high temperature and pressure Ag/AgCl electrodes of 10Mpa.
8. the method according to claim 1 tested using dynamic electrochemical appliance, which is characterized in that the work
It is 260 DEG C of maximum temperature to make electrode auxiliary stabilizing device and electrode holder, and maximum pressure is the polytetrafluoroethylene (PTFE) of 10Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810204840.8A CN108680491B (en) | 2016-05-16 | 2016-05-16 | Method for testing using dynamic electrochemical device |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810204840.8A CN108680491B (en) | 2016-05-16 | 2016-05-16 | Method for testing using dynamic electrochemical device |
| CN201610322136.3A CN105806774B (en) | 2016-05-16 | 2016-05-16 | High-temperature high-pressure dynamic electrochemical test experimental device and test method |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN111024604A (en) * | 2019-12-19 | 2020-04-17 | 韦正楠 | Corrosion and scaling experiment detection system and method for geothermal water heat exchange process |
| CN112213256A (en) * | 2020-10-09 | 2021-01-12 | 西南石油大学 | Testing arrangement of bacterium to steel corrosion influence under oil gas pipeline cathodic polarization |
| CN112986111A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Catalytic wet oxidation corrosion experiment device |
| CN113834765A (en) * | 2020-06-08 | 2021-12-24 | 中国石油化工股份有限公司 | Device and method for testing corrosion resistance of material |
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| CN105806774B (en) | 2018-07-03 |
| CN105806774A (en) | 2016-07-27 |
| CN108519324B (en) | 2020-05-08 |
| CN108680491B (en) | 2020-05-08 |
| CN108519324A (en) | 2018-09-11 |
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