CN104502264B - Top-corrosion electrochemical testing device in high-temperature and high-pressure environments - Google Patents
Top-corrosion electrochemical testing device in high-temperature and high-pressure environments Download PDFInfo
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- CN104502264B CN104502264B CN201410805227.3A CN201410805227A CN104502264B CN 104502264 B CN104502264 B CN 104502264B CN 201410805227 A CN201410805227 A CN 201410805227A CN 104502264 B CN104502264 B CN 104502264B
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Abstract
The invention provides a top-corrosion electrochemical testing device in high-temperature and high-pressure environments, belongs to the field of corrosive electrochemistry, and is suitable for top-corrosion simulation experiments and corrosion behavior mechanism research in high-temperature and high-pressure working conditions. The top-corrosion electrochemical testing device comprises a high-temperature and high-pressure reaction kettle, a heating and heat preservation system, a circulating condensate water tank refrigerating system, a three-electrode system, a signal conduction pathway, a control box, an external air supply system and a computer. The device has the advantages that actual high-temperature and high-pressure working conditions can be achieved; top-corrosion in-situ electrochemical signal testing can be carried out; and the method is of great significance on mechanism research on high-temperature and high-pressure top-corrosion behaviors and electrochemical reaction.
Description
Technical field
The present invention relates to corrosion electrochemistry field, particularly relate to a kind of corrosion electrochemistry test of high temperature and high pressure environment next top
Device.
Background technology
In recent years, increasingly increase with oil-gas field development industry, the pipeline of conveying oil gas there occurs a lot of failure accidents, top
Portion's corrosion is a wherein important part, can carry out grinding of top part corrosion electrochemical in-situ test therefore under high-temperature and high-pressure conditions
Study carefully and also receive much concern.Up to the present, the electrochemical corrosion apparatus for studying Pipeline Steel in Wet Natural Gas top do not occur, the present invention
It is the relatively advanced equipment in this one side.In oil and gas industry exploitation and course of conveying, the corrosive medium bag that relates generally to
Include CO2The organic acid containing Deng sour gas and water and part.Carrying out High Temperature High Pressure top part corrosion simulation experiment is research pipe
The important means of the corrosion resistance of line Steel material, corrosion mechanism and evaluation.Therefore, it is necessary to there be the high temperature that can simulate under physical condition
The device of high pressure top electrochemical corrosion experimental.But due under high-temperature and high-pressure conditions, to working electrode, reference electrode and auxiliary electricity
The structures such as pole and pressure bearing and seal have very high requirement it is not easy to realize the output of electrochemical signals.Generally, in High Temperature High Pressure
After being simulated experiment in reactor, then carry out electro-chemical test in static synthesis under normal pressure container, actual feelings can not be drawn
Electrochemical corrosion behavior in the corrosion process of condition next top.Due to the shortage of measurement High Temperature High Pressure top electrochemical signals, impact
Further investigation to High Temperature High Pressure top part corrosion behavior and mechanism.Therefore the present invention can fill up this vacancy, to a certain degree
Upper is to carry out in-depth study to establish equipment Foundations.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of high temperature and high pressure environment next top corrosion electrochemical test system,
The electrochemical corrosion performance testing at high-temperature and high-pressure conditions underground pipelines steel dampness top is solved the problems, such as with this.
This device includes high-temperature high-pressure reaction kettle, heating and thermal insulation system, circulating condensing Water tank refrigeration system, three electrode systems
System, working electrode signal transduction pathway, external control chamber, external air supply system and computer；Wherein, high-temperature high-pressure reaction kettle bag
Include high pressure kettle cover, kettle handle, autoclave body, relief valve, pressure display instrument, pressure transducer, air inlet and gas outlet, heating is protected
Warm system include thermoelectricity on a rare occasion, thermocouple two and temperature sensor, circulating condensing Water tank refrigeration system include cooling water circulation enter
The mouth of a river, cooling water circulation outlet and condensation water tank, three-electrode system includes Ag/AgCl reference electrode, working electrode, auxiliary electricity
Pole.External control chamber includes temperature in the kettle control instrument and pressure display instrument, and external air supply system includes gas cylinder, decompression
Valve, airway and control valve；Bolt hole is had on autoclave lid, autoclave body is connected by fastening bolt with high pressure kettle cover,
Centre is lined with rubber seal rings for seal；Autoclave body inner bottom part equipped with thermoelectricity on a rare occasion with thermocouple two, autoclave body internal upper part fill
Have condensation water tank, condensation water tank bottom equipped with three-electrode system, and pass through wire, by Ag/AgCl reference electrode, working electrode and
Auxiliary electrode guides to condensation water tank top, leads through Ag/AgCl reference electrode wire guide, working electrode wire guide, auxiliary electrode
String holes stretches out high pressure kettle cover, and autoclave lid separately has cooling water circulation inlet opening and cooling water circulation water outlet oral pore, for cooling
Water circulation water inlet and cooling water circulation outlet stretch out；Air inlet and the gas outlet of level is left on autoclave body top, gives vent to anger
Mouth connects control valve, and air inlet is sequentially connected relief valve, pressure display instrument and control valve.
Wherein, temperature sensor, thermoelectricity are on a rare occasion, thermocouple two and external control chamber connected by wire, by thermocouple
First, thermocouple two and temperature sensor make solution in kettle reach design temperature；The air relief valve of external air supply system gas cylinder, lead
It is threaded connection between trachea and the air inlet of autoclave, the experimental gas of external air supply system output pass through air relief valve pressure control
Entered in high-temperature high-pressure reaction kettle by airway afterwards, produce simulation experiment gas pressure intensity；Ag/AgCl reference electrode, auxiliary electricity
Pole and working electrode epoxy packages, and will be smooth with sand papering for packaged sample in annular clip, make at three electrodes
In approximately the same plane, then it is connected with external electrochemical workstation by wire；Three-electrode system passes through working electrode signal
Pathway is connected with external electrochemical workstation, carries out electro-chemical test, and external electrochemical workstation is connected computer and carried out
Data output, record and analyzing and processing；Pressure within autoclave body passes through pressure transducer and pressure gauge shows, and by control
Valve processed is adjusted, once exceeding the rated value of kettle pressure-bearing, relief valve would automatically turn on, the safety of protection whole system
Property.
The having the beneficial effect that of the technique scheme of the present invention：
This device has simple to operate, adaptable feature, compensate for the not enough shortcoming of top part corrosion research equipment.Can
More really to simulate actual working conditions, realize the corrosive environment at High Temperature High Pressure top, this invention can be deep to top part corrosion
The study mechanism entering provides equipment Foundations.Three-electrode system in this equipment is by working electrode (pipe line steel), reference electrode
(Ag/AgCl), auxiliary electrode (rustless steel) composition.This device has certain initiative, and experimental result also demonstrate that it
Reliability.
Brief description
Fig. 1 is the high temperature and high pressure environment next top corrosion electrochemical test system high pressure kettle cover structural representation of the present invention；
Fig. 2 is the high-temperature high-pressure reaction kettle structural representation of A-A section in Fig. 1；
Fig. 3 is three-electrode system schematic diagram of the present invention.
In figure：
1- working electrode；2-Ag/AgCl reference electrode；The cooling water circulation water inlet of 3-；4- fastening bolt；5- gas outlet；
6- rubber seal；7- autoclave body；8- thermoelectricity is on a rare occasion；9- temperature in the kettle control instrument；10- thermocouple two；11- tri- electrode system
System；12- condensation water tank；The external air supply system of 13-；14- control valve；15- pressure display instrument；16- relief valve；17- air inlet；
The cooling water circulation outlet of 18-；19- auxiliary electrode；20- kettle handle；21- bolt hole；The cooling water circulation inlet opening of 22-；23-
Ag/AgCl reference electrode wire guide；24- auxiliary electrode wire guide；25- high pressure kettle cover；26- working electrode wire guide；27- cools down
Water circulation water outlet oral pore.
Specific embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of high temperature and high pressure environment next top corrosion electrochemical test system, and this device includes High Temperature High Pressure
Reactor, heating and thermal insulation system, circulating condensing Water tank refrigeration system, three-electrode system 11, working electrode signal transduction pathway, outer
Connect control chamber, external air supply system and computer；High-temperature high-pressure reaction kettle includes high pressure kettle cover 25, kettle handle 20, autoclave body
7th, relief valve 16, pressure display instrument 15, pressure transducer, air inlet 17 and gas outlet 5, heating and thermal insulation system includes thermoelectricity on a rare occasion
8th, thermocouple 2 10 and temperature sensor, circulating condensing Water tank refrigeration system includes cooling water circulation water inlet 3, cooling water circulation
Outlet 18 and condensation water tank 12, three-electrode system 11 includes Ag/AgCl reference electrode 2, working electrode 1, auxiliary electrode 19.Outward
Connect control chamber and include temperature in the kettle control instrument 9 and pressure display instrument 15, external air supply system 13 includes gas cylinder, decompression
Valve, airway and control valve 14.
It is illustrated in figure 1 the high pressure kettle cover structural representation of this device, high pressure kettle cover 25 is provided with kettle handle 20, bolt hole
21, and have working electrode wire guide 26, Ag/AgCl reference electrode wire guide 23, auxiliary electrode wire guide 24, cooling water circulation
Inlet opening 22, cooling water circulation water outlet oral pore 27, gas outlet 5 and air inlet 17.
It is illustrated in figure 2 the structure overall schematic of this device A-A section along along Fig. 1, autoclave body 7 and high pressure kettle cover 25
Connected by fastening bolt 4, centre is lined with rubber seal 6 and seals；Autoclave body 7 inner bottom part is equipped with thermoelectricity on a rare occasion 8 and thermoelectricity
Even 2 10, equipped with condensation water tank 12, condensation water tank 12 bottom is equipped with three-electrode system 11, and passes through to lead for autoclave body 7 internal upper part
Line, Ag/AgCl reference electrode 2, working electrode 1 and auxiliary electrode 19 is guided to condensation water tank 12 top, is led by working electrode
String holes 26, Ag/AgCl reference electrode wire guide 23, auxiliary electrode wire guide 24 stretch out high pressure kettle cover 25, another on high pressure kettle cover 25
Holes, Cooling Water circulation water inlet 3 and cooling water circulation outlet 18 is had to stretch out；Entering of level is left on autoclave body 7 top
QI KOU 17 and gas outlet 5, gas outlet 5 connects control valve, and air inlet 17 is sequentially connected relief valve 16, pressure display instrument 15 and control
Valve 14 processed.
Wherein, temperature sensor, thermoelectricity on a rare occasion 8, thermocouple 2 10 and external control chamber are connected by wire；External supply
It is threaded connection between the air inlet 17 of the air relief valve of system high pressure gas cylinder, airway and autoclave, external air supply system is defeated
The experimental gas going out are entered in high-temperature high-pressure reaction kettle by airway after air relief valve pressure control, produce simulation experiment gas pressure
By force；As shown in figure 3, Ag/AgCl reference electrode 2, auxiliary electrode 19 and working electrode 1 are used epoxy packages in annular clip,
And will be smooth with sand papering for packaged sample, so that three electrodes is in approximately the same plane, then pass through wire and external electricity
Chem workstation connects；Three-electrode system 11 is connected with external electrochemical workstation by working electrode signal transduction pathway, enters
Row electro-chemical test, external electrochemical workstation is connected computer and is carried out data output, record and analyzing and processing；Autoclave body 7
Internal pressure passes through pressure transducer and pressure display instrument 15 shows, and is adjusted by control valve 14.
In application process, first according to preparing three-electrode system 11 sample shown in Fig. 3, by working electrode 1, Ag/AgCl
Reference electrode 2, auxiliary electrode 19 epoxy resin, dibutyl phthalate second two fat, ethylenediamine are according to 100:10:7 ratio
Example mixed preparing epoxy packages in fixture, with using alcohol washes, acetone oil removing after-blow after liquid honing to 800#
Dry standby.Pull down fastening bolt 4, open high pressure kettle cover 25, packaged three-electrode system 11 is fastened on condensation water tank 12
Bottom, and applying silica gel about with anti-gas-leak.The three of the wires connecting three-electrode system 11 is penetrated working electrode wire guide
(26), Ag/AgCl reference electrode wire guide (23), in auxiliary electrode wire guide (24) in case connecting external electrochemical workstation.
Water will be filled in condensation water tank 11.Pour the simulation medium solution of certain volume into into autoclave body 7, solution must not be allowed to cover cold
The bottom of condensation tank 12, to maintain a top part corrosion environment.Cover high pressure kettle cover 25, tighten fastening bolt 4.Enter from autoclave
QI KOU 17 is passed through gas N2Deoxygenation more than 8 hours, then passes to experimental gas (as CO2Gas) reach the pressure of setting.Open control
The heating and thermal insulation system control switch of case processed, in heating autoclave, solution to setting experimental temperature and is incubated.Open circulating condensing
Water tank pump switch, sets condensation temperature, makes cooling water circulation flowing.After temperature and pressure reaches setting value, system meeting
Maintain in this state, three electrode cables are connected with external telephoning telephony work station and can achieve electrochemical data output, record, place
The function such as reason and analysis.
The above is the preferred embodiment of the present invention it is noted that for those skilled in the art
For, on the premise of without departing from principle of the present invention, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (6)
1. high temperature and high pressure environment next top corrosion electrochemical test system it is characterised in that：This device includes high-temperature high-voltage reaction
Kettle, heating and thermal insulation system, circulating condensing Water tank refrigeration system, three-electrode system (11), working electrode signal transduction pathway, external
Control chamber, external air supply system and computer；Wherein, high-temperature high-pressure reaction kettle includes high pressure kettle cover (25), kettle handle (20), height
Pressure kettle (7), relief valve (16), pressure display instrument (15), pressure transducer, air inlet (17) and gas outlet (5), heating and thermal insulation
System includes thermoelectricity on a rare occasion (8), thermocouple two (10) and temperature sensor, and circulating condensing Water tank refrigeration system includes cooling water and follows
Ring water inlet (3), cooling water circulation outlet (18) and condensation water tank (12), three-electrode system (11) includes Ag/AgCl reference
Electrode (2), working electrode (1) and auxiliary electrode (19)；External control chamber includes temperature in the kettle control instrument (9) and pressure shows
Instrument (15), external air supply system (13) includes gas cylinder, air relief valve, airway and control valve (14)；High pressure kettle cover (25)
On have bolt hole (21), autoclave body (7) is connected by fastening bolt (4) with high pressure kettle cover (25), and it is close that centre is lined with rubber
Seal (6) seals；Autoclave body (7) inner bottom part is equipped with thermoelectricity on a rare occasion (8) and thermocouple two (10), autoclave body (7) internal upper part
Equipped with condensation water tank (12), condensation water tank (12) bottom is equipped with three-electrode system (11), and passes through wire, by Ag/AgCl reference
Electrode (2), working electrode (1) and auxiliary electrode (19) guide to condensation water tank (12) top, through Ag/AgCl reference electrode wire
Hole (23), working electrode wire guide (26), auxiliary electrode wire guide (24) stretch out high pressure kettle cover (25), and high pressure kettle cover (25) is upper another
Have cooling water circulation inlet opening (22) and a cooling water circulation water outlet oral pore (27), Cooling Water circulation water inlet (3) and cold
But water circulation outlet (18) stretches out；Air inlet (17) and gas outlet (5) of level, gas outlet are left in autoclave body (7) top
(5) connect control valve, air inlet (17) is sequentially connected relief valve (16), pressure display instrument (15) and control valve (14).
2. high temperature and high pressure environment next top corrosion electrochemical test system according to claim 1 it is characterised in that：Described
Temperature sensor, thermoelectricity on a rare occasion (8), thermocouple two (10) and external control chamber are connected by wire.
3. high temperature and high pressure environment next top corrosion electrochemical test system according to claim 1 it is characterised in that：Described
It is threaded connection between the air inlet (17) of the air relief valve, airway and autoclave of external air supply system gas cylinder, external
The experimental gas of air supply system output are entered in high-temperature high-pressure reaction kettle by airway after air relief valve pressure control, produce simulation
Experimental gas pressure.
4. high temperature and high pressure environment next top corrosion electrochemical test system according to claim 1 it is characterised in that：Described
Ag/AgCl reference electrode (2), auxiliary electrode (19) and working electrode (1) are encapsulated in annular clip, and by packaged sample
Smooth with sand papering, so that three electrodes is in approximately the same plane, be then connected with external electrochemical workstation by wire.
5. high temperature and high pressure environment next top corrosion electrochemical test system according to claim 1 it is characterised in that：Described
Three-electrode system (11) is connected with external electrochemical workstation by working electrode signal transduction pathway, carries out electro-chemical test,
External electrochemical workstation is connected computer and is carried out data output, record and analyzing and processing.
6. high temperature and high pressure environment next top corrosion electrochemical test system according to claim 1 it is characterised in that：Described
The internal pressure of autoclave body (7) passes through pressure transducer and pressure display instrument (15) display, and is entered by control valve (14)
Row is adjusted.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410805227.3A CN104502264B (en) | 2014-12-19 | 2014-12-19 | Top-corrosion electrochemical testing device in high-temperature and high-pressure environments |
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| CN201410805227.3A CN104502264B (en) | 2014-12-19 | 2014-12-19 | Top-corrosion electrochemical testing device in high-temperature and high-pressure environments |
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| CN104502264B true CN104502264B (en) | 2017-02-22 |
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| CN105699286B (en) * | 2016-04-06 | 2018-09-14 | 北京科技大学 | A kind of moisture loop top part corrosion test device |
| CN106706511B (en) * | 2017-02-16 | 2023-08-11 | 天津大学 | Electrochemical reaction kettle with two open sides and application method thereof |
| 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 |
| CN108932986B (en) * | 2018-07-06 | 2020-01-14 | 中国核动力研究设计院 | High-temperature high-pressure reaction kettle suitable for hot chamber irradiation environment and test method |
| CN109541084B (en) * | 2018-11-28 | 2021-11-16 | 湖北航天化学技术研究所 | Device for dynamically analyzing and detecting gas-phase product |
| CN109682937B (en) * | 2019-03-04 | 2024-02-06 | 中国科学院地球化学研究所 | Large-cavity high-temperature high-pressure gas-liquid two-phase flow experimental device and experimental method |
| CN109994231B (en) * | 2019-04-28 | 2023-04-25 | 东华理工大学 | Radiation corrosion testing device and testing method |
| CN110243754A (en) * | 2019-07-10 | 2019-09-17 | 北京科技大学 | The top part corrosion test macro and method that wind field regulates and controls in kettle based on rotating circular disk |
| CN110243755B (en) * | 2019-07-10 | 2023-12-22 | 北京科技大学 | Top corrosion test system and test method for variable wind field regulation in autoclave |
| CN111678859B (en) * | 2020-07-08 | 2023-05-16 | 中国石油大学(华东) | Device for simulating partial corrosion of top in wet gas conveying pipeline |
| CN111678860B (en) * | 2020-07-21 | 2023-04-14 | 中国海洋石油集团有限公司 | High-temperature high-pressure corrosion electrochemical testing device with controllable corrosion environment and testing method |
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| US5323429A (en) * | 1993-01-15 | 1994-06-21 | Westinghouse Electric Corporation | Electrochemical monitoring of vessel penetrations |
| CN2779387Y (en) * | 2005-03-25 | 2006-05-10 | 北京科技大学 | Experimental apparatus for dynamic high-temperature high-pressure electrochemical test |
| CN101520402A (en) * | 2009-02-24 | 2009-09-02 | 上海大学 | Experimental facility for testing electrochemical signals of various materials in high-temperature high-pressure environment |
| CN101865816A (en) * | 2010-05-28 | 2010-10-20 | 北京科技大学 | Experimental apparatus for high-temperature high-pressure loop spray corrosion simulation and electrochemical testing |
| CN203337521U (en) * | 2013-07-18 | 2013-12-11 | 北京科技大学 | High-temperature high-pressure dynamic electrochemical testing and pH in-situ monitoring testing device |
| CN204287006U (en) * | 2014-12-19 | 2015-04-22 | 北京科技大学 | High temperature and high pressure environment next top corrosion electrochemical test system |
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Owner name: ANKE PIPING ENGINEERING SCIENCE AND TECHNOLOGY CO. Effective date: 20150317 |
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Effective date of registration: 20150317 Address after: 100083 Haidian District, Xueyuan Road, No. 30, Applicant after: University of Science and Technology Beijing Applicant after: Anke Piping Engineering Science and Technology Co., Ltd., Beijing Address before: 100083 Haidian District, Xueyuan Road, No. 30, Applicant before: University of Science and Technology Beijing |
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