CN104502264A - 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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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, refer to a kind of high temperature and high pressure environment next top corrosion electrochemical test system especially.
Background technology
In recent years, along with oil-gas field development industry increases day by day, the pipeline of conveying oil gas there occurs a lot of failure accidents, and top part corrosion is a wherein important part, and the research therefore can carrying out the test of top part corrosion electrochemical in-situ under high-temperature and high-pressure conditions also receives much concern.Up to the present, do not occur for the electrochemical corrosion apparatus studying Pipeline Steel in Wet Natural Gas top, the present invention is the comparatively advanced equipment in this one side.In oil and gas industry exploitation and course of conveying, the corrosive medium related generally to comprises CO
2deng the organic acid that sour gas and water and part contain.Carry out the important means of corrosion stability that the simulated experiment of High Temperature High Pressure top part corrosion is research pipe line steel material, corrosion mechanism and evaluation.Therefore, the device of the High Temperature High Pressure top electrochemical corrosion experimental can simulated under physical condition must be had.But due under high-temperature and high-pressure conditions, there is very high requirement to the structures such as working electrode, contrast electrode and auxiliary electrode and pressure bearing and seal, be not easy the output realizing electrochemical signals.Usually, carry out simulated experiment in high-temperature high-pressure reaction kettle after, then carry out electro-chemical test in static synthesis under normal pressure container, the galvanic corrosion behavior in the corrosion process of actual conditions next top can not be drawn.Owing to measuring the shortage of High Temperature High Pressure top electrochemical signals, have impact on the further investigation to the behavior of High Temperature High Pressure top part corrosion and mechanism.Therefore the present invention can fill up this vacancy, establishes equipment Foundations to a certain extent for carrying out deep research.
Summary 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, solves the problem of the galvanic corrosion performance testing at high-temperature and high-pressure conditions underground pipelines steel moisture top with this.
This device comprises high-temperature high-pressure reaction kettle, heating and thermal insulation system, circulating condensing Water tank refrigeration system, three-electrode system, working electrode signal transduction pathway, external control box, external air supply system and computing machine; Wherein, high-temperature high-pressure reaction kettle comprises high pressure kettle cover, still handle, autoclave body, safety valve, pressure display instrument, pressure transducer, air intake opening and gas outlet, heating and thermal insulation system comprise thermoelectricity on a rare occasion, thermopair two and temperature sensor, circulating condensing Water tank refrigeration system comprises cooling water circulation water inlet, cooling water circulation water delivering orifice and condensation water tank, and three-electrode system comprises Ag/AgCl contrast electrode, working electrode, auxiliary electrode.External control box comprises temperature in the kettle control instrument and pressure display instrument, and external air supply system comprises gas cylinder, reduction valve, wireway and by-pass valve control; Autoclave covers and has bolt hole, and autoclave body is connected by fastening bolt with high pressure kettle cover, and centre is lined with rubber seal rings for seal; Autoclave body inner bottom part be equipped with thermoelectricity on a rare occasion with thermopair two, autoclave body internal upper part is equipped with condensation water tank, bottom condensation water tank, three-electrode system is housed, and pass through wire, Ag/AgCl contrast electrode, working electrode and auxiliary electrode are guided to condensation water tank top, high pressure kettle cover is stretched out through Ag/AgCl contrast electrode wire guide, working electrode wire guide, auxiliary electrode wire guide, autoclave covers separately cooling water circulation inlet opening and cooling water circulation water outlet oral pore, and Cooling Water circulation water inlet and cooling water circulation water delivering orifice stretch out; Air intake opening and the gas outlet of level are left in autoclave body top, and gas outlet connection control valve, air intake opening is connection safety valve, pressure display instrument and by-pass valve control successively.
Wherein, temperature sensor, thermoelectricity are on a rare occasion, thermopair two is connected by wire with external control box, by thermoelectricity on a rare occasion, thermopair two and temperature sensor make solution in still reach design temperature; The reduction valve of external air supply system gas cylinder, to be threaded connection between wireway and the air intake opening of autoclave, the experimental gas that external air supply system exports, by entering in high-temperature high-pressure reaction kettle by wireway after reduction valve pressure control, produces simulated experiment gas pressure intensity; Ag/AgCl contrast electrode, auxiliary electrode and working electrode epoxy packages in annular clip, and by smooth for packaged sample sand papering, made three electrodes be in same plane, are then connected with external electrochemical workstation by wire; Three-electrode system is connected with external electrochemical workstation by working electrode signal transduction pathway, carries out electro-chemical test, and external electrochemical workstation is connected computing machine and carried out data output, record and analyzing and processing; The pressure of autoclave body inside by pressure transducer and tensimeter display, and is regulated by by-pass valve control, once exceed the ratings of kettle pressure-bearing, safety valve will be opened automatically, the security of protection whole system.
The beneficial effect of technique scheme of the present invention is as follows:
This device has simple to operate, adaptable feature, compensate for the shortcoming of top part corrosion research equipment deficiency.Can simulate actual working conditions comparatively really, realize the corrosion environment at High Temperature High Pressure top, this invention can provide equipment Foundations to the study mechanism that top part corrosion is deep.Three-electrode system in this equipment is by working electrode (pipe line steel), and contrast electrode (Ag/AgCl), auxiliary electrode (stainless steel) forms.This device has certain initiative, and experimental result also demonstrate that its reliability.
Accompanying drawing explanation
Fig. 1 is high temperature and high pressure environment next top of the present invention corrosion electrochemical test system high pressure kettle cover structural representation;
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 contrast electrode; 3-cooling water circulation water inlet; 4-fastening bolt; 5-gas outlet; 6-rubber seal; 7-autoclave body; 8-thermoelectricity on a rare occasion; 9-temperature in the kettle control instrument; 10-thermopair two; 11-three-electrode system; 12-condensation water tank; The external air supply system of 13-; 14-by-pass valve control; 15-pressure display instrument; 16-safety valve; 17-air intake opening; 18-cooling water circulation water delivering orifice; 19-auxiliary electrode; 20-still handle; 21-bolt hole; 22-cooling water circulation inlet opening; 23-Ag/AgCl contrast electrode wire guide; 24-auxiliary electrode wire guide; 25-high pressure kettle cover; 26-working electrode wire guide; 27-cooling water circulation water outlet oral pore.
Embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearly, be described in detail below in conjunction with the accompanying drawings and the specific embodiments.
The invention provides a kind of high temperature and high pressure environment next top corrosion electrochemical test system, this device comprises high-temperature high-pressure reaction kettle, heating and thermal insulation system, circulating condensing Water tank refrigeration system, three-electrode system 11, working electrode signal transduction pathway, external control box, external air supply system and computing machine; High-temperature high-pressure reaction kettle comprises high pressure kettle cover 25, still handle 20, autoclave body 7, safety valve 14, pressure display instrument 15, pressure transducer, air intake opening 17 and gas outlet 5, heating and thermal insulation system comprise thermoelectricity on a rare occasion 8, thermopair 2 10 and temperature sensor, circulating condensing Water tank refrigeration system comprises cooling water circulation water inlet 3, cooling water circulation water delivering orifice 18 and condensation water tank 12, and three-electrode system 11 comprises Ag/AgCl contrast electrode 2, working electrode 1, auxiliary electrode 19.External control box comprises temperature in the kettle control instrument 9 and pressure display instrument 15, and external air supply system 13 comprises gas cylinder, reduction valve, wireway and by-pass valve control 14.
Be illustrated in figure 1 the high pressure kettle cover structural representation of this device, high pressure kettle cover 25 is provided with still handle 20, bolt hole 21, and has working electrode wire guide 26, Ag/AgCl contrast 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 intake opening 17.
Be illustrated in figure 2 the structure overall schematic of this device along A-A section in Fig. 1, autoclave body 7 is connected by fastening bolt 4 with high pressure kettle cover 25, and 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 thermopair 2 10, autoclave body 7 internal upper part is equipped with condensation water tank 12, three-electrode system 11 is housed bottom condensation water tank 12, and pass through wire, Ag/AgCl contrast electrode 2, working electrode 1 and auxiliary electrode 19 are guided to condensation water tank 12 top, high pressure kettle cover 25 is stretched out by working electrode wire guide 26, Ag/AgCl contrast electrode wire guide 23, auxiliary electrode wire guide 24, high pressure kettle cover 25 separately has holes, and Cooling Water circulation water inlet 3 and cooling water circulation water delivering orifice 18 stretch out; Air intake opening 17 and the gas outlet 5 of level are left in autoclave body 7 top, gas outlet 5 connection control valve, and air intake opening 17 is connection safety valve 16, pressure display instrument 15 and by-pass valve control 14 successively.
Wherein, temperature sensor, thermoelectricity are on a rare occasion 8, thermopair 2 10 is connected by wire with external control box; The reduction valve of external air supply system gas cylinder, to be threaded connection between wireway and the air intake opening 17 of autoclave, the experimental gas that external air supply system exports, by entering in high-temperature high-pressure reaction kettle by wireway after reduction valve pressure control, produces simulated experiment gas pressure intensity; As shown in Figure 3, use epoxy packages in annular clip Ag/AgCl contrast electrode 2, auxiliary electrode 19 and working electrode 1, and by smooth for packaged sample sand papering, make three electrodes be in same plane, be then connected with external electrochemical workstation by wire; Three-electrode system 11 is connected with external electrochemical workstation by working electrode signal transduction pathway, carries out electro-chemical test, and external electrochemical workstation is connected computing machine and carried out data output, record and analyzing and processing; The pressure of autoclave body 7 inside is shown by pressure transducer and pressure display instrument 15, and is regulated by by-pass valve control 14.
In application process, first according to preparing three-electrode system 11 sample shown in Fig. 3, by working electrode 1, Ag/AgCl contrast electrode 2, auxiliary electrode 19 epoxy resin, dibutyl phthalate second two fat, ethylenediamine according to the epoxy packages of the ratio mixed preparing of 100:10:7 in fixture, use alcohol washes with after liquid honing to 800#, dry up for subsequent use after acetone oil removing.Pull down fastening bolt 4, open high pressure kettle cover 25, packaged three-electrode system 11 is fastened on the bottom of condensation water tank 12, and around it, be coated with silica gel with anti-gas-leak.Three wires connecting three-electrode system 11 are penetrated in working electrode wire guide (26), Ag/AgCl contrast electrode wire guide (23), auxiliary electrode wire guide (24) in order to connecting external electrochemical workstation.Water is filled by condensation water tank 11.In autoclave body 7, pour the simulation medium solution of certain volume into, do not allow solution cover the bottom of condensation water tank 12, to maintain a top part corrosion environment.Cover high pressure kettle cover 25, tighten fastening bolt 4.Gas N is passed into from autoclave air intake opening 17
2deoxygenation more than 8 hours, then passes into experimental gas (as CO
2gas) reach the pressure of setting.Open the heating and thermal insulation system control switch of control box, in heating high-pressure still, solution is to setting experimental temperature and being incubated.Open circulating condensing Water in Water Tank switch pump, setting condensing temperature, makes cooling water circulation flow.After temperature and pressure reaches setting value, system can maintain this state, is connected by three electrode cables can realize electrochemical data and export, record, process and the function such as analysis with external telephoning telephony workstation.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. high temperature and high pressure environment next top corrosion electrochemical test system, is characterized in that: this device comprises high-temperature high-pressure reaction kettle, heating and thermal insulation system, circulating condensing Water tank refrigeration system, three-electrode system (11), working electrode signal transduction pathway, external control box, external air supply system and computing machine, wherein, high-temperature high-pressure reaction kettle comprises high pressure kettle cover (25), still handle (20), autoclave body (7), safety valve (16), pressure display instrument (15), pressure transducer, air intake opening (17) and gas outlet (5), heating and thermal insulation system comprises thermoelectricity on a rare occasion (8), thermopair two (10) and temperature sensor, circulating condensing Water tank refrigeration system comprises cooling water circulation water inlet (3), cooling water circulation water delivering orifice (18) and condensation water tank (12), three-electrode system (11) comprises Ag/AgCl contrast electrode (2), working electrode (1) and auxiliary electrode (19), external control box comprises temperature in the kettle control instrument (9) and pressure display instrument (15), and external air supply system (13) comprises gas cylinder, reduction valve, wireway and by-pass valve control (14), high pressure kettle cover (25) has bolt hole (21), autoclave body (7) is connected by fastening bolt (4) with high pressure kettle cover (25), and centre is lined with rubber seal (6) sealing, autoclave body (7) inner bottom part is equipped with thermoelectricity on a rare occasion (8) and thermopair two (10), autoclave body (7) internal upper part is equipped with condensation water tank (12), three-electrode system (11) is equipped with in condensation water tank (12) bottom, and pass through wire, by Ag/AgCl contrast electrode (2), working electrode (1) and auxiliary electrode (19) guide to condensation water tank (12) top, through Ag/AgCl contrast electrode wire guide (23), working electrode wire guide (26), auxiliary electrode wire guide (24) stretches out high pressure kettle cover (25), high pressure kettle cover (25) separately has cooling water circulation inlet opening (22) and cooling water circulation water outlet oral pore (27), Cooling Water circulation water inlet (3) and cooling water circulation water delivering orifice (18) stretch out, air intake opening (17) and gas outlet (5) of level are left in autoclave body (7) top, gas outlet (5) connection control valve, air intake opening (17) is connection safety valve (16), pressure display instrument (15) and by-pass valve control (14) successively.
2. high temperature and high pressure environment next top according to claim 1 corrosion electrochemical test system, is characterized in that: described temperature sensor, thermoelectricity on a rare occasion (8), thermopair two (10) are connected by wire with external control box.
3. high temperature and high pressure environment next top according to claim 1 corrosion electrochemical test system, it is characterized in that: the reduction valve of described external air supply system gas cylinder, to be threaded connection between wireway and the air intake opening (17) of autoclave, the experimental gas that external air supply system exports, by entering in high-temperature high-pressure reaction kettle by wireway after reduction valve pressure control, produces simulated experiment gas pressure intensity.
4. high temperature and high pressure environment next top according to claim 1 corrosion electrochemical test system, it is characterized in that: described Ag/AgCl contrast electrode (2), auxiliary electrode (19) and working electrode (1) are encapsulated in annular clip, and by smooth for packaged sample sand papering, make three electrodes be in same plane, be then connected with external electrochemical workstation by wire.
5. high temperature and high pressure environment next top according to claim 1 corrosion electrochemical test system, it is characterized in that: described three-electrode system (11) is connected with external electrochemical workstation by working electrode signal transduction pathway, carry out electro-chemical test, external electrochemical workstation is connected computing machine and is carried out data output, record and analyzing and processing.
6. high temperature and high pressure environment next top according to claim 1 corrosion electrochemical test system, it is characterized in that: the pressure of described autoclave body (7) inside by pressure transducer and pressure display instrument (15) display, and is regulated by by-pass valve control (14).
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Cited By (12)
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| CN105699286A (en) * | 2016-04-06 | 2016-06-22 | 北京科技大学 | Top corrosion testing device of wet gas loop |
| CN106706511A (en) * | 2017-02-16 | 2017-05-24 | 天津大学 | Electrochemical reaction still with openings in two sides and using 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 |
| CN108932986A (en) * | 2018-07-06 | 2018-12-04 | 中国核动力研究设计院 | A kind of high-temperature high-pressure reaction kettle and test method suitable for hot cell radiation environment |
| CN109541084A (en) * | 2018-11-28 | 2019-03-29 | 湖北航天化学技术研究所 | A kind of device of dynamic analysis detection gas-phase product |
| CN109682937A (en) * | 2019-03-04 | 2019-04-26 | 中国科学院地球化学研究所 | A kind of large cavity high temperature and pressure gas liquid two-phase flow experimental provision and experimental method |
| CN109994231A (en) * | 2019-04-28 | 2019-07-09 | 东华理工大学 | A kind of radiation corrosion test device and test method |
| CN110231364A (en) * | 2019-07-03 | 2019-09-13 | 中国特种设备检测研究院 | A kind of on-line checking dew point corrosion probe unit |
| CN110243755A (en) * | 2019-07-10 | 2019-09-17 | 北京科技大学 | It can be changed the top part corrosion test macro and test method of wind field regulation in autoclave |
| 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 |
| CN111678859A (en) * | 2020-07-08 | 2020-09-18 | 中国石油大学(华东) | Testing device for simulating local corrosion of top in wet gas conveying pipeline |
| CN111678860A (en) * | 2020-07-21 | 2020-09-18 | 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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Cited By (20)
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| CN105699286A (en) * | 2016-04-06 | 2016-06-22 | 北京科技大学 | Top corrosion testing device of wet gas loop |
| CN105699286B (en) * | 2016-04-06 | 2018-09-14 | 北京科技大学 | A kind of moisture loop top part corrosion test device |
| CN106706511A (en) * | 2017-02-16 | 2017-05-24 | 天津大学 | Electrochemical reaction still with openings in two sides and using method thereof |
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| 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 |
| CN108932986A (en) * | 2018-07-06 | 2018-12-04 | 中国核动力研究设计院 | A kind of high-temperature high-pressure reaction kettle and test method suitable for hot cell radiation environment |
| CN109541084A (en) * | 2018-11-28 | 2019-03-29 | 湖北航天化学技术研究所 | A kind of device of dynamic analysis detection gas-phase product |
| 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 |
| CN109682937A (en) * | 2019-03-04 | 2019-04-26 | 中国科学院地球化学研究所 | A kind of large cavity high temperature and pressure gas liquid two-phase flow experimental provision and experimental method |
| 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 |
| CN109994231A (en) * | 2019-04-28 | 2019-07-09 | 东华理工大学 | A kind of radiation corrosion test device and test method |
| CN110231364B (en) * | 2019-07-03 | 2024-05-03 | 中国特种设备检测研究院 | On-line detection dew point corrosion probe device |
| CN110231364A (en) * | 2019-07-03 | 2019-09-13 | 中国特种设备检测研究院 | A kind of on-line checking dew point corrosion probe unit |
| 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 |
| CN110243755A (en) * | 2019-07-10 | 2019-09-17 | 北京科技大学 | It can be changed the top part corrosion test macro and test method of 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 |
| CN111678859A (en) * | 2020-07-08 | 2020-09-18 | 中国石油大学(华东) | Testing device for simulating local 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 |
| CN111678860A (en) * | 2020-07-21 | 2020-09-18 | 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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