CN204269527U - The buffering agent evaluation apparatus of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH - Google Patents

The buffering agent evaluation apparatus of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH Download PDF

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Publication number
CN204269527U
CN204269527U CN201420796506.3U CN201420796506U CN204269527U CN 204269527 U CN204269527 U CN 204269527U CN 201420796506 U CN201420796506 U CN 201420796506U CN 204269527 U CN204269527 U CN 204269527U
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China
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high pressure
dissolved oxygen
high temperature
electrode
hole
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Expired - Fee Related
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CN201420796506.3U
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Chinese (zh)
Inventor
许立宁
路民旭
王贝
范晓丽
李东阳
张玉楠
吝彭彭
朱诗俊
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ANKE PIPING ENGINEERING SCIENCE AND TECHNOLOGY Co Ltd BEIJING
University of Science and Technology Beijing USTB
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ANKE PIPING ENGINEERING SCIENCE AND TECHNOLOGY Co Ltd BEIJING
University of Science and Technology Beijing USTB
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Abstract

The utility model provides the buffering agent evaluation apparatus of a kind of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH, comprise high-temperature high-pressure reaction kettle, reactor heating and heat-insulating device, electrochemical test system, dissolved oxygen DO detection system, pH test macro, external air supply system and computing machine, wherein external air supply system comprises: gas cylinder, reduction valve, the first wireway and by-pass valve control.Advantage is dissolved oxygen content and pH value change when monitoring solution near body simulated solution electrochemical in-situ signal and continuous monitoring material surface after corrosion inhibiter filling, avoid the danger of the high temperature and high pressure kettle sample analysis be in operation, and the cross pollution to sample, this utility model has great importance on the research that corrosion inhibiter corrosion mitigating effect affects on the electrochemical behavior of corrosion inhibiter under researching high-temperature hyperbaric environment and dissolved oxygen content, pH value.

Description

The buffering agent evaluation apparatus of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH
Technical field
The utility model belongs to corrosion electrochemistry field, relates to the experimental provision of oxygen content affecting laws in the corrosion electrochemical action of metal material under a kind of high temperature pressure corrosion environment, solution, pH affecting laws and corrosion inhibiter evaluation.
Background technology
In recent years, along with oil-gas field development increases day by day, can the research of in-situ evaluation corrosion inhibiter also receive much concern under high-temperature and high-pressure conditions.In oil and gas industry exploitation and course of conveying, the corrosive medium related generally to is CO 2in sour gas and water, therefore to containing CO 2it is necessary for adding corrosion inhibiter in the conveyance conduit of gas.But, after adding corrosion inhibiter, the pH value of material surface and the influence research of electrochemical reaction are still lacked.Usually, carry out corrosion inhibiter evaluation experimental in high-temperature high-pressure reaction kettle after, then in static synthesis under normal pressure container, carry out the electro-chemical test of corrosion inhibiter, the electrochemical behavior in corrosion process under actual conditions can not be reflected.Therefore, owing to measuring the shortage of the technical equipment of high-temperature and high pressure electrochemistry signal and pH value etc., have impact on the further investigation to the behavior of High Temperature High Pressure Dynamic Corrosion and mechanism.Meanwhile, in actual applications, much operate, such as: annular injection nitrogen, down-hole re-injection CO 2, inject corrosion inhibiter, re-injection recovered water etc. all can bring O under oil well 2, thus make to there is certain O in the oil and gas environments of down-hole 2content, makes oil well pipe be in original CO in oil reservoir 2with O ground entering into down-hole 2under coexisted environment.Meanwhile, data shows, O 2the impact of concentration on corrosion rate and corrosion inhibiter inhibition efficiency be can not ignore, O 2and CO 2the corrosion rate caused that coexists increase also more than simple overlaying relation want serious many.But, in the world to O 2research for the impact of corrosion inhibiter inhibition efficiency is not deep enough yet, does not often consider the introducing of oxygen when evaluating corrosion inhibiter yet, and this is abnormally dangerous and inappropriate.
Utility model content
The purpose of this utility model is the buffering agent evaluation apparatus of a kind of High Temperature High Pressure Real-Time Monitoring dissolved oxygen in order to solve the problems of the technologies described above, pH, detect after being applicable to corrosion inhibiter filling and adjust the dissolved oxygen content of solution near body simulated solution and material surface at any time, solving under high temperature and high pressure environment dissolved oxygen DO and pH value to the problem of corrosion inhibiter in-situ evaluation under the impact of corrosion inhibiter corrosion mitigating effect and high temperature and high pressure environment.
In order to achieve the above object, the technical scheme that provides of the utility model is as follows:
The buffering agent evaluation apparatus of a kind of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH, comprise: high-temperature high-pressure reaction kettle, reactor heating and heat-insulating device, electrochemical test system, external air supply system and computing machine, external air supply system comprises: gas cylinder, reduction valve, the first wireway and by-pass valve control, described buffering agent evaluation apparatus also comprises dissolved oxygen DO detection system and pH test macro, described dissolved oxygen DO detection system comprises High Temperature High Pressure dissolved oxygen meter probe and external dissolved oxygen meter, and described pH test macro comprises pH combination electrode system and external pH instrument.
Further, described high-temperature high-pressure reaction kettle comprises: autoclave body, safety valve, tensimeter, pressure transducer, high pressure kettle cover and fastening bolt, described high pressure kettle cover is placed in autoclave body upper end and is connected by fastening bolt, by rubber seal rings for seal, the high pressure kettle cover center of circle is provided with the second High Temperature High Pressure Ag/AgCl contrast electrode hole, and centered by the center of circle, be disposed with working electrode hole counterclockwise, pH electrode hole, first High Temperature High Pressure Ag/AgCl contrast electrode hole, auxiliary electrode hole, dissolved oxygen probe hole, above-mentioned 5 holes with distance of center circle from equal, wherein working electrode hole, pH electrode hole, auxiliary electrode hole, equiangularly arranged between dissolved oxygen probe hole, first High Temperature High Pressure Ag/AgCl contrast electrode hole is arranged in the middle of pH electrode hole and auxiliary electrode hole, high pressure kettle cover is also provided with thermocouple jack, high pressure kettle cover outer rim is equidistant to be provided with some bolts hole and to coordinate with fastening bolt.
Further, the High Temperature High Pressure dissolved oxygen meter of described dissolved oxygen DO detection system is popped one's head in the dissolved oxygen probe hole covered through autoclave, and is connected with external dissolved oxygen meter by wire.
Further, the pH combination electrode system of described pH test macro comprises: High Temperature High Pressure pH electrode and the first High Temperature High Pressure Ag/AgCl contrast electrode, High Temperature High Pressure pH electrode and the first High Temperature High Pressure Ag/AgCl contrast electrode are each passed through in high pressure kettle cover pH electrode hole and the first High Temperature High Pressure Ag/AgCl contrast electrode hole, and are connected with external pH instrument by wire.
Further, described autoclave is covered with air admission hole, venthole and pressure detection mouth, be threaded connection between the reduction valve of air admission hole and external air supply system, the first wireway, first wireway enters in autoclave body, first wireway end is placed in autoclave body lower end, venthole is connected with by-pass valve control, and pressure detection mouth is connected with the safety valve outside autoclave body, tensimeter, pressure transducer by the second wireway.
Further, described reactor heating and heat-insulating device comprises: heating tape, thermopair and external control box, wherein external control box comprises: temperature in the kettle control instrument and pressure display instrument, heating tape is arranged in autoclave body sidewall, thermopair is through the thermocouple jack of high pressure kettle cover, its one end is placed in outside autoclave body, and the other end is placed in autoclave body, and heating tape, thermopair are connected by wire with external control box.
Further, described electrochemical test system comprises: working electrode, the second High Temperature High Pressure Ag/AgCl contrast electrode, auxiliary electrode and external electrochemical workstation, working electrode, the second High Temperature High Pressure Ag/AgCl contrast electrode and auxiliary electrode are each passed through the working electrode hole of high pressure kettle cover, the second High Temperature High Pressure Ag/AgCl contrast electrode hole, auxiliary electrode hole, and be connected with external electrochemical workstation by wire, the electrode probe end of working electrode, the second High Temperature High Pressure Ag/AgCl contrast electrode and auxiliary electrode is in same level.
The utility model has the advantage of: after adding corrosion inhibiter, the electrochemical in-situ signal under High Temperature High Pressure aerobic or oxygen-free environment can be measured, carry out the electro-chemical test of corrosion inhibiter without the need to off-line.In addition, adopt High Temperature High Pressure dissolved oxygen meter to realize Real-Time Monitoring and dissolved oxygen content change in recording solution, quantitative test dissolved oxygen content on the impact of corrosion inhibiter corrosion mitigating effect, and can regulate dissolved oxygen content accordingly at any time.Simultaneously can the change of Real-Time Monitoring pH value of solution, avoid in experimentation, the pollution that sample analysis dissolved oxygen content and pH value cause experimental solutions from solution and High Temperature High Pressure sample the danger brought.
Accompanying drawing explanation
Fig. 1 is high temperature and high pressure kettle upper cover schematic diagram of the present utility model;
Fig. 2 is the whole still structural representation of the utility model A-A section;
Fig. 3 is the whole still structural representation of the utility model B-B section;
Fig. 4 is the whole still structural representation of the utility model C-C section.
Each element sequence number in figure: bolt hole 1, working electrode hole 2, pH electrode hole 3, first High Temperature High Pressure Ag/AgCl contrast electrode hole 4, dissolved oxygen probe hole 5, second High Temperature High Pressure Ag/AgCl contrast electrode hole 6, auxiliary electrode hole 7, thermocouple jack 8, second High Temperature High Pressure Ag/AgCl contrast electrode 9, auxiliary electrode 10, thermopair 11, fastening bolt 12, venthole 13, heating tape 14, working electrode 15, air admission hole 16, High Temperature High Pressure pH electrode 17, safety valve 18, tensimeter 19, pressure unit 20, pressure detection mouth 21, High Temperature High Pressure dissolved oxygen meter probe 22, first High Temperature High Pressure Ag/AgCl contrast electrode 23.
Embodiment
In order to make the purpose of this utility model, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the utility model is explained in further detail.Should be appreciated that specific embodiment described herein only for explaining the utility model, and be not used in restriction the utility model.
On the contrary, the utility model is contained any by the substituting of making on marrow of the present utility model and scope of defining of claim, amendment, equivalent method and scheme.Further, in order to make the public have a better understanding to the utility model, in hereafter details of the present utility model being described, detailedly describe some specific detail sections.Do not have the description of these detail sections can understand the utility model completely for a person skilled in the art yet.Below in conjunction with accompanying drawing and embodiment, the utility model is further illustrated.
The buffering agent evaluation apparatus of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH, comprise: high-temperature high-pressure reaction kettle, reactor heating and heat-insulating device, electrochemical test system, dissolved oxygen DO detection system, pH test macro, external air supply system and computing machine, wherein external air supply system comprises: gas cylinder, reduction valve, the first wireway and by-pass valve control.
As Fig. 1, 2, 3, described high-temperature high-pressure reaction kettle comprises: autoclave body, safety valve 18, tensimeter 19, pressure transducer 20, high pressure kettle cover and fastening bolt 12, described high pressure kettle cover is placed in autoclave body upper end and is connected by fastening bolt 12, by rubber seal rings for seal, the high pressure kettle cover center of circle is provided with the second High Temperature High Pressure Ag/AgCl contrast electrode hole 6, and centered by the center of circle, be disposed with working electrode hole 2 counterclockwise, pH electrode hole 3, first High Temperature High Pressure Ag/AgCl contrast electrode hole 4, auxiliary electrode hole 7, dissolved oxygen probe hole 5, above-mentioned 5 holes with distance of center circle from equal, wherein working electrode hole 2, pH electrode hole 3, auxiliary electrode hole 7, equiangularly arranged between dissolved oxygen probe hole 5, first High Temperature High Pressure Ag/AgCl contrast electrode hole 4 is arranged in the middle of pH electrode hole 3 and auxiliary electrode hole 7, high pressure kettle cover is also provided with thermocouple jack 8, high pressure kettle cover outer rim is equidistant to be provided with some bolts hole 1 and to fix high pressure kettle cover for fastening bolt 12.
Autoclave is covered with air admission hole 16, venthole 13 and pressure detection mouth 21, the reduction valve of air admission hole 16 and external air supply system, be threaded connection between wireway, the experimental gas that gas cylinder exports is by entering in autoclave body by the first wireway after reduction valve pressure control, wireway end is placed in autoclave body lower end, produce simulated experiment gas pressure intensity, venthole 13 is connected with by-pass valve control, pressure detection mouth 21 is by the safety valve 18 outside the second wireway and autoclave body, tensimeter 19, pressure transducer 20 is connected, the pressure of autoclave body inside is shown by pressure transducer 20 and tensimeter 19, when in autoclave body, pressure exceedes predetermined value, regulate by the reduction valve of air admission hole 16 and venthole 13 by-pass valve control, once exceed the ratings of autoclave body pressure-bearing, safety valve 18 will be opened automatically, the security of protection whole system.
As shown in Figure 2, reactor heating and heat-insulating device comprises: heating tape 14, thermopair 11 and external control box, heating tape 14 is arranged in autoclave body sidewall, thermopair 11 is placed in autoclave body through thermocouple jack 8, heating tape 14, thermopair 11 are connected by wire with external control box, make solution in autoclave body reach setting high temperature by heating tape 14 and thermopair 11.
Described electrochemical test system comprises: working electrode 15, second High Temperature High Pressure Ag/AgCl contrast electrode 9, auxiliary electrode 10 and external electrochemical workstation, wherein working electrode 15, second High Temperature High Pressure Ag/AgCl contrast electrode 9 is each passed through working electrode hole 2 with auxiliary electrode 10, second High Temperature High Pressure Ag/AgCl contrast electrode hole 6 and auxiliary electrode hole 7, be threaded with using between high pressure kettle cover, and be connected with external electrochemical workstation by wire, working electrode 15 is squares material being cut into 10mm × 10mm, one side is burn-on wire wherein, ensure its circuit turn-on, by epoxy resin, dibutyl phthalate second two fat, ethylenediamine mixes according to the ratio of 100:10:7, a workplace is exposed in guarantee, be made into working electrode 15, working electrode 15 is connected with external electrochemical workstation by signal transduction pathway, described working electrode 15, the electrode probe end of the second High Temperature High Pressure Ag/AgCl contrast electrode 9 and auxiliary electrode 10 is in same level, form a galvanochemistry three-electrode system.
As shown in Figure 3, described dissolved oxygen DO monitoring system comprises: High Temperature High Pressure dissolved oxygen meter probe 22 and external dissolved oxygen meter, High Temperature High Pressure dissolved oxygen meter probe 22 can dissolved oxygen content near test probe in solution, external dissolved oxygen meter can realize the time dependent continuous record of dissolved oxygen content, and according to record result, the dissolved oxygen content in solution can be changed by adjusting air inflow quantity size at any time.
Described pH test macro comprises: pH combination electrode system and external pH instrument, wherein pH combination electrode system comprises: High Temperature High Pressure pH electrode 17 and the first High Temperature High Pressure Ag/AgCl contrast electrode 23, High Temperature High Pressure pH electrode 17 and the first High Temperature High Pressure Ag/AgCl contrast electrode 23 are each passed through pH electrode hole 3 and the first High Temperature High Pressure Ag/AgCl contrast electrode hole 4, described first High Temperature High Pressure Ag/AgCl contrast electrode 23 is obliquely installed, its electrode probe is close to the second High Temperature High Pressure Ag/AgCl contrast electrode 9 electrode probe, pH combination electrode system is connected by T-shaped adapter with external pH instrument, the pH value of solution near High Temperature High Pressure pH electrode 17 probe end can be monitored, external pH instrument can be connected computing machine and realize the time dependent continuous record of pH.
The use maximum temperature of the utility model first warm high pressure Ag/AgCl contrast electrode 23 and the second High Temperature High Pressure Ag/AgCl contrast electrode 9 is 150 C, top pressure is 5Mpa, auxiliary electrode 10 is Pt metal, High Temperature High Pressure dissolved oxygen meter 22 serviceability temperatures of popping one's head in are 1-130 C, top pressure is 0.6Mpa, the square electric chemistry sample that working electrode 15 uses epoxy resin to seal.
The utility model has the advantage of: after adding corrosion inhibiter, the electrochemical in-situ signal under High Temperature High Pressure aerobic or oxygen-free environment can be measured, carry out the electro-chemical test of corrosion inhibiter without the need to off-line.In addition, adopt High Temperature High Pressure dissolved oxygen meter to realize Real-Time Monitoring and dissolved oxygen content change in recording solution, quantitative test dissolved oxygen content on the impact of corrosion inhibiter corrosion mitigating effect, and can regulate dissolved oxygen content accordingly at any time.Simultaneously can the change of Real-Time Monitoring pH value of solution, avoid in experimentation, the pollution that sample analysis dissolved oxygen content and pH value cause experimental solutions from solution and High Temperature High Pressure sample the danger brought.

Claims (7)

1. a High Temperature High Pressure Real-Time Monitoring dissolved oxygen, the buffering agent evaluation apparatus of pH, comprise: high-temperature high-pressure reaction kettle, reactor heating and heat-insulating device, electrochemical test system, external air supply system and computing machine, external air supply system comprises: gas cylinder, reduction valve, first wireway and by-pass valve control, it is characterized in that, described buffering agent evaluation apparatus also comprises dissolved oxygen DO detection system and pH test macro, described dissolved oxygen DO detection system comprises High Temperature High Pressure dissolved oxygen meter probe (22) and external dissolved oxygen meter, described pH test macro comprises pH combination electrode system and external pH instrument.
2. buffering agent evaluation apparatus according to claim 1, it is characterized in that, described high-temperature high-pressure reaction kettle comprises: autoclave body, safety valve (18), tensimeter (19), pressure transducer (20), high pressure kettle cover and fastening bolt (12), described high pressure kettle cover is placed in autoclave body upper end and is connected by fastening bolt (12), by rubber seal rings for seal, the high pressure kettle cover center of circle is provided with the second High Temperature High Pressure Ag/AgCl contrast electrode hole (6), and centered by the center of circle, be disposed with working electrode hole (2) counterclockwise, pH electrode hole (3), first High Temperature High Pressure Ag/AgCl contrast electrode hole (4), auxiliary electrode hole (7), dissolved oxygen probe hole (5), above-mentioned 5 holes with distance of center circle from equal, wherein working electrode hole (2), pH electrode hole (3), auxiliary electrode hole (7), equiangularly arranged between dissolved oxygen probe hole (5), first High Temperature High Pressure Ag/AgCl contrast electrode hole (4) is arranged in the middle of pH electrode hole (3) and auxiliary electrode hole (7), high pressure kettle cover is also provided with thermocouple jack (8), the equidistant some bolts hole (1) that are provided with of high pressure kettle cover outer rim coordinate with fastening bolt (12).
3. buffering agent evaluation apparatus according to claim 2, is characterized in that, the dissolved oxygen probe hole (5) that the High Temperature High Pressure dissolved oxygen meter of described dissolved oxygen DO detection system probe (22) covers through autoclave, and is connected with external dissolved oxygen meter by wire.
4. buffering agent evaluation apparatus according to claim 2, it is characterized in that, the pH combination electrode system of described pH test macro comprises: High Temperature High Pressure pH electrode (17) and the first High Temperature High Pressure Ag/AgCl contrast electrode (23), High Temperature High Pressure pH electrode (17) and the first High Temperature High Pressure Ag/AgCl contrast electrode (23) are each passed through in high pressure kettle cover pH electrode hole (3) with the first High Temperature High Pressure Ag/AgCl contrast electrode hole (4), and are connected with external pH instrument by wire.
5. buffering agent evaluation apparatus according to claim 2, it is characterized in that, described autoclave is covered with air admission hole (16), venthole (13) and pressure detection mouth (21), the reduction valve of air admission hole (16) and external air supply system, be threaded connection between first wireway, first wireway enters in autoclave body, first wireway end is placed in autoclave body lower end, venthole (13) is connected with by-pass valve control, pressure detection mouth (21) is by the safety valve (18) outside the second wireway and autoclave body, tensimeter (19), pressure transducer (20) is connected.
6. buffering agent evaluation apparatus according to claim 2, it is characterized in that, described reactor heating and heat-insulating device comprises: heating tape (14), thermopair (11) and external control box, wherein external control box comprises: temperature in the kettle control instrument and pressure display instrument, heating tape (14) is arranged in autoclave body sidewall, thermopair (11) is through the thermocouple jack (8) of high pressure kettle cover, its one end is placed in outside autoclave body, the other end is placed in autoclave body, and heating tape (14), thermopair (11) are connected by wire with external control box.
7. buffering agent evaluation apparatus according to claim 2, it is characterized in that, described electrochemical test system comprises: working electrode (15), second High Temperature High Pressure Ag/AgCl contrast electrode (9), auxiliary electrode (10) and external electrochemical workstation, working electrode (15), second High Temperature High Pressure Ag/AgCl contrast electrode (9) and auxiliary electrode (10) are each passed through the working electrode hole (2) of high pressure kettle cover, second High Temperature High Pressure Ag/AgCl contrast electrode hole (6), auxiliary electrode hole (7), and be connected with external electrochemical workstation by wire, working electrode (15), the electrode probe end of the second High Temperature High Pressure Ag/AgCl contrast electrode (9) and auxiliary electrode (10) is in same level.
CN201420796506.3U 2014-12-16 2014-12-16 The buffering agent evaluation apparatus of High Temperature High Pressure Real-Time Monitoring dissolved oxygen, pH Expired - Fee Related CN204269527U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104515730A (en) * 2014-12-16 2015-04-15 北京科技大学 Evaluation device and detection method for high temperature and high pressure real-time monitoring of dissolved oxygen and pH value of corrosion inhibitor
CN109187700A (en) * 2018-09-12 2019-01-11 中石化(洛阳)科技有限公司 The evaluating apparatus and method of corrosion inhibiter filming performance

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104515730A (en) * 2014-12-16 2015-04-15 北京科技大学 Evaluation device and detection method for high temperature and high pressure real-time monitoring of dissolved oxygen and pH value of corrosion inhibitor
CN109187700A (en) * 2018-09-12 2019-01-11 中石化(洛阳)科技有限公司 The evaluating apparatus and method of corrosion inhibiter filming performance

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20150415

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