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CN102121896B - Experimental device for jet etching simulation and electrochemical test of high-temperature high-pressure loop - Google Patents

Experimental device for jet etching simulation and electrochemical test of high-temperature high-pressure loop Download PDF

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CN102121896B
CN102121896B CN201010620993.4A CN201010620993A CN102121896B CN 102121896 B CN102121896 B CN 102121896B CN 201010620993 A CN201010620993 A CN 201010620993A CN 102121896 B CN102121896 B CN 102121896B
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autoclave
temperature
loop
pressure
cooling system
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CN102121896A (en
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柳伟
俞曼丽
李新仲
常炜
郭宏
郑利军
路民旭
王春升
王建丰
樊学华
蔡峰
王振国
刘太元
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ANKE PIPING ENGINEERING SCIENCE AND TECHNOLOGY Co Ltd BEIJING
University of Science and Technology Beijing USTB
China National Offshore Oil Corp CNOOC
CNOOC Research Institute Co Ltd
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ANKE PIPING ENGINEERING SCIENCE AND TECHNOLOGY Co Ltd BEIJING
University of Science and Technology Beijing USTB
China National Offshore Oil Corp CNOOC
CNOOC Research Center
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Abstract

本发明涉及一种高温高压环路喷射腐蚀模拟及电化学测试实验装置，属于电化学领域。特别适用于模拟石油天然气等采集和输送管道中的弯头、三通等复杂部件所出现的冲刷腐蚀情况，以进行输送高温高压多相流体管道部件冲刷腐蚀的模拟实验，以及进行冲刷条件下的高温高压流体冲刷腐蚀的原位电化学信号测试。该装置由高压釜、加热保温系统、环路进水口、三电极体系、管道转接法兰、循环回路、高温高压液体流量计、控制阀门、排液口、旋涡泵、循环冷却系统、测温系统、管道连接法兰、环路出水口、喷头、试样夹具、控制箱、信号传导通路、外接电化学工作站及外接高压气瓶构成。该装置能够很好的模拟油气管线中流体介质的冲刷腐蚀情况，以及测试工作电极在高速喷射条件下的电化学信号，如极化曲线和交流阻抗等，对于进行高温高压流体冲刷腐蚀行为、规律以及机理的研究具有重要的意义。

Figure 201010620993

The invention relates to a high-temperature and high-pressure loop spray corrosion simulation and electrochemical test experimental device, which belongs to the field of electrochemistry. It is especially suitable for simulating the scouring and corrosion of complex parts such as elbows and tees in oil and gas collection and transportation pipelines, so as to carry out simulation experiments on scouring and corrosion of high-temperature and high-pressure multi-phase fluid pipeline components, and to carry out scouring conditions. In situ electrochemical signal test of high temperature and high pressure fluid erosion corrosion. The device consists of an autoclave, a heating and heat preservation system, a loop water inlet, a three-electrode system, a pipe adapter flange, a circulation loop, a high-temperature and high-pressure liquid flow meter, a control valve, a liquid discharge port, a vortex pump, a circulating cooling system, and a temperature measurement system. System, pipeline connection flange, loop water outlet, nozzle, sample fixture, control box, signal transmission path, external electrochemical workstation and external high-pressure gas cylinder. The device can well simulate the erosion and corrosion of fluid medium in oil and gas pipelines, and test the electrochemical signals of the working electrode under high-speed injection conditions, such as polarization curves and AC impedance. And the study of the mechanism is of great significance.

Figure 201010620993

Description

A kind of high-temperature high-pressure loop spray corrosion simulation and electro-chemical test experimental provision
Technical field
The invention belongs to electrochemical field, relate to the experimental provision of erosion corrosion behavior, rule and the mechanism research usefulness of a kind of high temperature pressure corrosion medium metal material under the high velocity jet working condition.Be applicable to the research of complex component erosion corrosion behaviors in the high temperature and high pressure flow body medium such as channel bend, threeway, be particularly useful for simulating the erosion corrosion situation that the complex component such as elbow in the collections such as petroleum gas and the conveyance conduit, threeway occur, carry the simulated experiment of High Temperature High Pressure heterogeneous fluid conduit component erosion corrosion, and the electrochemical in-situ signal testing that carries out the high-temperature, high pressure fluid erosion corrosion under the Scouring Condition.
Background technology
The high-temperature, high pressure fluid erosion corrosion is that a kind of galvanic corrosion and mechanical erosion interact and the material failure phenomenon that causes, and it is main that complex component such as the elbow of pipeline in oil and gas industry collection and the course of conveying, threeway lost efficacy mainly with the erosion corrosion of high-temperature, high pressure fluid.Containing CO 2In the oil gas transmission Deng sour gas, because the flow velocity of internal pipe pressure, temperature and medium is higher, easily form turbulent flow at complex component places such as elbow, threeways, produce very large shearing stress at inner-walls of duct and greatly accelerated the damage at pipe fitting position.Carrying out the High Temperature High Pressure erosion-corrosion experiment is the important means of corrosion stability, erosion behavior and the mechanism of material under the evaluation flow at high speed ambient condition.Therefore, the high-temperature, high pressure fluid erosion-corrosion experiment that can simulate under the physical condition and the device that carries out the electrochemical in-situ corrosion experiment must be arranged.But because under the injection conditions of High Temperature High Pressure and high-velocity fluid, bearing capacity requirement and the structures such as dynamic duty electrode and contrast electrode to pipe connecting part, volute pump, flowmeter and by-pass valve control have very high requirement, and are not easy to realize the measurement of electrochemical signals.Usually, in normal temperature and pressure conditions, carry out erosion-corrosion experiment, and carry out the electrochemical in-situ test experiments of normal temperature and pressure.Therefore, during erosion corrosion mechanism under the research trends condition, owing to the device that lacks High Temperature High Pressure erosion-corrosion experiment device and measure the high-temperature and high pressure electrochemistry signal affects further investigation to High Temperature High Pressure erosion corrosion behavior, rule and mechanism.
Summary of the invention
For the problems referred to above, the object of the present invention is to provide high-temperature, high pressure fluid erosion corrosion simulated experiment and electrochemical in-situ experimental apparatus for testing, carry high-temperature, high pressure fluid for the research conduit component and cause the corrosion resisting property of behavior, rule, mechanism and the evaluation material of erosion corrosion, cover simulation High Temperature High Pressure erosion-corrosion experiment and an electro-chemical test experimental provision is provided.This experimental provision can be simulated conduit component caused erosion corrosion phenomenon in carrying the high-temperature high-pressure medium flow liquid process easily.
A kind of high-temperature high-pressure loop spray corrosion simulation and electro-chemical test experimental provision is characterized in that: this device comprises autoclave 31, heat tracing system, loop water delivering orifice 5, three-electrode system, pipeline adapter flange 8, closed circuit 10, high-temperature high-pressure liquid flowmeter body 11, by-pass valve control, leakage fluid dram 14, volute pump 15, circulating cooling system 17, temp measuring system, pipeline coupling flange 20, loop water inlet 22, shower nozzle 25, specimen holder 33, control box, signal transduction pathway, external electrochemical workstation and external gas cylinder; Autoclave 31 is made of draft tube 1, autoclave loam cake 2, autoclave body 4, autoclave lower cover 6, viton seal ring 1, pressure transducer 26, tensimeter 27, safety valve 28 and gas outlet 30; The heat tracing system is made of autoclave heating and heat-insulating device 3 and closed circuit heating and heat-insulating device 46; Three-electrode system is made of auxiliary electrode 7, working electrode copper rod 9 and High Temperature High Pressure Ag/AgCl contrast electrode 21; By-pass valve control comprises flowmeter valve 12 and bypass valve 13; Circulating cooling system 17 is made of circulating cooling system water delivering orifice 16 and circulating cooling system water inlet 19; Temp measuring system is made of temperature sensor 29 in closed circuit temperature sensor 18 and the autoclave; Control box is made of temperature in the kettle control instrument, loop temperature control instrument, circulating cooling system gauge tap and volute pump gauge tap; Signal transduction pathway is made of the wire between electrochemical workstation and three electrodes; The wireway of external gas cylinder and the draft tube of autoclave 1 are threaded connection.Autoclave lower cover 6 is connected with autoclave body 4 by bolt, and utilizes viton seal ring one 23 sealings.The loop water inlet 22 of closed circuit 10 links to each other with autoclave lower cover 6 by welding, and lower end use pipeline coupling flange 20, makes things convenient for the dismounting of loop and autoclave.Circulating cooling system 17 inside pass into the recirculated cooling water (refrigerator circulation) of uniform temperature, eliminate the heat that the high temperature and high pressure flow body medium produces at shower nozzle 25 places, and keeping the stability of whole system temperature in conjunction with loop heat tracing system (other positions that do not comprise cooling system in Fig. 1 closed circuit 10) and autoclave heat tracing system 3, autoclave 31 and closed circuit 10 internal liquid temperature are measured by temperature sensor in the autoclave 29 and closed circuit temperature sensor 18 respectively.The water side of closed circuit 10 changes pipe diameter by pipeline adapter flange 8, is convenient to link to each other with autoclave 31, and loop water delivering orifice 5 is connected with autoclave lower cover 6 by the bite type web member, guarantees impermeability.Control box links to each other with autoclave 31, loop heat tracing system, circulating cooling system 17 and volute pump 15 by wire.Fluid media (medium) in the device circulates by volute pump 15, and utilizes flowmeter valve 12 and bypass valve 13 to regulate the flow velocity of shower nozzle 25 place's media, shows the flow at shower nozzle 25 places by high-temperature high-pressure liquid flowmeter body 11.The inner pressure of device passes through pressure transducer 23 and tensimeter 24 shows, when whole device pressure surpasses predetermined value, can regulate by gas outlet 30, in case overrate, safety valve 27 will be opened automatically, guarantee the security of whole system.Liquid in the whole device is by leakage fluid dram 14 emptyings.
Electrochemical testing device is by auxiliary electrode 7, working electrode copper rod 9, and High Temperature High Pressure Ag/AgCl contrast electrode 21, signal transduction pathway and external electrochemical workstation consist of.Auxiliary electrode 7 and High Temperature High Pressure Ag/AgCl contrast electrode 21 utilize with autoclave lower cover 6 and are threaded.The concrete structure of working electrode copper rod 9 as shown in Figure 2, the polytetrafluoro anchor clamps 33 that polytetrafluoro bolt 32 will stud with sample 24 are fixed on the jig pallet 34, and utilize polytetrafluoro O-ring seal 2 36 to seal, avoid internal work electrode copper rod 9 to contact with liquid medium, jig pallet 34 is fixed on the basetray 39 by tray supporter 38, tray supporter 38 utilizes with basetray 39 and is threaded, and utilize tray supporter 38 will be with cone polytetrafluoro sleeve 40 and copper rod 9 press seals, basetray 39 and autoclave lower cover 6 guarantee its concentricity by being weldingly connected.Sample 24 contacts with copper rod 9 by copper spring 35, guarantees that both contact well.Cylinder copper nut 37 is connected with copper rod 9, guarantee that copper rod bears higher pressure in the vertical direction, and cylinder copper nut 37 utilizes polytetrafluoro pad 2 45 to avoid contacting with jig pallet 34.Copper rod 9 utilizes band cone polytetrafluoro sleeve 40 and polytetrafluoro circular cone 41 to guarantee the sealing of autoclave lower cover 6.Polytetrafluoro circular cone 41 utilizes polytetrafluoro pad 1 and copper nut one 42 lockings, copper rod 9 utilizes copper nut 2 43 to link to each other with the working electrode end of electrochemical workstation, and auxiliary electrode 7 links to each other with the corresponding interface of electrochemical workstation respectively with High Temperature High Pressure Ag/AgCl contrast electrode 21.The autoclave volume is 8L, and whole device volume is 12L, and 180 ℃ of maximum operating temperatures, maximum working pressure (MWP) are 2MPa, and the maximum spout jet velocity is 40m/s.
The invention has the advantages that and to simulate the high-temperature, high pressure fluid erosion-corrosion experiment, and the electrochemical in-situ signal (linear polarization, polarization curve and electrochemical impedance etc.) of monitoring electrode in high-temperature, high pressure fluid injection situation, and erosion corrosion weightlessness and morphology observation sample can be provided, can be used for carrying out erosion corrosion behavior, rule and the research on mechanism of high temperature and high pressure flow body medium.
Description of drawings
Fig. 1 is structural representation of the present invention, wherein, and the 1-draft tube, 2-autoclave loam cake, 3-autoclave heating and heat-insulating device, 4-autoclave body, 5-loop water delivering orifice, 6-autoclave lower cover, 7-auxiliary electrode, 8-pipeline adapter flange, 9-working electrode copper rod, 10-closed circuit, 11-high-temperature high-pressure liquid flowmeter body, 12-flowmeter valve, 13-bypass valve, the 14-leakage fluid dram, 15-volute pump, 16-circulating cooling system water delivering orifice, the 17-circulating cooling system, 18-closed circuit temperature sensor, 19-circulating cooling system water inlet, 20-pipeline coupling flange, 21-High Temperature High Pressure Ag/AgCl contrast electrode, 22-loop water inlet, 23-viton seal ring, 24-sample, the 25-shower nozzle, the 26-pressure transducer, 27-tensimeter, 28-safety valve, temperature sensor in the 29-autoclave, the 30-gas outlet, 31-autoclave, 46-closed circuit heating and heat-insulating device;
Fig. 2 is the structural representation in A district among Fig. 1 of the present invention, wherein, and 32-polytetrafluoro bolt, the 33-specimen holder, 34-jig pallet, 35-copper spring, 36-viton seal ring two, 37-cylinder copper nut, 38-tray supporter, the 39-basetray, 40-band cone polytetrafluoro sleeve, 41-polytetrafluoro circular cone, 42-copper nut one, 43-copper nut two, 44-polytetrafluoro pad one, 45-polytetrafluoro pad two.
Embodiment
With reference to Fig. 1,2, this is high-temperature, high pressure fluid erosion corrosion simulated experiment and the electro-chemical test experimental provision that provides according to technique scheme.Opening high pressure still loam cake 2 is pulled down shower nozzle 25, the sample 24 of processing is fixed on the specimen holder 33, utilizes polytetrafluoro bolt 32 that specimen holder 33 is fixed on the jig pallet 34, sample 24 links to each other with copper rod 9 by copper spring 35, consist of the working electrode in the three-electrode system, mounting spray head 25.Pour the dielectric solution of certain volume in the autoclave 31 into, open simultaneously the leakage fluid dram 14 in the closed circuit 10, the gas emptying in will device, the liquid level of medium solution will be higher than the upper surface of sample 24, covers autoclave loam cake 2.Pass into gas N from autoclave air intake opening 1 2More than the deoxygenation 8h, after pass into the experimental gas of certain pressure (such as CO 2Gas) and be heated to design temperature.Open the gauge tap of the volute pump 15 in the control box, make volute pump 15 runnings carry out injection experiment, open simultaneously circulating cooling system 17, the heat tracing system of closed circuit 10, guarantee that whole device is in steady state (SS).Adjust flux meter valve 12 and bypass valve 13 change the flow that passes through high-temperature high-pressure liquid flowmeter body 11, thereby change the flow velocity of shower nozzle 25 place's fluids, reach the erosion corrosion simulated experiment effect of expection.Working electrode copper rod 9 utilizes copper nut 2 43 to link to each other with the working electrode end of electrochemical workstation, and auxiliary electrode 7 links to each other with the corresponding interface of electrochemical workstation respectively by signal transduction pathway with High Temperature High Pressure Ag/AgCl contrast electrode 21.The temperature of pressure, temperature and closed circuit 10 within control box shows autoclave 31.

Claims (2)

1.一种高温高压环路喷射腐蚀模拟及电化学测试实验装置，其特征在于：包括高压釜(31)、加热保温系统、环路出水口(5)、三电极体系、管道转接法兰(8)、循环回路(10)、高温高压液体流量计(11)、控制阀门、排液口(14)、旋涡泵(15)、循环冷却系统(17)、测温系统、管道连接法兰(20)、环路进水口(22)、喷头(25)、试样夹具(33)、控制箱、信号传导通路、外接电化学工作站及外接高压气瓶；1. A high-temperature and high-pressure loop spray corrosion simulation and electrochemical test experimental device, characterized in that it includes an autoclave (31), a heating and heat preservation system, a loop water outlet (5), a three-electrode system, and a pipeline adapter flange (8), circulating loop (10), high temperature and high pressure liquid flow meter (11), control valve, liquid outlet (14), vortex pump (15), circulating cooling system (17), temperature measuring system, pipe connection flange (20), loop water inlet (22), nozzle (25), sample fixture (33), control box, signal conduction path, external electrochemical workstation and external high-pressure gas cylinder; 高压釜(31)由进气管(1)、高压釜上盖(2)、高压釜体(4)、高压釜下盖(6)、氟橡胶密封圈一(23)、压力传感器(26)、压力表(27)、安全阀(28)及出气口(30)构成；加热保温系统由高压釜加热保温装置(3)和循环回路加热保温装置(46)构成；三电极体系由辅助电极(7)、工作电极铜棒(9)和高温高压Ag/AgCl参比电极(21)构成；控制阀门包括流量计阀门(12)和旁路阀门(13)；循环冷却系统(17)由循环冷却系统出水口(16)和循环冷却系统进水口(19)构成；测温系统由循环回路温度传感器(18)和高压釜内温度传感器(29)构成；控制箱由釜内温度控制仪表、环路温度控制仪表、循环冷却系统控制开关和旋涡泵控制开关构成；信号传导通路由电化学工作站与三电极之间的导线构成；The autoclave (31) consists of an air inlet pipe (1), an autoclave upper cover (2), an autoclave body (4), an autoclave lower cover (6), a fluororubber sealing ring one (23), a pressure sensor (26), A pressure gauge (27), a safety valve (28) and an air outlet (30); the heating and heat preservation system consists of an autoclave heating and heat preservation device (3) and a circulation loop heating and heat preservation device (46); the three-electrode system consists of an auxiliary electrode (7 ), a working electrode copper rod (9) and a high temperature and high pressure Ag/AgCl reference electrode (21); the control valve includes a flow meter valve (12) and a bypass valve (13); the circulating cooling system (17) consists of a circulating cooling system The water outlet (16) and the water inlet (19) of the circulating cooling system are composed; the temperature measurement system is composed of a circulating loop temperature sensor (18) and a temperature sensor (29) in the autoclave; the control box is composed of a temperature control instrument in the kettle, a loop temperature The control instrument, the control switch of the circulating cooling system and the control switch of the vortex pump are composed; the signal conduction path is composed of the wires between the electrochemical workstation and the three electrodes; 高压气瓶的导气管与高压釜的进气管(1)之间利用螺纹连接；控制箱通过导线与高压釜(31)、环路加热保温系统、循环冷却系统(17)以及旋涡泵(15)相连；环路出水口(5)和环路进水口(22)与高压釜下盖(6)分别通过焊接和螺栓卡套连接；循环回路(10)与高压釜(31)利用管道连接法兰(20)和管道转接法兰(8)连接；循环回路的出水端通过管道转接法兰(8)改变管路直径；循环回路(10)管道外壁装有循环冷却系统(17)和加热保温系统；循环冷却系统(17)与循环回路(10)之间利用螺栓连接；喷头(25)处的流速通过流量计阀门(12)和旁路阀门(13)调节；辅助电极(7)和高温高压Ag/AgCl参比电极(21)与高压釜下盖(6)为螺纹连接；试样(24)镶嵌在试样夹具(33)上，试样夹具(33)与夹具托盘(34)利用聚四氟螺栓(32)紧固，氟橡胶密封圈二(36)进行密封；试样(24)与铜棒(9)之间利用铜弹簧(35)相连，铜棒(9)通过圆柱状铜螺母(37)与夹具托盘(34)紧固，并与高压釜下盖(6)之间利用带锥聚四氟套筒(40)和聚四氟圆锥(41)进行密封，铜螺母一(42)和聚四氟垫片一(44)紧固；高压釜的压力传感器(26)测量釜内环境压力，精度为0.01MPa；高压釜内温度传感器(29)测量釜内溶液温度，循环回路温度传感器(18)测量环路溶液温度，精度为0.1℃。The gas guide pipe of the high-pressure gas cylinder and the inlet pipe (1) of the autoclave are connected by thread; the control box is connected with the autoclave (31), the loop heating and heat preservation system, the circulating cooling system (17) and the vortex pump (15) through the wire connected; the loop water outlet (5) and the loop water inlet (22) are connected to the autoclave lower cover (6) by welding and bolt ferrules respectively; the loop loop (10) and the autoclave (31) are connected to the flange by pipes (20) is connected with the pipeline adapter flange (8); the water outlet end of the circulation loop changes the pipeline diameter through the pipeline adapter flange (8); the circulation loop (10) pipeline outer wall is equipped with a circulating cooling system (17) and heating Insulation system; the circulating cooling system (17) and the circulating circuit (10) are connected by bolts; the flow rate at the nozzle (25) is regulated by the flow meter valve (12) and the bypass valve (13); the auxiliary electrode (7) and The high-temperature and high-pressure Ag/AgCl reference electrode (21) is threadedly connected to the lower cover (6) of the autoclave; the sample (24) is embedded in the sample holder (33), and the sample holder (33) and the holder tray (34) Utilize PTFE bolts (32) to fasten, fluorine rubber sealing ring two (36) to seal; Utilize copper spring (35) to connect between sample (24) and copper rod (9), copper rod (9) passes cylinder The copper nut (37) is fastened to the fixture tray (34), and is sealed with the lower lid of the autoclave (6) with a tapered PTFE sleeve (40) and a PTFE cone (41). The copper nut One (42) and polytetrafluoro gasket one (44) are fastened; the pressure sensor (26) of the autoclave measures the ambient pressure in the still, and the accuracy is 0.01MPa; the temperature sensor (29) in the autoclave measures the solution temperature in the still, The loop temperature sensor (18) measures the loop solution temperature with an accuracy of 0.1°C. 2.如权利要求1所述的一种高温高压环路喷射腐蚀模拟及电化学测试实验装置，其特征在于：循环冷却系统(17)利用制冷器消除喷头(25)处产生的热量，并结合循环回路(10)的加热保温系统和高压釜的加热保温系统(3)保证整个装置处于稳定状态；循环回路(10)通过管道连接法兰(20)和管道转接法兰(8)与高压釜(31)连接，方便拆卸；试样夹具(33)与夹具托盘(34)之间利用聚四氟螺栓(32)紧固，并使用氟橡胶密封圈二(36)进行密封，保证铜棒(9)不与溶液介质接触；铜棒(9)与试样(24)通过铜弹簧(35)相连，保证铜棒与试样两者接触良好；铜棒(9)利用圆柱铜螺母(37)、铜螺母一(42)、托盘立柱(38)、带锥聚四氟套筒(40)以及聚四氟锥(41)进行紧固密封；喷头(25)通过螺纹与管道连接。2. A kind of high temperature and high pressure loop injection corrosion simulation and electrochemical test experimental device as claimed in claim 1, is characterized in that: the circulation cooling system (17) utilizes refrigerator to eliminate the heat that spray nozzle (25) place produces, and combines The heating and heat preservation system (3) of the circulation circuit (10) and the autoclave ensure that the whole device is in a stable state; The kettle (31) is connected for easy disassembly; the sample fixture (33) and the fixture tray (34) are fastened with polytetrafluorobolts (32) and sealed with a fluororubber sealing ring (36) to ensure that the copper rod (9) not in contact with the solution medium; the copper rod (9) is connected to the sample (24) by a copper spring (35), ensuring good contact between the copper rod and the sample; the copper rod (9) utilizes a cylindrical copper nut (37 ), copper nut one (42), tray column (38), tapered polytetrafluoro sleeve (40) and polytetrafluoro cone (41) for fastening and sealing; the nozzle (25) is connected to the pipeline by threads.
CN201010620993.4A 2010-05-28 2010-12-23 Experimental device for jet etching simulation and electrochemical test of high-temperature high-pressure loop Active CN102121896B (en)

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CN201010194447A CN101865816A (en) 2010-05-28 2010-05-28 A high temperature and high pressure loop spray corrosion simulation and electrochemical test experimental device
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