CN104614310A - High temperature and high pressure corrosion electrochemical measuring device and measuring method - Google Patents
High temperature and high pressure corrosion electrochemical measuring device and measuring method Download PDFInfo
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- CN104614310A CN104614310A CN201510044673.1A CN201510044673A CN104614310A CN 104614310 A CN104614310 A CN 104614310A CN 201510044673 A CN201510044673 A CN 201510044673A CN 104614310 A CN104614310 A CN 104614310A
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Abstract
The invention discloses a high temperature and high pressure corrosion electrochemical measuring device and a measuring method. The measuring device comprises a high pressure kettle heating jacket, a high pressure kettle body sleeved by the high pressure kettle heating jacket, and a high pressure kettle end cover fixed on the high pressure kettle body through a high pressure kettle fastening bolt, wherein a gas inlet, an exhaust port, a pressure gauge socket and a temperature measuring blind pipe socket are formed on the high pressure kettle end cover, and screw holes into which a reference electrode, a working electrode and an auxiliary electrode can be inserted are further formed on the high pressure kettle end cover; a gas inlet pipe at the gas inlet is provided with a gas inlet stop valve for opening/closing gas inletting; an exhaust pipe at the exhaust port is provided with a gas outlet stop valve for opening/closing the gassing; the invention further discloses the measuring method of the device; the measuring device is reliable and easy to realize, the problems that the high temperature and high pressure corrosion electrochemical measuring electrode is expensive in price, difficult in manufacturing and difficult in high temperature sealing are solved; the device disclosed by the invention is simple in manufacturing, good in sealing, and capable of meeting the corrosion electrochemical measurement in high temperature and high pressure environment.
Description
Technical field
The invention belongs to high temperature pressure corrosion electrochemical measuring technology field, be specifically related to a kind of high temperature pressure corrosion electro-chemical measuring apparatus and measuring method.
Background technology
In the high-temperature high pressure water media environment of station boiler and nuclear steam generator, concentrated due to corrosive impurity, the corrosion of heat exchange pipeline is commonplace.The important means of electrochemical measuring technology evaluating material corrosion stability, corrosion behavior and mechanism.But relative to normal temperature and pressure system, under high-temperature and high-pressure conditions there is larger difficulty in electrochemical measurement, mainly owing to being not easy the sealing realizing measuring-signal transfer wire and high temperature high pressure device simultaneously.At present, domestic related research institutes, the potential electrode generally adopting CORTEST company of the U.S. or Japanese Dong Shen company to provide carries out high temperature pressure corrosion electrochemical research, and the price of electrode also costly.Metal Inst., Chinese Academy of Sciences has obtained the patent of high-temperature and high pressure electrochemistry electrode fabrication correlation technique, but manufacture craft relative complex, market has no relevant commercially produced product.Because the acquisition of high temperature pressure corrosion electrochemical measuring electrode exists difficulty, affect the corrosion behavior of material in High Temperature High Pressure water environment, study mechanism to a certain extent.
Summary of the invention
In order to solve above-mentioned prior art Problems existing, the object of the present invention is to provide a kind of high temperature pressure corrosion electro-chemical measuring apparatus and measuring method, this measurement mechanism is reliable and be easy to realize, solve high temperature pressure corrosion electrochemical measuring electrode expensive, make difficulty and the problem of elevated-temperature seal difficulty; Apparatus of the present invention make simple, good airproof performance, can meet the measurement of corrosion electrochemistry in high temperature, hyperbaric environment.
For achieving the above object, the present invention adopts following technical scheme:
A kind of high temperature pressure corrosion electro-chemical measuring apparatus, is comprised autoclave heating jacket 1, is inserted in the autoclave body 2 in autoclave heating jacket 1, be fixed on the autoclave end cap 4 on autoclave body 2 by autoclave fastening bolt 3; Described autoclave end cap 4 has air intake opening 5, exhausr port 10, tensimeter 6 socket and thermometric blind pipe 11 socket, also has the screw that contrast electrode 7, working electrode 8 and auxiliary electrode 9 insert; The draft tube of described air intake opening 5 is provided with the air intake opening stop valve K1 opening and closing air inlet, the gas outlet of exhausr port 10 is provided with the gas outlet stop valve K2 opening and closing and give vent to anger; Described contrast electrode 7 is identical with the structure of auxiliary electrode 9, comprise wire column 15, be socketed in the glass tube 13 of outside, wire column 15 upper end, be welded on wire column 15 outside and be welded on the electrode low head 14 of glass tube 13 lower end, be welded on the electrode external thread sleeve 12 of outside, glass tube 13 upper end, wire column 15 bottom is welded with platinized platinum 16 by wire 18, the material of wire 18 is identical with the material of platinized platinum 16, and contrast electrode 7 is connected with the screw on autoclave end cap 4 by electrode external thread sleeve 12 with auxiliary electrode 9; The structure of described working electrode 8 is welded with test electrode sheet 17 by wire 18 except wire column 15 bottom, and the material of wire 18 identical with the material of test electrode sheet 17 outside, other structure is with contrast electrode 7 and auxiliary electrode 9, and working electrode 8 also electrode external thread sleeve 12 is connected with the screw on autoclave end cap 4.
The material of described electrode external thread sleeve 12, electrode low head 14 and wire column 15 is the kovar alloy close with glass tube thermal expansivity, ensure that and can carry out soldering between glass tube 13 and electrode external thread sleeve 12, electrode low head 14, achieve sealing, meet high temperature and high pressure environment request for utilization.
The measuring method of high temperature pressure corrosion electro-chemical measuring apparatus described above, first, is processed into test electrode sheet 17 by test material, be connected by the wire column 15 of wire 18 with working electrode 8 lower end; Then the electrode external thread sleeve 12 of contrast electrode 7, working electrode 8, auxiliary electrode 9 is connected with the screw be reserved on autoclave end cap 4; Poured into by test solution subsequently in autoclave body 2, the liquid level of test solution will control, under wire column 15 with the tie point of wire electrode 18, to avoid wire column 15 or wire column 15 to contact with test fluid with the tie point of wire electrode 18; Autoclave fastening bolt (3) is adopted autoclave end cap 4 and autoclave body 2 to be sealed subsequently; As needs deoxygenation, close air intake opening valve K1 and gas outlet valve K2, carry out deoxygenation operation by air intake opening 5, exhausr port 10 pairs of systems; Subsequently autoclave body 2 is heated, after medium temperature reaches setting value in autoclave body 2, the wire column 15 of contrast electrode 7, working electrode 8, auxiliary electrode 9 is connected with electrochemical workstation, carries out electro-chemical test.
Compared to the prior art comparatively, tool has the following advantages in the present invention:
1) manufacture craft of electrode is simple, and high pressure etching apparatus is installed, it is simple to make.
2) reliability of glass tube and kovar alloy is high, test macro good seal performance, most high-temperature resistant 400 DEG C, the highest withstand voltage 20MPa.
3) electrode adopts sleeve type structure, and the use of glass tube achieves the insulation of wire column and kettle.
Accompanying drawing explanation
Fig. 1 is measurement mechanism structural representation of the present invention.
Fig. 2 is the structural representation of contrast electrode, working electrode and auxiliary electrode.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
As shown in Figure 1, a kind of high temperature pressure corrosion electro-chemical measuring apparatus of the present invention, is comprised autoclave heating jacket 1, is inserted in the autoclave body 2 in autoclave heating jacket 1, be fixed on the autoclave end cap 4 on autoclave body 2 by autoclave fastening bolt 3; Described autoclave end cap 4 has air intake opening 5, exhausr port 10, tensimeter 6 socket and thermometric blind pipe 11 socket, also has the screw that contrast electrode 7, working electrode 8 and auxiliary electrode 9 insert; The draft tube of described air intake opening 5 is provided with the air intake opening stop valve K1 opening and closing air inlet, the gas outlet of exhausr port 10 is provided with the gas outlet stop valve K2 opening and closing and give vent to anger.
As shown in Figure 2, described contrast electrode 7 is identical with the structure of auxiliary electrode 9, comprise wire column 15, be socketed in the glass tube 13 of outside, wire column 15 upper end, be welded on wire column 15 outside and be welded on the electrode low head 14 of glass tube 13 lower end, be welded on the electrode external thread sleeve 12 of outside, glass tube 13 upper end, wire column 15 bottom is welded with platinized platinum 16 by wire 18, the material of wire 18 is identical with the material of platinized platinum 16, and contrast electrode 7 is connected with the screw on autoclave end cap 4 by electrode external thread sleeve 12 with auxiliary electrode 9; The structure of described working electrode 8 is welded with test electrode sheet 17 by wire 18 except wire column 15 bottom, and the material of wire 18 identical with the material of test electrode sheet 17 outside, other structure is with contrast electrode 7 and auxiliary electrode 9, and working electrode 8 also electrode external thread sleeve 12 is connected with the screw on autoclave end cap 4.
As the preferred embodiment of the present invention, the material of described electrode external thread sleeve 12, electrode low head 14 and wire column 15 is the kovar alloy close with glass tube thermal expansivity, ensure that and can carry out soldering between glass tube 13 and electrode external thread sleeve 12, electrode low head 14, achieve sealing, meet high temperature and high pressure environment request for utilization.
As shown in Figure 1, the measuring method of high temperature pressure corrosion electro-chemical measuring apparatus of the present invention, first, is processed into test electrode sheet 17 by test material, is connected by the wire column 15 of wire 18 with working electrode 8 lower end; Then the electrode external thread sleeve 12 of contrast electrode 7, working electrode 8, auxiliary electrode 9 is connected with the screw be reserved on autoclave end cap 4; Poured into by test solution subsequently in autoclave body 2, the liquid level of test solution will control, under wire column 15 with the tie point of wire electrode 18, to avoid wire column 15 or wire column 15 to contact with test fluid with the tie point of wire electrode 18; Autoclave fastening bolt (3) is adopted autoclave end cap 4 and autoclave body 2 to be sealed subsequently; As needs deoxygenation, close air intake opening valve K1 and gas outlet valve K2, carry out deoxygenation operation by air intake opening 5, exhausr port 10 pairs of systems; Subsequently autoclave body 2 is heated, after in autoclave body 2, medium temperature reaches setting value, the wire column 15 of contrast electrode 7, working electrode 8, auxiliary electrode 9 is connected with electrochemical workstation, carry out electro-chemical test, method of testing is: polarization curve test conventional during corrosion electrochemistry can be adopted to study and electrochemical impedance test, studies the corrosion characteristics of working electrode 8 in high-temperature high-pressure medium.
Claims (3)
1. a high temperature pressure corrosion electro-chemical measuring apparatus, it is characterized in that: comprise autoclave heating jacket (1), be inserted in the autoclave body (2) in autoclave heating jacket (1), be fixed on the autoclave end cap (4) on autoclave body (2) by autoclave fastening bolt (3), described autoclave end cap (4) has air intake opening (5), exhausr port (10), tensimeter (6) socket and thermometric blind pipe (11) socket, also has the screw that contrast electrode (7), working electrode (8) and auxiliary electrode (9) insert, the draft tube of described air intake opening (5) is provided with the air intake opening stop valve (K1) opening and closing air inlet, the gas outlet of exhausr port (10) is provided with the gas outlet stop valve (K2) opening and closing and give vent to anger, described contrast electrode (7) is identical with the structure of auxiliary electrode (9), comprise wire column (15), be socketed in the glass tube (13) of wire column (15) outside, upper end, be welded on wire column (15) outside and be welded on the electrode low head (14) of glass tube (13) lower end, be welded on the electrode external thread sleeve (12) of glass tube (13) outside, upper end, wire column (15) bottom is welded with platinized platinum (16) by wire (18), the material of wire (18) is identical with the material of platinized platinum (16), contrast electrode (7) is connected with the screw on autoclave end cap (4) by electrode external thread sleeve (12) with auxiliary electrode (9), the structure of described working electrode (8) is passed through wire (18) except wire column (15) bottom and is welded with test electrode sheet (17), and the material of wire (18) identical with the material of test electrode sheet (17) outside, the same contrast electrode of other structure (7) and auxiliary electrode (9), working electrode (8) also electrode external thread sleeve (12) is connected with the screw on autoclave end cap (4).
2. a kind of high temperature pressure corrosion electro-chemical measuring apparatus according to claim 1, is characterized in that: the material of described electrode external thread sleeve (12), electrode low head (14) and wire column (15) is the kovar alloy close with glass tube thermal expansivity.
3. the measuring method of high temperature pressure corrosion electro-chemical measuring apparatus described in claim 1, it is characterized in that: first, test material is processed into test electrode sheet (17), is connected with the wire column (15) of working electrode (8) lower end by wire (18); Then the electrode external thread sleeve (12) of contrast electrode (7), working electrode (8), auxiliary electrode (9) is connected with the screw be reserved on autoclave end cap (4); Subsequently test solution is poured in autoclave body (2), the liquid level of test solution will control, under wire column (15) with the tie point of wire electrode (18), to avoid wire column (15) or wire column (15) to contact with test fluid with the tie point of wire electrode (18); Autoclave fastening bolt (3) is adopted autoclave end cap (4) and autoclave body (2) to be sealed subsequently; As needs deoxygenation, close air intake opening valve (K1) and gas outlet valve (K2), by air intake opening (5), exhausr port (10), deoxygenation operation is carried out to system; Subsequently autoclave body (2) is heated, after in autoclave body (2), medium temperature reaches setting value, the wire column (15) of contrast electrode (7), working electrode (8), auxiliary electrode (9) is connected with electrochemical workstation, carries out electro-chemical test.
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Cited By (9)
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| CN106468650A (en) * | 2015-08-21 | 2017-03-01 | 中国石油天然气股份有限公司 | Reactor and corrosion test system |
| CN106644917A (en) * | 2016-08-22 | 2017-05-10 | 中国船舶重工集团公司第七二五研究所 | Electrolytic bath apparatus used for simulating deep-sea environment for electrochemical testing |
| CN108169117A (en) * | 2018-02-12 | 2018-06-15 | 华电电力科学研究院有限公司 | Electrochemical corrosion measurement device and its application method in a kind of four main tubes of boiler deoxygenation condition solution medium |
| CN108956446A (en) * | 2018-10-15 | 2018-12-07 | 浙江德威硬质合金制造有限公司 | The test method of hard alloy corrosion resistance |
| CN109269974A (en) * | 2018-11-20 | 2019-01-25 | 重庆市特种设备检测研究院 | A kind of test method of the online Electrochemical corrosion rate of boiler |
| CN109297897A (en) * | 2018-12-13 | 2019-02-01 | 福州大学 | The experimental rig and method of the high voltage electric field environmental corrosion of controllable temperature and humidity |
| CN109827898A (en) * | 2019-03-29 | 2019-05-31 | 河海大学 | A kind of metal corrosion test device |
| CN110095405A (en) * | 2019-05-30 | 2019-08-06 | 华能山东石岛湾核电有限公司 | A kind of sealing device and application method of high temperature pressure corrosion electrochemical working electrode |
| CN114221047A (en) * | 2021-12-08 | 2022-03-22 | 北京工业大学 | High-voltage-resistant battery powder testing pool |
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| CN106468650A (en) * | 2015-08-21 | 2017-03-01 | 中国石油天然气股份有限公司 | Reactor and corrosion test system |
| CN106644917A (en) * | 2016-08-22 | 2017-05-10 | 中国船舶重工集团公司第七二五研究所 | Electrolytic bath apparatus used for simulating deep-sea environment for electrochemical testing |
| CN108169117A (en) * | 2018-02-12 | 2018-06-15 | 华电电力科学研究院有限公司 | Electrochemical corrosion measurement device and its application method in a kind of four main tubes of boiler deoxygenation condition solution medium |
| CN108956446A (en) * | 2018-10-15 | 2018-12-07 | 浙江德威硬质合金制造有限公司 | The test method of hard alloy corrosion resistance |
| CN109269974A (en) * | 2018-11-20 | 2019-01-25 | 重庆市特种设备检测研究院 | A kind of test method of the online Electrochemical corrosion rate of boiler |
| CN109297897A (en) * | 2018-12-13 | 2019-02-01 | 福州大学 | The experimental rig and method of the high voltage electric field environmental corrosion of controllable temperature and humidity |
| CN109297897B (en) * | 2018-12-13 | 2023-08-18 | 福州大学 | Temperature and humidity controllable high-voltage electric field environment corrosion test device and method |
| CN109827898A (en) * | 2019-03-29 | 2019-05-31 | 河海大学 | A kind of metal corrosion test device |
| CN109827898B (en) * | 2019-03-29 | 2021-09-17 | 河海大学 | Metal corrosion test device |
| CN110095405A (en) * | 2019-05-30 | 2019-08-06 | 华能山东石岛湾核电有限公司 | A kind of sealing device and application method of high temperature pressure corrosion electrochemical working electrode |
| CN110095405B (en) * | 2019-05-30 | 2024-03-26 | 华能山东石岛湾核电有限公司 | Sealing device for high-temperature high-pressure corrosion electrochemical working electrode and use method |
| CN114221047A (en) * | 2021-12-08 | 2022-03-22 | 北京工业大学 | High-voltage-resistant battery powder testing pool |
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