CN110361437A - A kind of multi-functional electrochemical testing device and method based on pressure control - Google Patents
A kind of multi-functional electrochemical testing device and method based on pressure control Download PDFInfo
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- CN110361437A CN110361437A CN201810180299.1A CN201810180299A CN110361437A CN 110361437 A CN110361437 A CN 110361437A CN 201810180299 A CN201810180299 A CN 201810180299A CN 110361437 A CN110361437 A CN 110361437A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
A kind of multi-functional electrochemical testing device and method based on pressure control, it is characterized in that, device specifically includes that pressure control panel, first blowdown line, first constant pressure gas source, first boosted flow control valve, first intake valve, first pressure release flow control valve, differential pressure indicator, second pressure release flow control valve, second boosted flow control valve, second safety valve, first safety valve, second constant pressure gas source, second blowdown line, high temperature and high pressure kettle, glass container, movable collet, threaded screw rod, common reference electrode, method based on the device can realize the insulation of three-electrode system and surrounding structure, in conjunction with common reference electrode and differential pressure control method can realize in electro-chemical test under low temperature-hyperbaric environment, it is able to satisfy the military service operating condition of oil gas pipeline completely, and it is directed to underground high temperature and high pressure condition, join in combination with high temperature and pressure The electro-chemical test under corrosive environment is realized than electrode and differential pressure control method, reduces electrochemistry experiment cost under simulation operating condition to greatest extent.
Description
Technical field
This patent is related to metal corrosion and protection equipment technical field, is specifically to provide a kind of more function based on pressure control
Energy electrochemical testing device and method are suitable for the corrosive mediums operating condition items such as middle normal temperature and pressure, middle low temperature-high pressure, high tcmpcrauire-higb pressure
Part is particularly suitable for the middle low temperature based on common reference electrode-high pressure corrosion electrochemistry signal testing research.
Technical background
In recent years, deepening continuously with oil-gas exploration and development, HTHP peracidity oil gas well are continuously increased, are related to
Corrosive medium be mainly CO2Equal sour gas and water and part organic acid, the various pipelines and container being related to, which face, more dislikes
Bad Service Environment, wherein the oil-gas pipeline in recovery process mainly faces the corrosion of high temperature (> 100 DEG C)-high pressure multiphase medium,
And oil-gas gathering and transportation and it is long it is defeated during pipeline mainly face the corrosion of middle low temperature (< 80 DEG C)-high pressure multiphase medium, exactly these
Corrosion causes various pipelines and container in oil-gas mining and transmission process that frequent failure occurs.To prevent and reducing oil-gas pipeline
Corrosion failure accident, there is an urgent need to carry out the electrochemical corrosion experimental under Simulated Service Environment to evaluate oil-gas pipeline material
The corrosion inhibition of corrosion resistance, corrosion behavior and mechanism and novel corrosion inhibitor.In addition, low temperature-high pressure and high tcmpcrauire-higb pressure in can carrying out
Under the conditions of electrochemical corrosion experimental device be essential.However, since high-temperature and high-pressure conditions (especially high pressure) are to anti-
Answer the structures such as kettle and reference electrode that there is very high requirement, such as the insulation of electrode system, and the output of its electrochemical signals and
Measure also relatively difficult, the easy interference by surrounding metal structures and conductor of electrode signal.
Currently, to solve the above problems, mainly using following two method: the first, it is carried out in high temperature and high pressure kettle
After corrosion experiment, electrochemical signals (such as polarization curve, impedance spectrum) is measured in atmospheric conditions, actual condition can not be obtained
Electrochemical behavior during lower oil-gas pipeline material corrosion;It is second, high using the high temperature from the import of CORTEST company, the U.S.
Electrochemical testing device (equipped with expensive high temperature and pressure reference electrode) is pressed, the control of the device is not only extremely difficult, leads to reality
The success rate tested is extremely low, and price and experimental cost too expensive;The third, the country only has a small number of scholars and is based on high temperature and pressure
The experimental provision (such as CN200510011477.0 dynamic high-temperature and pressure electro-chemical measurement experimental device) of kettle transformation, the device is necessary
Using expensive high temperature and pressure reference electrode, most important its cannot be realized between electrode and surrounding metal structures well
Insulation, test process holds interference of the electrochemical signals vulnerable to surrounding metal conductor, and success rate is also very low, and test result is not
Accurately.
It is not difficult to find that so far, can accurately measure oil-gas pipeline electrochemical signals in the case where simulating operating condition due to lacking
Experimental provision affects centering hypo-hyperthermia-behavior of high-pressure metal material corrosion and mechanism further investigation.Therefore, based on general
The characteristic (operating temperature is lower than 80 DEG C, and operating pressure is generally 1-2bar) of logical reference electrode, the present invention proposes a kind of based on pressure
The multi-functional electrochemical testing device and method of power control, the device combine low in common reference electrode and differential pressure control method realization
Warm (20-80 DEG C)-high pressure electrochemistry test, fully meets the military service operating condition of oil gas pipeline, and is directed to underground high temperature and pressure
Extreme operating condition, the device combination high temperature and pressure reference electrode and differential pressure control method are realized, thus before realizing electrochemical measurement
It puts, device and experimental cost can be reduced to the greatest extent.
Summary of the invention
It is an object of the invention to propose a kind of multi-functional electrochemical testing device and method based on pressure control, with solution
Certainly in the past cannot to the oil-gas pipeline technical problem that corrosion process electrochemical signals are accurately measured under actual condition, and
While reaching above-mentioned purpose, device and experimental cost are reduced to greatest extent.
In order to achieve the above objectives, the invention adopts the following technical scheme: a kind of multi-functional electrochemistry based on pressure control
Test device, specifically includes that pressure control panel, the first blowdown line, the first admission line, the first constant pressure gas source, first into
Atmospheric pressure table, the first boosted flow control valve, the first intake valve, the first pressure release flow control valve, differential pressure indicator, the second pressure release flow
Control valve, the second intake valve, the second boosted flow control valve, the second boost gauge, the second safety valve, the first safety valve, the
Two constant pressure gas sources, the second admission line, the second blowdown line, second pressure gauge, high temperature and high pressure kettle, glass container, movable collet,
Threaded screw rod, heating mantle, kettle cover, thermometer, to electrode, working electrode, exhaust pipe, reference electrode, small air inlet hole, first pressure
Table, wherein pressure control panel is used to control the pressure of entire test macro, the first constant pressure gas source and the first admission line composition
First pressure piping is for giving glass container injection experiments gas (such as CO2) generate hyperbaric environment, the first intake valve and the first peace
Full valve is for quickly cutting off the air-flow in the first pressure piping, and the first boosted flow control valve is for controlling in the first pressure piping
Air velocity, the first boost gauge is for showing the first constant pressure bleed pressure, the first blowdown line and the first pressure release flow
Control valve is used for the pressure of unloading glass container;Second pressure piping of the second constant pressure gas source and the second admission line composition is used for
The hyperbaric environment equal with glass container is generated to high temperature and high pressure kettle injection inert gas, the second intake valve and the second safety valve are used
Air-flow in quickly the second pressure piping of cutting, for showing the second constant pressure bleed pressure, second lets out the second boost gauge
Pressure pipeline and the second pressure release flow control valve are used to unload the pressure of high temperature and high pressure kettle;Differential pressure indicator for show pressurization, pressure stabilizing and
Pressure difference between pressure leak process high temperature autoclave and glass container;First pressure gauge and second pressure gauge are respectively used to show
The pressure of glass container and high temperature and high pressure kettle, thermometer are used to show the temperature of glass container;Heating mantle is for heating high temperature height
Kettle is pressed, the liquid (water or oil) in high temperature and high pressure kettle is used to heat the solution in glass container to experimental temperature;Threaded screw rod and
For fixing glass container, threaded screw rod is fixed on kettle cover movable collet;Reference electrode, working electrode, to electrode and external
Electro-chemical test instrument is connected, and reference electrode includes common Ag/AgCl reference electrode and high temperature and pressure reference containing small air inlet hole
Electrode can directly carry out high-temperature and pressure electro-chemical measurement using high temperature and pressure reference electrode;Exhaust pipe is for excluding glass container
In air.
First boosted flow control valve of the present invention and the second boosted flow control valve can be by controlling gas flow rate
Realize that pressure is increased in glass container and high temperature and high pressure kettle with the speed of 0.02bar/s, the first pressure release flow control valve and second
Pressure release flow control valve can realize that pressure is in glass container and high temperature and high pressure kettle with the speed of 0.02bar/s by control gas flow rate
Degree reduces, precision be 0.02bar differential pressure indicator can pressure difference before real-time display glass container and high temperature and high pressure kettle, glass container and
Pressure difference between high temperature and high pressure kettle can maintain 0.2bar or less always.
Reaction vessel of the glass container of the present invention as electrochemistry experiment, can not only realize electrode system well
Insulation between surrounding structure, and its volume can be adjusted in 50ml-500ml according to experiment demand, in high temperature and high pressure kettle
Interior position liquid level can be moved up and down in and kettle lower greatly according to its volume by movable collet.
Common reference electrode active section of the present invention is located at glass container, and small air inlet hole and high temperature and high pressure kettle connect
Logical, by controlling the pressure of high temperature and high pressure kettle and glass container, pressure difference can maintain 0.2bar always hereinafter, can make commonly to join
It is worked normally under middle low temperature-hyperbaric environment than electrode.
First constant pressure gas source of the present invention and the second constant pressure gas source are sustainable constantly high to glass container and high temperature
Press provided in kettle with the equal air-flow of setting pressure, with dynamically make up in entire test process because portion gas glass container with
The pressure drop that dissolution generates in high temperature and high pressure kettle.
The invention has the following advantages over the prior art:
(1) present invention using common Ag/AgCl reference electrode and differential pressure control method can realize in low temperature (20-80 DEG C)-high pressure it is rotten
The electro-chemical test under environment is lost, is able to satisfy the military service operating condition of oil-gas transportation (collection is defeated and length is defeated) pipeline completely, and is directed to underground
The electrification under high temperature and pressure reference electrode and differential pressure control method realization corrosive environment can be used in high temperature and pressure extreme operating condition, the present invention
Test is learned, reduces electrochemistry experiment cost under simulation operating condition to greatest extent.
(2) it can be realized well using simple glass as reaction vessel of the oil-gas pipeline under high temperature pressure corrosion environment
To working electrode, reference electrode and to the insulation of electrode, surrounding metal structures are shielded completely, electro-chemical test signal is done
It disturbs.
Detailed description of the invention
Fig. 1 is electrochemical testing device schematic diagram.
Fig. 2 is pressure control panel schematic diagram.
Specific embodiment
With reference to the accompanying drawing, the present invention will be described in detail.
As shown in the picture, a kind of multi-functional electrochemical testing device based on pressure control proposed by the present invention mainly wraps
It includes: pressure control panel 1, the first blowdown line 2, the first admission line 3, the first constant pressure gas source 4, the first boost gauge 5,
One boosted flow control valve 6, the first intake valve 7, the first pressure release flow control valve 8, differential pressure indicator 9, the second pressure release flow control valve
10, the second intake valve 11, the second boosted flow control valve 12, the second boost gauge 13, the second safety valve 14, the first safety valve
15, the second constant pressure gas source 16, the second admission line 17, the second blowdown line 18, the second operating pressure table 19, high temperature and high pressure kettle
20, glass container 21, movable collet 22, threaded screw rod 23, heating mantle 24, kettle cover 25, thermometer 26, to electrode 27, work electricity
Pole 28, exhaust pipe 29, reference electrode 30, small air inlet hole 31, the first operating pressure table 32, wherein pressure control panel 1 is for controlling
The pressure of entire test macro is made, the first constant pressure gas source 4 and the first admission line 3 form the first pressure piping and be used to hold to glass
21 injection experiments gas (such as CO of device2) hyperbaric environment, the first intake valve 7 and the first safety valve 15 are generated for quickly cutting off first
Air-flow in pressure piping, the first boosted flow control valve 6 are used to control the air velocity in the first pressure piping, the first air inlet
Pressure gauge 5 is for showing 4 pressure of the first constant pressure gas source, the first blowdown line 2 and the first pressure release flow control valve 8 for unloading glass
The pressure of glass container 21;Second pressure piping of the second constant pressure gas source 16 and the second admission line 17 composition is used for high temperature and pressure
Kettle 20 injects inert gas and generates the hyperbaric environment equal with glass container 21, and the second intake valve 11 and the second safety valve 14 are used for
Quickly cutting the second pressure piping in air-flow, the second boost gauge 13 for show 16 pressure of the second constant pressure gas source, second
Blowdown line 18 and the second pressure release flow control valve 10 are used to unload the pressure of high temperature and high pressure kettle 20;Differential pressure indicator 9 increases for showing
Pressure difference between pressure, pressure stabilizing and pressure leak process high temperature autoclave 20 and glass container 21;First operating pressure table 32 and
Two operating pressure tables 19 are respectively used to the pressure of display glass container 21 and high temperature and high pressure kettle 20, and thermometer 26 is for showing glass
The temperature of container 21;Heating mantle 24 is for heating high temperature and high pressure kettle 20, and the liquid (water or oil) in high temperature and high pressure kettle 20 is for adding
Solution in thermal glass container 21 is to experimental temperature;Threaded screw rod 23 and movable collet 22 are for fixing glass container 21, screw thread
Screw rod 23 is fixed on kettle cover 25;To electrode 27, working electrode 28, Ag/AgCl reference electrode 30 and external electrochemical test
Device is connected, and reference electrode 30 includes common Ag/AgCl reference electrode and high temperature and pressure reference electrode containing small air inlet hole 31, utilizes
High temperature and pressure reference electrode can directly carry out high-temperature and pressure electro-chemical measurement;Exhaust pipe 29 is used to exclude the sky in glass container 21
Gas.
First boosted flow control valve 6 and the second boosted flow control valve 12 of the present invention can be by controlling gas stream
Speed realizes that pressure is increased in glass container 21 and high temperature and high pressure kettle 20 with the speed of 0.02bar/s, the first pressure release flow control valve 8
With the second pressure release flow control valve 10 can be realized by control gas flow rate in glass container 21 and high temperature and high pressure kettle 20 pressure with
The speed of 0.02bar/s reduces, precision be 0.02bar differential pressure indicator 9 can real-time display glass container 21 and high temperature and high pressure kettle 20 it
Preceding pressure difference, the pressure difference between glass container 21 and high temperature and high pressure kettle 20 can maintain 0.2bar or less always.
Reaction vessel of the glass container 21 of the present invention as electrochemistry experiment, can not only realize electrode body well
Insulation between system and surrounding structure, and its volume can be adjusted in 50ml-500ml according to experiment demand, in high temperature and pressure
Position in kettle 20 liquid level can be moved up and down in and kettle lower greatly according to its volume by movable collet 22.
Common reference electrode active section of the present invention is located in glass container 21, and small air inlet hole 31 is located at glass appearance
Device 21 is outer and be connected to high temperature and high pressure kettle 20, and by the pressure of control high temperature and high pressure kettle 20 and glass container 21, pressure difference can one
Directly 0.2bar is maintained hereinafter, common reference electrode 30 can be made to work normally under middle low temperature-hyperbaric environment.
First constant pressure gas source 4 of the present invention and the second constant pressure gas source 16 are sustainable constantly to glass container 21 and height
The air-flow equal with setting pressure is provided in warm autoclave 20, dynamically to make up in entire test process because portion gas is in glass
The pressure drop that dissolution generates in container 21 and high temperature and high pressure kettle 20.
To be more clear goal of the invention of the invention, technical solution and advantage, with reference to the accompanying drawing 1 and attached drawing 2 and this
Invention is based on common Ag/AgCl reference electrode, to oil gas pipeline in middle low temperature-high pressure CO2Electrochemistry is surveyed under corrosive environment
The specific embodiment of examination is illustrated, and detailed step is as follows:
A. glass container 21 is fixed on the suitable position in high temperature and high pressure kettle 20, opened on common Ag/AgCl reference electrode 30
Small air inlet hole 31, close pressure control panel 1 on all valves, complete the installation of entire test macro;
B. exhaust pipe 29, the first constant pressure gas source 4, the first safety valve 15, the first boosted flow control valve 6, the are successively slowly opened
One intake valve 7, is passed through CO2Deoxygenation is carried out to glass container 21, after the completion of deoxygenation, closes all valves and exhaust pipe 29;
C. the first constant pressure gas source 4(CO is first opened2), the first safety valve 15, the first intake valve 7, the second constant pressure gas source 16(N2),
Then second safety valve 14 and the second intake valve 11 open simultaneously the first boosted flow control valve 6 and the control of the second boosted flow
Valve 12 carries out constant speed pressurization to glass container 21 and high temperature and high pressure kettle 20 (pressure speedup is identical);
D. after reaching setting pressure, all valves is closed, heating water bath is carried out to glass container 21 with heating mantle 24, is adopted in real time
With 10 condition pressure difference of the first pressure release flow control valve 8 and the second pressure release flow control valve;
E. after reaching set temperature (20-80 DEG C), continue to open the first pressure release flow control valve 8 and the second pressure release flow control
Valve 10 carries out constant speed pressure release until system pressure is setting pressure to glass container 21 and high temperature and high pressure kettle 20;
F. the first constant pressure gas source 4 and 16 outlet pressure of the second constant pressure gas source are adjusted to setting pressure, then successively open first
Constant pressure gas source 4, the first safety valve 15, the first intake valve 7, the first boosted flow control valve 6 and the second constant pressure gas source 16, second peace
Full valve 14, the second intake valve 11 and the second boosted flow control valve 12;
G. after system balance reaches, start to carry out electrochemical signals test;
H. after completing test, all valves are first closed, then open simultaneously the first pressure release flow control valve 8 and the second pressure release flow
Control valve 11 carries out constant speed pressure release until system pressure is atmospheric pressure to glass container 21 and high temperature and high pressure kettle 20.
Claims (4)
1. a kind of multi-functional electrochemical testing device based on pressure control, which is characterized in that device specifically includes that pressure control
Panel (1), the first blowdown line (2), the first constant pressure gas source (4), the first boosted flow control valve (6), the first intake valve (7),
First pressure release flow control valve (8), differential pressure indicator (9), the second pressure release flow control valve (10), the second boosted flow control valve
(12), the second safety valve (14), the first safety valve (15), the second constant pressure gas source (16), the second blowdown line (18), high temperature and pressure
Kettle (20), glass container (21), movable collet (22), threaded screw rod (23), reference electrode (30), small air inlet hole (31), wherein
Pressure control panel (1) is used to control the pressure of entire test macro, the first constant pressure gas source (4) and the first admission line (3) group
It is used to generate hyperbaric environment, the first intake valve (7) and first to glass container (21) injection experiments gas at the first pressure piping
Safety valve (15) is for quickly cutting off the air-flow in the first pressure piping, and the first boosted flow control valve (6) is for controlling first
Air velocity in pressure piping, the first boost gauge (5) is for showing first constant pressure gas source (4) pressure, the first relief tube
Line (2) and the first pressure release flow control valve (8) are used for the pressure of unloading glass container (21);Second constant pressure gas source (16) and second
(the second pressure piping of 17 compositions is used to generate to high temperature and high pressure kettle (20) injection inert gas and glass container for admission line
(21 equal hyperbaric environments, the second intake valve (11) and the second safety valve (14) are for quickly cutting off in the second pressure piping
Air-flow, the second boost gauge (13) for showing second constant pressure gas source (16) pressure, let out by the second blowdown line (18) and second
Pressure flow control valve (10) is used to unload the pressure of high temperature and high pressure kettle (20);Differential pressure indicator (9) is for showing pressurization, pressure stabilizing and pressure release
Pressure difference between high temperature and high pressure kettle (20) and glass container (21) in the process;First operating pressure table (32) and the second work pressure
Power table (19) is respectively used to the pressure of display glass container (21) and high temperature and high pressure kettle (20), and thermometer (26) is for showing glass
The temperature of container (21);Heating mantle (24) is for heating high temperature and high pressure kettle (20), and the liquid in high temperature and high pressure kettle (20) is for adding
Solution in thermal glass container (21) is to experimental temperature;Threaded screw rod (23) and movable collet (22) are for fixing glass container
(21), threaded screw rod (23) is fixed on kettle cover (25);To electrode (27), working electrode (28), reference electrode (30) and outside
Electro-chemical test instrument is connected, and reference electrode (30) includes common Ag/AgCl reference electrode and high temperature containing small air inlet hole (31)
High pressure reference electrode can directly carry out high-temperature and pressure electro-chemical measurement using high temperature and pressure reference electrode;Exhaust pipe (29) is used for
Exclude the air in glass container (21).
2. a kind of multi-functional electrochemical testing device based on pressure control according to claim 1, it is characterised in that:
First boosted flow control valve (6) and the second boosted flow control valve (12) can realize glass container by control gas flow rate
(21) increased with high temperature and high pressure kettle (20) interior pressure with the speed of 0.02bar/s, the first pressure release flow control valve (8) and second is let out
Press flow control valve (10) can be realized by control gas flow rate glass container (21) and high temperature and high pressure kettle (20) interior pressure with
The speed of 0.02bar/s reduces, and precision is that 0.02bar differential pressure indicator (9) can real-time display glass container (21) and high temperature and high pressure kettle
(20) pressure difference before, the pressure difference between glass container (21) and high temperature and high pressure kettle (20) can maintain always a 0.2bar with
Under.
3. a kind of multi-functional electrochemical testing device based on pressure control, feature exist according to claim 1
In reaction vessel of the glass container (21) as electrochemistry experiment, not only can realize well electrode system and surrounding structure it
Between insulation, and the volume of glass container (21) can be adjusted in 50ml-500ml according to experiment demand, in high temperature and high pressure kettle
(20) position in liquid level can be moved up and down in and kettle lower greatly according to its volume by movable collet (22);Common reference electrode
(30) active section is located in glass container (21), and small air inlet hole (31) is located at glass container (21) outside and and high temperature and high pressure kettle
(20) it is connected to, by controlling the pressure of high temperature and high pressure kettle (20) and glass container (21), pressure difference can maintain always 0.2bar
Hereinafter, common reference electrode (30) can be made to work normally under middle low temperature-hyperbaric environment;First constant pressure gas source (4) and the second perseverance
Pressurized air source (16) is sustainable constantly to provide the air-flow equal with setting pressure to glass container (21) and high temperature and high pressure kettle (20),
Dynamically to make up the dissolution generation in glass container (21) and high temperature and high pressure kettle (20) because of portion gas in entire test process
Pressure drop.
4. it is a kind of based on pressure control multi-functional electrochemical test method, which is characterized in that it is described based on pressure control
Multi-functional electrochemical test method the following steps are included:
A. glass container (21) is fixed on the suitable position in high temperature and high pressure kettle (20), opens common Ag/AgCl reference electrode
(30) small air inlet hole (31) on closes all valves on pressure control panel (1), completes the installation of entire test macro;
B. exhaust pipe (29), the first constant pressure gas source (4), the first safety valve (15), the control of the first boosted flow are successively slowly opened
Valve (6), the first intake valve (7), are passed through CO2Deoxygenation is carried out to glass container (21), after the completion of deoxygenation, closes all valves and row
Tracheae (29);
C. the first constant pressure gas source (4), the first safety valve (15), the first intake valve (7), the second constant pressure gas source (16), are first opened
Two safety valves (14) and the second intake valve (11) then open simultaneously the first boosted flow control valve (6) and the second boosted flow
Control valve (12) carries out constant speed pressurization to glass container (21) and high temperature and high pressure kettle (20);
D. after reaching setting pressure, all valves is closed, heating water bath is carried out to glass container (21) with heating mantle (24), it is real
Shi Caiyong the first pressure release flow control valve (8) and second pressure release flow control valve (10) condition pressure difference;
E. after reaching set temperature (20-80 DEG C), continue to open the first pressure release flow control valve (8) and the second pressure release flow control
Valve (10) processed carries out constant speed pressure release until system pressure is setting pressure to glass container (21) and high temperature and high pressure kettle (20);
F. the first constant pressure gas source (4) and second constant pressure gas source (16) outlet pressure are adjusted to setting pressure, then successively opened
First constant pressure gas source (4), the first safety valve (15), the first intake valve (7), the first boosted flow control valve (6) and the second constant pressure
Gas source (16), the second safety valve (14), the second intake valve (11) and the second boosted flow control valve (12);
G. after system balance reaches, start to carry out electrochemical signals test;
H. after completing test, all valves are first closed, then open simultaneously the first pressure release flow control valve (8) and the second pressure release stream
Control valve (11) carries out constant speed pressure release until system pressure is that atmospheric pressure is to glass container (21) and high temperature and high pressure kettle (20)
Only.
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CN112362494A (en) * | 2020-10-15 | 2021-02-12 | 中国特种设备检测研究院 | Hydraulic bulging test system |
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