CN109100298A - Autoclave reactor and electrochemical appliance for measuring pollutant hydrothermal oxidization system - Google Patents
Autoclave reactor and electrochemical appliance for measuring pollutant hydrothermal oxidization system Download PDFInfo
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- CN109100298A CN109100298A CN201811052351.1A CN201811052351A CN109100298A CN 109100298 A CN109100298 A CN 109100298A CN 201811052351 A CN201811052351 A CN 201811052351A CN 109100298 A CN109100298 A CN 109100298A
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 52
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 51
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 51
- 239000000463 material Substances 0.000 claims abstract description 67
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 239000012530 fluid Substances 0.000 claims description 41
- 238000009434 installation Methods 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 9
- 239000007800 oxidant agent Substances 0.000 claims description 8
- 230000003750 conditioning effect Effects 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 6
- 239000003566 sealing material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007769 metal material Substances 0.000 claims description 5
- GNKTZDSRQHMHLZ-UHFFFAOYSA-N [Si].[Si].[Si].[Ti].[Ti].[Ti].[Ti].[Ti] Chemical compound [Si].[Si].[Si].[Ti].[Ti].[Ti].[Ti].[Ti] GNKTZDSRQHMHLZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 abstract description 18
- 230000007797 corrosion Effects 0.000 abstract description 18
- 238000012360 testing method Methods 0.000 abstract description 7
- 230000005518 electrochemistry Effects 0.000 abstract description 6
- 238000002848 electrochemical method Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 8
- 230000003068 static effect Effects 0.000 description 7
- 230000005611 electricity Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910021332 silicide Inorganic materials 0.000 description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical group [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 210000004508 polar body Anatomy 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
- B01J2219/0218—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components of ceramic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
- B01J2219/0277—Metal based
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0809—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes
- B01J2219/0811—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes employing three electrodes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Biodiversity & Conservation Biology (AREA)
- Toxicology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
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Abstract
A kind of electrochemical appliance the invention discloses autoclave reactor and for measuring pollutant hydrothermal oxidization system, autoclave reactor includes autoclave body and kettle cover, the autoclave body includes jacket layer and the liner layer that is set in jacket layer, the material of the jacket layer is nickel-base alloy, the material of the liner layer is ceramics, it is fixed outside the jacket layer to have heating mantle, for heating the autoclave body, low thermal conductive layer is equipped between the jacket layer and the top and the kettle cover bottom of liner layer, electrode fairlead is equipped on the kettle cover, material inlet and material outlet, electrode is equipped in the electrode fairlead, the first end of the electrode is located in autoclave body, and second end passes through electrode fairlead and is exported by lead to normal temperature and pressure area；The present invention can effectively solve the problems, such as that the prior art is existing when in use cannot carry out corrosion electrochemistry test in temperature, the higher practical pollutant hydrothermal oxidization environment of pressure.
Description
Technical field
A kind of electrochemical appliance the present invention relates to autoclave reactor and for measuring pollutant hydrothermal oxidization system, especially
It is related to related to Novel corrosion design of material for equipment material corrosion resistance monitoring in pollutant hydrothermal oxidization
Electrochemical measuring technology belongs to environmental equipment field.
Background technique
Pollutant hydrothermal oxidation technology is fast with reaction speed, oxygenolysis is thorough, equal clear superiorities without secondary pollution, and one
The directly extensive concern and attention by researcher and engineering specialists.However, with the scale trial operation of the technology,
And people are directed to going deep into for organic pollutant degradation efficiency, reaction process, apparatus, cost-effectiveness etc. research,
Problem also generates therewith.Currently, restricting one of key technical problem of the technology commercialization sizable application is mainly equipment and materials
Long-play is under the conditions of high temperature and pressure, strong oxidizing property, highly acid, hydrothermal system and waste material environment complex in composition, pole
It is subject to serious corrosion and fails.
Although the etching problem that domestic and international scientists are directed to material in hydrothermal oxidization system has been carried out more wide
General and in-depth study, but simple, feasible, efficient and with application prospect anticorrosion technique still lacks.Reason is material
Expect that the corrosion process in pollutant hydrothermal oxidization system is controlled by many factors, complex.And current most researchers
By simulate corrosive environment method carry out material corrosion test, such as use contain heteroatomic organic matter or directly use inorganic acid as
Corrosive medium.Obviously, these experimental results can only partially reflect the corrosion condition under hydrothermal condition, it is difficult to show actual motion effect
The synergistic effect of fruit and a variety of corrosion origin causes of formation.
It importance in view of above-mentioned hydrothermal oxidization system anticorrosion material and technological development and its is faced at present various
Predicament, the electrochemistry the purpose of the present invention is to provide a kind of autoclave reactor and for measuring pollutant hydrothermal oxidization system
Device can be directed to this practical systems of pollutant hydrothermal oxidization and carry out the design of anticorrosion material and grinding for anticorrosion technique
Hair, to understand derogatory behaviour and mechanism of the material under the conditions of hydrothermal oxidization in depth, detects the faulted condition of material, is pollutant
The research and development of hydrothermal oxidization equipment provide anticorrosion technique data, push the application conversion of pollutant hydrothermal oxidation technology.
Summary of the invention
The technical problem to be solved by the present invention is providing a kind of autoclave reactor and for measuring pollutant hydrothermal oxidization
The electrochemical appliance of system, for equipping the monitoring of material corrosion resistance and Novel corrosion when can be used for pollutant hydrothermal oxidization
The related electrochemical measurement of design of material, cannot be in temperature, the higher reality of pressure to solve that the prior art is existing when in use
The problem of corrosion electrochemistry test is carried out in the pollutant hydrothermal oxidization environment of border.
The technical scheme is that a kind of autoclave reactor, including autoclave body and kettle cover, the autoclave body include jacket layer
With the liner layer being set in jacket layer, the material of the jacket layer is nickel-base alloy, and the material of the liner layer is ceramics,
It is fixed outside the jacket layer to have heating mantle, for heating the autoclave body, the top and the kettle cover of the jacket layer and liner layer
It is equipped with low thermal conductive layer between bottom, electrode fairlead, material inlet and material outlet are equipped on the kettle cover, the electrode draws
Electrode is equipped in portalling, the first end of the electrode is located in autoclave body, and second end passes through electrode fairlead and leads by lead
Out to normal temperature and pressure area.
It further include temperature conditioning unit, the temperature conditioning unit includes thermocouple and temperature controller, and wherein thermocouple passes through the kettle cover
It is electrically connected for measuring the intracorporal temperature of kettle, temperature controller and thermocouple and heating mantle, for controlling the work of heating mantle.
The electrode fairlead is 3, is respectively used to installment work electrode, auxiliary electrode and reference electrode.
The working electrode, auxiliary electrode and reference electrode are wire electrode, outer surface wrap up one layer of glassy state without
Expose the bottom end of machine nonmetallic materials, wire electrode.
It is sealed between the electrode and electrode fairlead by inorganic sealing material, and keeps electrode and electrode fairlead exhausted
Edge.
The material of the low thermal conductive layer is silicide, ceramics or titanium silicate.
The material inlet is equipped with imported valve, and the material outlet is equipped with outlet valve.
The present invention also provides a kind of for measuring the electrochemical appliance of pollutant hydrothermal oxidization system, comprising:
Fluid metering pumping installations, for the mixture of prepared pollutant, water and oxidant to be pumped into fluid heater；
Fluid heater, for being heated to the mixture；
The autoclave reactor, material inlet are connect with the delivery outlet of the fluid heater；
Fluid output device, including back pressure system and depressurized system, the back pressure system and depressurized system are sequentially arranged at described
On the material outlet of autoclave reactor, by the way that the pressure of back pressure system is arranged, make to be more than the pressure inside autoclave reactor
Extra material by depressurized system depressurize after be derived automatically from autoclave reactor.
The fluid metering pumping installations is high-pressure metering pump.
The fluid heater is tube type electric-heating device.
The beneficial effects of the present invention are:
1, the autoclave body of the autoclave reactor in the present invention is made of nickel-base alloy housing and lined ceramics, avoids whole uses
Since the interaction between body material and pollutant hydrothermal oxidization system is to being carried out when nickel-base alloy makes autoclave body
Electrochemical measurement influence, keep measurement result more accurate.
2, electrode involved in the present invention, i.e. working electrode, auxiliary electrode, the reference electrode equal quilt inside autoclave body
Glassy state inorganic material is wrapped in, and to avoid the interaction around electrode material between pollutant hydrothermal oxidization system, is made
The area that electrode material and hydrothermal system interact when electrochemical measurement is more controllable.
3, it is separated by one compared with the low thermal conductive layer of low thermal conductivity when mesohigh autoclave body of the present invention connect sealing with kettle cover, makes height
The high temperature of pressure autoclave body is difficult to transmit by nickel-based alloy jacket to kettle cover, not only reduces the thermal loss of autoclave body, simultaneously
So that the temperature of high pressure kettle cover is unlikely to too high, be conducive to the sealing that autoclave covers each interface.
4, working electrode, auxiliary electrode involved in the present invention, reference electrode are placed in multifunctional high pressure autoclave body
Portion, keeps the relativity of electrochemical measurement more prominent, is applicable in system more simply, and be conducive under identical conditions
The comparative studies of the corrosion electrochemistry performance of different materials and different anticorrosion techniques.
5, the regulation of the invention by sending device to fluid metering pump, so that working electrode, auxiliary electrode, reference electrode were both
Static pollutant hydrothermal oxidization system can also can be in simultaneously simultaneously in the pollutant hydrothermal oxidization system flowed
In, it can the material corrosion electrochemical measurement in current system and static system is carried out respectively, more meets pollutant hydro-thermal oxygen
Change the actual motion condition of apparatus, specific aim is stronger, design of the data obtained for anticorrosion hydrothermal oxidization device
Advantageously.
In short, the present invention is compared with the existing various electrochemical appliances for high pressure hydrothermal system, structure is simple, performance
Stablize, measurement results reliability is high, practical, especially can be widely used for material in wider temperature and pressure range (- 500 DEG C of room temperature, often
Press -30 MPa) pollutant hydrothermal oxidization system in electrochemical corrosion measurement, and can obtain flowing and static two kinds of items
Material corrosion electrochemical data under part, measurement result is closer to actual conditions, more convincingness.
Detailed description of the invention
Fig. 1 is the sectional view of autoclave reactor；
Fig. 2 is the top view of autoclave reactor；
Fig. 3 is the structural schematic diagram of electrochemical appliance；
In attached drawing: 1 material inlet, 2 imported valves, 3 inorganic sealing materials, 4 working electrodes, 5 auxiliary electrodes, 6 glassy states are inorganic
Nonmetallic materials, 7 liner layers, 8 jacket layers, 9 heating mantles, 10 reference electrodes, 11 low thermal conductive layers, 12 kettle covers, 13 washers, 14 spiral shells
Mother, 15 bolts, 16 outlet valves, 17 material outlets, 18 thermocouples, 19 contact conductors.
Specific embodiment
With reference to the accompanying drawing and invention is described further in specific embodiment:
A kind of autoclave reactor according to the present invention, including autoclave body and kettle cover 12, autoclave body are pollutant hydrothermal oxidization system and electricity
Polar body system interacts to carry out the place of electrochemical measurement, is equivalent to the effect of electrolytic cell, autoclave body and kettle cover 12 using conventional
Connection type, such as bolt 15 connect.In one example, pass through 8 bolts 15 and nut 14 between autoclave body and kettle cover 12
It is attached and seals, wherein bolt 15 passes through kettle cover 12 and is connected in autoclave body, passes through nut 14 and washer on 15 top of bolt
13 realization kettle covers 12 are fastenedly connected with autoclave body.
Autoclave body includes jacket layer 8 and the liner layer 7 that is set in jacket layer 8, and wherein the material of jacket layer 8 is Ni-based conjunction
Gold, the material of liner layer 7 is ceramics, fixed outside jacket layer 8 to have heating mantle 9, for heating the autoclave body.Preferably, it heats
Set 9 is electric heater
Low thermal conductive layer 11 is equipped between 12 bottom of the top and kettle cover of jacket layer 8 and liner layer 7, the material of low thermal conductive layer 11 is
Silicide, ceramics, titanium silicate etc..To reduce from autoclave body to the heat transfer of kettle cover 12, avoid 12 temperature of kettle cover excessively high and unfavorable
In the sealing of each interface.
Electrode fairlead, material inlet 1 and material outlet 17 are equipped on kettle cover 12, wherein material inlet 1 and material go out
Mouth 17 is respectively used to pollutant hydrothermal oxidization fluid be imported and exported autoclave body, and electrode fairlead is used to install electrode,
The quantity of electrode is installed according to actual needs.In one example, electrode fairlead is 3, is respectively used to installment work
The first end of electrode 4, auxiliary electrode 5 and reference electrode 10, each electrode is located in autoclave body, and second end passes through electrode fairlead simultaneously
It is exported by lead to normal temperature and pressure area, is connect with the electrochemical workstation respective electrode for being in room temperature pressure area together, to carry out dirt
Contaminate the electrochemical measurement under the conditions of object hydrothermal oxidization.It, can be using a variety of electrochemical methods to dirt by the electrochemical workstation
The material contaminated in object hydrothermal oxidization system carries out electrochemical corrosion measurement, as steady-state polarization test, Ta Feier test, volt-ampere are surveyed
Examination, ac impedance measurement, step test etc..
In one example, material inlet 1 is equipped with imported valve 2, and material outlet 17 is equipped with outlet valve 16.
Preferably, electrode is wire electrode.In one example, working electrode 4, auxiliary electrode 5 and reference electrode 10 are equal
For wire electrode, one layer of glassy state inorganic non-metallic material 6 is wrapped up in outer surface, and the bottom end of wire electrode is exposed.The glassy state
The effect of inorganic non-metallic material 6 is for surrounding them to be sealed, it is isolated with hydrothermal system, and only by electrode bottom
End is exposed, to carry out various electro-chemical tests in pollutant hydrothermal oxidization system.In one example, glassy state inorganic non-metallic
Material 6 is barium monoxide-calcia-alumina-silica, magnesia-calcia-alumina-silica, calcia-alumina-
Silica etc..
It is sealed between electrode and electrode fairlead by inorganic non-metallic sealing material, and keeps electrode and electrode fairlead exhausted
Edge.Specifically, working electrode 4, auxiliary electrode 5, reference electrode 10 by the electrode fairlead of kettle cover 12 by autoclave body inside
It when exporting to the outside of room temperature pressure area, is sealed by inorganic non-metallic sealing material, and electrode and leadout hole is made to insulate.?
In one example, three electrodes in pollutant hydrothermal oxidization system are connected to the electrochemical operation in room temperature pressure area
The contact conductor 19 for respective electrode of standing is the precious metal of certain diameter.
Preferably, temperature conditioning unit is installed on autoclave reactor, temperature conditioning unit includes thermocouple 18 and temperature controller,
Middle thermocouple 18 passes through the kettle cover 12 for measuring the intracorporal temperature of kettle, and temperature controller is electric with thermocouple 18 and heating mantle 9 respectively
Gas connection, for controlling the work of heating mantle 9.So the intracorporal temperature of kettle can be detected by thermocouple 18, and then feed back to temperature
Device is controlled, then by the work of temperature controller control heating mantle 9, the intracorporal temperature of autoclave reactor kettle is regulated and controled with realizing.Heating mantle 9
It is preferred that electric heater, can also be convenient for covering the heater heated on autoclave body to be any of.
It is a kind of for measuring the electrochemical appliance of pollutant hydrothermal oxidization system according to the present invention, comprising: fluid metering pump
Send device, fluid heater, autoclave reactor and fluid output device, wherein fluid metering pumping installations will be for that will match
The mixture of the pollutant, water and the oxidant that make is pumped into fluid heater, and fluid heater is used for the mixture
Heating, for heating the mixture of pollutant, water, oxidant, forms it into pollutant hydrothermal oxidization system, autoclave
Reactor is used to provide the described the hydrothermal oxidization of mixture, and material inlet 1 is connect with the delivery outlet of fluid heater, fluid
Output device includes back pressure system and depressurized system, and back pressure system and depressurized system are sequentially arranged at the autoclave reactor
On material outlet 17, by the way that the pressure of back pressure system is arranged, make logical more than the extra material of the pressure inside autoclave reactor
Autoclave reactor is derived automatically from after crossing depressurized system decompression.
Preferably, fluid metering pumping installations is high-pressure metering pump, and fluid heater is one and autoclave reactor object
The tube type electric-heating device that is connected of material import 1, the outlet of another port and high-pressure metering pump, the back pressure system and
Depressurized system is existing conventional system, and back pressure system is mainly made of counterbalance valve, and depressurized system mainly by reducer unit at.
In one example, for fluid metering pumping installations in conveying, delivery rate range is 1-20 ml/min.
By regulating and controlling the delivery rate of fluid metering pumping installations, working electrode 4, auxiliary electrode 5, reference electrode 10 can be made while being located
In pollutant hydrothermal oxidization system different in flow rate, corrosion electricity of the material under the conditions of pollutant hydrothermal oxidization of flowing is measured
Chemical data.
In one example, outlet valve 16 is closed, and enters autoclave in a certain amount of pollutant hydrothermal oxidization fluid
Behind reactor autoclave body inside, fluid metering pumping installations is closed, working electrode 4, auxiliary electrode 5, reference electrode 10 can be made same
When in static pollutant hydrothermal oxidization system, measure material under the conditions of static pollutant hydrothermal oxidization corrosion electricity
Chemical data.
A kind of method that electrochemical appliance carries out the electrochemical measurement under the conditions of pollutant hydrothermal oxidization according to the present invention, packet
Include following steps:
(1) electrochemical measurement system is assembled
Step 1: outside using 6 pairs of glassy state inorganic non-metallic material Filamentous working electrodes 4, auxiliary electrode 5, reference electrode 10
Surface is wrapped up, and keeps apart surrounding them with locating hydrothermal oxidization system, and by the emery cloth of certain partial size by electrode
End face is polished, and the electrode surface with certain surface product is obtained, which directly contacts with pollutant hydrothermal oxidization system,
It is the main region that electrochemical reaction occurs.
Step 2: being exported by inorganic sealing material 3 to autoclave body, this is without secret after electrode fabrication is good
Closure material 3 not only plays the role of sealing, but also electrode is made to insulate with kettle cover 12 by the insulating materials.Working electrode 4, auxiliary electricity
Pole 5, reference electrode 10 are fixed on kettle cover 12 according to certain requirement, after kettle cover 12 connect sealing with autoclave body, also just certainly
It so is placed in inside autoclave body.
Step 3: autoclave body and kettle cover 12 are connected by bolt 15, nut 14 and gasket, make working electrode 4,
Auxiliary electrode 5 and reference electrode 10 are placed in inside autoclave body simultaneously, and by its outside lead and in the electricity of room temperature pressure area
Chem workstation respective electrode connects.
(2) electrochemical measurement under the conditions of pollutant hydrothermal oxidization
Step 1: pollutant, water, oxidant are configured to fluid-mixing according to certain mass ratio, wherein oxidant is normal
The oxidant of rule, such as hydrogen peroxide, configuration proportion are usually hydrogen peroxide mass content 30%.
Step 2: opening fluid heater, kept constant after its temperature reaches set temperature.
Step 3: the mixture of prepared pollutant, water, oxidant is squeezed into fluid by fluid metering pumping installations
Heating device, make its via fluid heater after, pass through the material inlet 1 that is placed on multifunctional high pressure kettle cover 12 and import high pressure
Inside autoclave body.
Step 4: opening heating and the temperature conditioning unit of autoclave reactor, keep permanent after its temperature reaches set temperature
It is fixed.
Step 5: the counterbalance valve pressure of setting fluid output device, makes the extra fluid more than the pressure pass through decompression
Autoclave body is exported after valve decompression, to guarantee that the electrode inside autoclave body is in identical with pollutant hydrothermal oxidization system always
Under the conditions of pressure and temperature.
Step 6: electrochemical measurement.
Current system: more more than counterbalance valve pressure after pollutant hydrothermal oxidization fluid enters autoclave body inside
Residual current body exports autoclave body after depressurizing by pressure reducing valve, makes to keep the disengaging of fluid to reach dynamic equilibrium inside autoclave body,
And the corrosion after temperature and pressure is stablized, by electrochemical workstation to material in the pollutant hydrothermal oxidization system of flowing
Electrochemistry can be carried out test.
Static system: the material export valve of fluid output device is closed, and is entered in pollutant hydrothermal oxidization fluid
Inside autoclave body and after reaching a certain amount, the material closed on fluid metering pumping installations and high pressure kettle cover 12 imports valve
Door, makes the temperature and pressure of the pollutant hydrothermal oxidization system inside autoclave body reach stable, then passes through electrochemical operation
It stands and corrosion electrochemistry performance of the material in static pollutant hydrothermal oxidization system is tested.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (10)
1. a kind of autoclave reactor, including autoclave body and kettle cover (12), it is characterised in that: the autoclave body include jacket layer (8) and
The liner layer (7) being set in jacket layer (8), the material of the jacket layer (8) are nickel-base alloy, the material of the liner layer (7)
Matter is ceramics, fixed outside the jacket layer (8) to have heating mantle (9), for heating the autoclave body, the jacket layer (8) and interior
Low thermal conductive layer (11) are equipped between the top and the kettle cover (12) bottom of lining (7), electrode is equipped on the kettle cover (12)
Fairlead, material inlet (1) and material outlet (17), the electrode fairlead is interior to be equipped with electrode, the first end position of the electrode
In in autoclave body, and second end passes through electrode fairlead and is exported by lead to normal temperature and pressure area.
2. autoclave reactor according to claim 1, it is characterised in that: it further include temperature conditioning unit, the temperature conditioning unit
Including thermocouple (18) and temperature controller, wherein thermocouple (18) passes through the kettle cover (12) and is used to measure the intracorporal temperature of kettle, temperature
It controls device and thermocouple (18) and heating mantle (9) is electrically connected, for controlling the work of heating mantle (9).
3. autoclave reactor according to claim 1, it is characterised in that: the electrode fairlead is 3, is respectively used to
Installment work electrode (4), auxiliary electrode (5) and reference electrode (10).
4. autoclave reactor according to claim 1, it is characterised in that: the working electrode (4), auxiliary electrode (5)
It is wire electrode with reference electrode (10), one layer of glassy state inorganic non-metallic material (6) is wrapped up in outer surface, wire electrode
Expose bottom end.
5. autoclave reactor according to claim 1, it is characterised in that: pass through between the electrode and electrode fairlead
Inorganic sealing material (3) sealing, and electrode and electrode fairlead is made to insulate.
6. autoclave reactor according to claim 1, it is characterised in that: the material of the low thermal conductive layer (11) is silication
Object, ceramics or titanium silicate.
7. autoclave reactor according to claim 1, it is characterised in that: the material inlet (1) is equipped with inlet valve
Door (2), the material outlet (17) are equipped with outlet valve (16).
8. a kind of for measuring the electrochemical appliance of pollutant hydrothermal oxidization system characterized by comprising
Fluid metering pumping installations, for the mixture of prepared pollutant, water and oxidant to be pumped into fluid heater；
Fluid heater, for being heated to the mixture；
Any autoclave reactor of claim 1 to 7, the output of material inlet (1) and the fluid heater
Mouth connection；
Fluid output device, including back pressure system and depressurized system, the back pressure system and depressurized system are sequentially arranged at described
On the material outlet (17) of autoclave reactor, by the way that the pressure of back pressure system is arranged, make to be more than to be somebody's turn to do inside autoclave reactor
The extra material of pressure is derived automatically from autoclave reactor after depressurizing by depressurized system.
9. according to claim 8 for measuring the electrochemical appliance of pollutant hydrothermal oxidization system, it is characterised in that: institute
Stating fluid metering pumping installations is high-pressure metering pump.
10. according to claim 8 for measuring the electrochemical appliance of pollutant hydrothermal oxidization system, it is characterised in that:
The fluid heater is tube type electric-heating device.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109916526A (en) * | 2019-03-11 | 2019-06-21 | 西北工业大学 | A kind of the back pin configuration and preparation method of the extraction of the ito thin film thermocouple electric signal on turbo blade |
| CN110102235A (en) * | 2019-05-07 | 2019-08-09 | 北京缔森科技发展有限公司 | A kind of high-temperature and high pressure electrochemistry reactor |
| CN110420607A (en) * | 2019-08-19 | 2019-11-08 | 遵义师范学院 | Material corrosion behavioral study device and its reaction kettle in hydrothermal system |
| CN110575799A (en) * | 2019-10-24 | 2019-12-17 | 西南大学 | Tank for researching electromagnetic field chemical effect |
| CN112221433A (en) * | 2020-08-18 | 2021-01-15 | 华电电力科学研究院有限公司 | Double-kettle test device and method suitable for high-temperature and high-pressure water environment or steam environment |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002102671A (en) * | 2000-09-29 | 2002-04-09 | Toshiba Corp | High pressure corrosion resistant reaction vessel, treatment apparatus, and method for corrosion resistant treatment of the apparatus |
| CN101520402A (en) * | 2009-02-24 | 2009-09-02 | 上海大学 | Experimental facility for testing electrochemical signals of various materials in high-temperature high-pressure environment |
| CN101865816A (en) * | 2010-05-28 | 2010-10-20 | 北京科技大学 | Experimental apparatus for high-temperature high-pressure loop spray corrosion simulation and electrochemical testing |
| CN102288504A (en) * | 2011-07-22 | 2011-12-21 | 中国科学院金属研究所 | High-temperature high-pressure in-situ scratching and corrosive wear test device |
| CN103940863A (en) * | 2014-03-14 | 2014-07-23 | 长沙理工大学 | Autoclave apparatus for measuring high temperature electrochemistry, and method thereof |
| 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 |
| CN105806774A (en) * | 2016-05-16 | 2016-07-27 | 天津大学 | High-temperature high-pressure dynamic electrochemical test experimental device and test method |
| CN208751994U (en) * | 2018-09-10 | 2019-04-16 | 遵义师范学院 | Autoclave reactor and electrochemical appliance for measuring pollutant hydrothermal oxidization system |
-
2018
- 2018-09-10 CN CN201811052351.1A patent/CN109100298A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002102671A (en) * | 2000-09-29 | 2002-04-09 | Toshiba Corp | High pressure corrosion resistant reaction vessel, treatment apparatus, and method for corrosion resistant treatment of the apparatus |
| CN101520402A (en) * | 2009-02-24 | 2009-09-02 | 上海大学 | Experimental facility for testing electrochemical signals of various materials in high-temperature high-pressure environment |
| CN101865816A (en) * | 2010-05-28 | 2010-10-20 | 北京科技大学 | Experimental apparatus for high-temperature high-pressure loop spray corrosion simulation and electrochemical testing |
| CN102288504A (en) * | 2011-07-22 | 2011-12-21 | 中国科学院金属研究所 | High-temperature high-pressure in-situ scratching and corrosive wear test device |
| CN103940863A (en) * | 2014-03-14 | 2014-07-23 | 长沙理工大学 | Autoclave apparatus for measuring high temperature electrochemistry, and method thereof |
| 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 |
| CN105806774A (en) * | 2016-05-16 | 2016-07-27 | 天津大学 | High-temperature high-pressure dynamic electrochemical test experimental device and test method |
| CN208751994U (en) * | 2018-09-10 | 2019-04-16 | 遵义师范学院 | Autoclave reactor and electrochemical appliance for measuring pollutant hydrothermal oxidization system |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109916526A (en) * | 2019-03-11 | 2019-06-21 | 西北工业大学 | A kind of the back pin configuration and preparation method of the extraction of the ito thin film thermocouple electric signal on turbo blade |
| CN110102235A (en) * | 2019-05-07 | 2019-08-09 | 北京缔森科技发展有限公司 | A kind of high-temperature and high pressure electrochemistry reactor |
| CN110420607A (en) * | 2019-08-19 | 2019-11-08 | 遵义师范学院 | Material corrosion behavioral study device and its reaction kettle in hydrothermal system |
| CN110575799A (en) * | 2019-10-24 | 2019-12-17 | 西南大学 | Tank for researching electromagnetic field chemical effect |
| CN113529115A (en) * | 2020-04-16 | 2021-10-22 | 中国科学院大连化学物理研究所 | Double-cell high-voltage electrochemical reaction device |
| CN113529115B (en) * | 2020-04-16 | 2022-09-16 | 中国科学院大连化学物理研究所 | Double-cell high-voltage electrochemical reaction device |
| CN112221433A (en) * | 2020-08-18 | 2021-01-15 | 华电电力科学研究院有限公司 | Double-kettle test device and method suitable for high-temperature and high-pressure water environment or steam environment |
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