CN106770536A - The electrolytic cell of electrochemical measurement under the conditions of a kind of concentrated acid for high temperature - Google Patents
The electrolytic cell of electrochemical measurement under the conditions of a kind of concentrated acid for high temperature Download PDFInfo
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- CN106770536A CN106770536A CN201710096632.6A CN201710096632A CN106770536A CN 106770536 A CN106770536 A CN 106770536A CN 201710096632 A CN201710096632 A CN 201710096632A CN 106770536 A CN106770536 A CN 106770536A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
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Abstract
The invention discloses a kind of electrolytic cell of electrochemical measurement under the conditions of concentrated acid for high temperature, interlayer cylinder and the cover supporting with the cylinder including holding electrolyte, place the L-type glass tube of reference electrode, place the horizontal ground-glass joints of working electrode, the oil inlet connected with the cylinder body outer wall, the oil-out connected with the cylinder body outer wall.On the one hand electrolytic cell of the present invention can simulate the actual operating condition of high-temperature fuel cell, probe into catalytic performance and Catalysis Principles of the catalyst under this harsh conditions；On the other hand electrochemistry three-electrode system can also be simulated, the electrochemical measurement under different temperatures and concentration conditions is carried out to catalyst.Simple structure of the present invention, assembling, easy to operate, catalytic performance that can be under rapid evaluation catalyst different condition.
Description
Technical field
The invention belongs to electrochemical measuring technology field, in particular it relates to a kind of under the conditions of high temperature concentrated acid
The electrolytic cell of electrochemical measurement.
Background technology
Proton Exchange Membrane Fuel Cells (HT-PEMFCs) based on phosphate-doped PBI because its electrolyte SPA have compared with
Low-vapor pressure and can be run at a temperature of 100-200 DEG C, compared to being based onFilm and it is only capable of below 100 DEG C
The low-temperature protonic exchange film fuel battery (LT-PEMFCs) of operation, HT-PEMFCs has anti-CO and SO higher2Poisoning capability
And faster reaction rate the advantages of.Meanwhile, high temperature can also make battery produce the product of vaporous, and then simplify battery
Single-phase water management, improves the utilization ratio of used heat product.HT-PEMFCs is therefore as generator efficiently, environmentally friendly in hair
The aspect such as power station and compact power is with a wide range of applications.HT-PEMFCs still need update with maintain its work as
Preceding market position
In electrocatalytic reaction, reaction rate often by catalyst freely activity digit and reactant and product reach and
The mass transport for leaving these active sites is determined.Phosphoric acid is because of its strong absorption to Pt active sites and poisons and to vapor reaction
It is relatively low that the low solubility and low transmission rate of thing turn into the cathode-current density for causing HT-PEMFCs particularly hydrogen reduction to occur
Key reason.To probe into the H of various concentrations and temperature3PO4Solution is on the influence degree of catalyst oxygen reduction performance and the tool of influence
Body mechanism, and also to characterize the hydrogen reduction catalytic performance of new catalyst, a set of HT-PEMFCs high temperature and dense of can simulating
The electrochemical testing device of acid environment seems particularly significant.
Conventional electrochemical test device is different from, the novel test device needs to realize the regulation and control of electrolyte temperature, and energy
High temperature and strong acid are enough tolerated, the device need to meet the measurement demand of the working electrode based on gas-diffusion electrode operation principle, together
When working electrode catalyst layer must keep extremely short spacing with reference electrode, with the voltage for avoiding high concentration electrolyte from causing
Drop, reference electrode is also required to keep appropriately distance with bulk electrolysis liquid, to avoid the jumping effect reference electricity of electrolyte temperature
The stability of electrode potential.
The content of the invention
Present invention aim to address the deficiencies in the prior art, there is provided one kind is for electrochemical measurement under the conditions of high temperature concentrated acid
Electrolytic cell, on the one hand electrolytic cell of the present invention can simulate the actual operating condition of high-temperature fuel cell, probe into catalyst herein
Catalytic performance and Catalysis Principles under harsh conditions；On the other hand electrochemistry three-electrode system can also be simulated, catalyst is entered
Electrochemical measurement under row different temperatures and concentration conditions.
To achieve the above object, the electrolytic cell for electrochemical measurement under the conditions of high temperature concentrated acid designed by the present invention, bag
The interlayer cylinder and the cover supporting with the cylinder for holding electrolyte are included, multiple circular holes, institute are provided with the cover end face
The middle side part for stating cylinder is provided with L-type glass tube for placing reference electrode, and one end of the L-type glass tube is capillary
Pipe, the Capillary of the L-type glass tube is penetrated in the cylinder, and the other end of the L-type glass tube is used to place reference electricity
Pole；
The cylinder with the L-type glass tube opposite side in the middle part of be provided with place working electrode horizontal ground glass connect
Head, the ground-glass joints are connected in the cylinder inboard wall；
The cylinder is provided with oil inlet in the middle side lower part of the L-type glass tube and the ground-glass joints, institute
Oil inlet is stated to be connected with the outer wall of the cylinder；
The cylinder is provided with oil-out in the oil inlet with respect to upper lateral part, the outer wall of the oil-out and the cylinder
Connect.
Preferably, the cover material is polytetrafluoroethylene (PTFE).
Preferably, 3 circular holes are provided with the cover end face, for fixing auxiliary electrode, thermocouple.
Preferably, the cylinder is cylinder.
Preferably, the capillary is Luggin capillary, and Luggin capillary belongs to one kind of salt bridge, mainly uses
To eliminate liquid potential and solution resistance.
Preferably, on the capillary and the same center line of the ground-glass joints.
Preferably, the capillary and the distance of working electrode catalyst layer are 2~2.5mm.
Preferably, the working electrode is gas-diffusion electrode.
Preferably, the electrolytic cell material is borosilicate glass material.
Used as more preferably scheme, the L-type glass tube is more than the 2/ of the cylinder internal diameter with the spacing of the cylinder body outer wall
5。
The present invention has advantages below：
First, the present invention is resistant to height for measuring hydrogen reduction catalytic capability of the catalyst under the conditions of high temperature, concentrated acid
Gentle strong acid；
Second, used as common electrochemistry three-electrode system, measurement catalyst is in different temperatures and concentration conditions for the present invention
Under chemical property, disclosure satisfy that the measurement demand of the working electrode based on gas-diffusion electrode operation principle；
3rd, the working electrode catalyst layer of electrolytic cell of the present invention keeps extremely short spacing with reference electrode, it is to avoid height
The voltage drop that concentration electrolytic solution is caused；Reference electrode and bulk electrolysis liquid keeps appropriately distance, it is to avoid electrolyte temperature
The stability of jumping effect reference electrode current potential；
4th, simple structure of the present invention is assembling, easy to operate, catalysis that can be under rapid evaluation catalyst different condition
Performance.
Brief description of the drawings
Fig. 1 is main view cross-sectional view of the invention；
Fig. 2 is that right side of the invention regards cross-sectional view；
Fig. 3 is overlooking the structure diagram of the invention；
Fig. 4 is the overlooking the structure diagram of cover in the present invention.
In figure, 1- cylinders, 2- covers, 3-L types glass tube, 4- capillaries, 5- circular holes, 6- ground-glass joints, 7- oil-feeds
Mouth, 8- oil-outs, 9- inwalls, 10- outer walls.
Specific embodiment
The present invention is described in detail below in conjunction with the accompanying drawings：
As shown in Figure 1, Figure 2, Figure 3, Figure 4, the invention provides electrochemical measurement under the conditions of a kind of concentrated acid for high temperature
Electrolytic cell, including the interlayer cylinder 1 and the cover 2 supporting with the cylinder 1 of electrolyte are held, set on the end face of the cover 2
There are multiple circular holes 5, a middle side part of the cylinder 1 is provided with the L-type glass tube 3 for placing reference electrode, the L-type glass
One end of pipe 3 is capillary 4, and the end of capillary 4 of the L-type glass tube 3 is penetrated in the cylinder 1, the L-type glass tube 3
The other end is used to place reference electrode；The cylinder 1 with the opposite side of L-type glass tube 3 in the middle part of be provided with placement work electricity
The horizontal ground-glass joints 3 of pole, the ground-glass joints 6 are connected in the inwall 9 of the cylinder 1；The cylinder 1 is in the L
Type glass tube 3 is provided with oil inlet 7, the oil inlet 7 and the cylinder 1 with the middle side lower part of the ground-glass joints 6
Outer wall 10 connect；The cylinder 1 is provided with oil-out 8 in the oil inlet 7 with respect to upper lateral part, the oil-out 8 with it is described
The outer wall 10 of cylinder 1 is connected, and the material of the cover 2 is polytetrafluoroethylene (PTFE), and 3 circular holes 5, institute are provided with the end face of the cover 2
It is cylinder to state cylinder 1, and the capillary 4 is Luggin capillary, during the capillary 4 is same with the ground-glass joints 6
On heart line, the capillary 4 is 2~2.5mm with the distance of working electrode catalyst layer, and the working electrode is gas diffusion electricity
Pole, the electrolytic cell material is borosilicate glass material, and the L-type glass tube 3 is more than described with the spacing of the outer wall 10 of the cylinder 1
The 2/5 of the internal diameter of cylinder 1.
Operation principle of the invention is, during test, working electrode to be measured is put the ring set of polytetrafluoroethylene (PTFE) material, insertion
Connect in the ground-glass joints 3 of the inwall 9 of cylinder 1, working electrode to be measured is combined closely with cylinder 1, and working electrode
The distance between Luggin capillary of catalyst layer and the one end of L-type glass tube 3 is 2~2.5mm.Then to cylinder 1 and L-type glass
The electrolyte solution to be measured of the height of cylinder 1 2/3 is added in pipe 3, the bubble of remaining in L-type glass tube 3 is drained.Again by oil inlet 7,
Oil-out 8 is connected with external temperature adjusting means, and design temperature is to treat measured value.After liquid temperature stabilization to be electrolysed, by reversible hydrogen electricity
Pole is put into after salt bridge in stretching into L-type glass tube 3, it is desirable to reference electrode and electrolyte contacts.Cover 2 is covered on cylinder 1, will be auxiliary
In helping electrode to stretch into electrolyte by circular hole 51, rotation cover 2 make auxiliary electrode and working electrode as close possible to；By thermocouple
In being put into the glass tube with conduction oil and stretching into electrolyte by circular hole 52, thermocouple bottom stretches at cylinder 1/2 and is
Preferably, and away from working electrode and auxiliary electrode to avoid interference, the thermocouple other end is connected to temperature-adjusting device to feed back tune
Section electrolyte temperature.Just electrochemistry survey can be started after connection working electrode, auxiliary electrode and reference electrode to electrochemical workstation
Amount.
Adjustment external temperature adjusting means, just can realize the electro-chemical test under different temperatures；Change electrolyte and gas
Diffusion electrode, just can realize the electro-chemical test under different electrolytes concentration and different catalysts.
The specific embodiment of present invention described above, is not intended to limit the scope of the present invention..Any basis
Various other corresponding change and deformation that technology design of the invention is made, should be included in the guarantor of the claims in the present invention
In the range of shield.
Claims (10)
1. under the conditions of a kind of concentrated acid for high temperature electrochemical measurement electrolytic cell, it is characterised in that：Folder including holding electrolyte
Layer cylinder (1) and the cover (2) supporting with the cylinder (1), multiple circular holes (5) are provided with cover (2) end face, described
One middle side part of cylinder (1) is provided with the L-type glass tube (3) for placing reference electrode, one end of the L-type glass tube (3)
It is capillary (4) that capillary (4) end of the L-type glass tube (3) is penetrated in the cylinder (1), the L-type glass tube (3)
The other end is used to place reference electrode；
The cylinder (1) is being provided with the horizontal ground glass of placement working electrode with L-type glass tube (3) opposite side middle part
Joint (6), the ground-glass joints (6) are connected in the cylinder (1) inwall (9)；
The cylinder (1) is provided with oil-feed in the L-type glass tube (3) and the middle side lower part of the ground-glass joints (6)
Mouth (7), the oil inlet (7) is connected with the outer wall (10) of the cylinder (1)；
The cylinder (1) is provided with oil-out (8), the oil-out (8) and the cylinder in the oil inlet (7) with respect to upper lateral part
The outer wall (10) of body (1) is connected.
2. under the conditions of the concentrated acid for high temperature according to claim 1 electrochemical measurement electrolytic cell, it is characterised in that：It is described
Cover (2) material is polytetrafluoroethylene (PTFE).
3. under the conditions of the concentrated acid for high temperature according to claim 1 electrochemical measurement electrolytic cell, it is characterised in that：It is described
3 circular holes (5) are provided with cover (2) end face.
4. under the conditions of the concentrated acid for high temperature according to claim 1 electrochemical measurement electrolytic cell, it is characterised in that：It is described
Cylinder (1) is cylinder.
5. under the conditions of the concentrated acid for high temperature according to claim 1 electrochemical measurement electrolytic cell, it is characterised in that：It is described
Capillary (4) is Luggin capillary.
6. the electrolytic cell for electrochemical measurement under the conditions of high temperature concentrated acid according to any one in Claims 1 to 5, its
It is characterised by：On the capillary (4) and the ground-glass joints (6) same center line.
7. the electrolytic cell for electrochemical measurement under the conditions of high temperature concentrated acid according to any one in Claims 1 to 5, its
It is characterised by：The capillary (4) is 2~2.5mm with the distance of working electrode catalyst layer.
8. the electrolytic cell for electrochemical measurement under the conditions of high temperature concentrated acid according to any one in Claims 1 to 5, its
It is characterised by：The working electrode is gas-diffusion electrode.
9. the electrolytic cell for electrochemical measurement under the conditions of high temperature concentrated acid according to any one in Claims 1 to 5, its
It is characterised by：The electrolytic cell material is borosilicate glass material.
10. the electrolytic cell for electrochemical measurement under the conditions of high temperature concentrated acid according to any one in Claims 1 to 5,
It is characterized in that：The L-type glass tube (3) is more than the 2/ of the cylinder (1) internal diameter with the spacing of the cylinder (1) outer wall (10)
5。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710096632.6A CN106770536A (en) | 2017-02-22 | 2017-02-22 | The electrolytic cell of electrochemical measurement under the conditions of a kind of concentrated acid for high temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710096632.6A CN106770536A (en) | 2017-02-22 | 2017-02-22 | The electrolytic cell of electrochemical measurement under the conditions of a kind of concentrated acid for high temperature |
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| Publication Number | Publication Date |
|---|---|
| CN106770536A true CN106770536A (en) | 2017-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710096632.6A Pending CN106770536A (en) | 2017-02-22 | 2017-02-22 | The electrolytic cell of electrochemical measurement under the conditions of a kind of concentrated acid for high temperature |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109143100A (en) * | 2018-08-28 | 2019-01-04 | 重庆大学 | A kind of small-sized fuel battery stability test device |
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| US3032493A (en) * | 1959-12-31 | 1962-05-01 | Dohrmann Instr Company | Electrolytic titration apparatus |
| JP2008261711A (en) * | 2007-04-11 | 2008-10-30 | Toyota Motor Corp | Electrochemical measuring device |
| CN102735604A (en) * | 2012-06-13 | 2012-10-17 | 上海大学 | Electrolytic cell for corrosion electrochemical measurement |
| CN203479745U (en) * | 2013-08-27 | 2014-03-12 | 工业和信息化部电子第五研究所华东分所 | Electrochemical testing device for three-electrode system |
| CN204116270U (en) * | 2014-10-29 | 2015-01-21 | 国家电网公司 | Can the coulometry minor amount of water electrolytic cell bottle of constant temperature |
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2017
- 2017-02-22 CN CN201710096632.6A patent/CN106770536A/en active Pending
Patent Citations (7)
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|---|---|---|---|---|
| US3032493A (en) * | 1959-12-31 | 1962-05-01 | Dohrmann Instr Company | Electrolytic titration apparatus |
| JP2008261711A (en) * | 2007-04-11 | 2008-10-30 | Toyota Motor Corp | Electrochemical measuring device |
| CN102735604A (en) * | 2012-06-13 | 2012-10-17 | 上海大学 | Electrolytic cell for corrosion electrochemical measurement |
| CN203479745U (en) * | 2013-08-27 | 2014-03-12 | 工业和信息化部电子第五研究所华东分所 | Electrochemical testing device for three-electrode system |
| CN204116270U (en) * | 2014-10-29 | 2015-01-21 | 国家电网公司 | Can the coulometry minor amount of water electrolytic cell bottle of constant temperature |
| CN204649680U (en) * | 2015-05-27 | 2015-09-16 | 汪强 | A kind of electrolytic cell for measuring oxygen reduction reaction |
| CN204988980U (en) * | 2015-09-06 | 2016-01-20 | 南京钢铁股份有限公司 | Corrode electrochemistry measuring constant temperature electrolytic bath |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109143100A (en) * | 2018-08-28 | 2019-01-04 | 重庆大学 | A kind of small-sized fuel battery stability test device |
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