CN107638853A - Electrochemical reaction appts and preparation method thereof - Google Patents
Electrochemical reaction appts and preparation method thereof Download PDFInfo
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- CN107638853A CN107638853A CN201710797546.8A CN201710797546A CN107638853A CN 107638853 A CN107638853 A CN 107638853A CN 201710797546 A CN201710797546 A CN 201710797546A CN 107638853 A CN107638853 A CN 107638853A
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- reaction kettle
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Abstract
The invention discloses a kind of electrochemical reaction appts and preparation method thereof, including the reaction kettle cover that reaction kettle body matches with reaction kettle body, it is characterised in that：The reaction kettle body is made of superhigh temperature ceramic material, and above embedded with three graphite electrodes and three heating element heaters, the graphite electrode is located at reaction kettle body isometry position with heating element heater, and is alternately uniformly distributed on the circumference of reaction kettle body isometry position.The electrochemical reaction appts that the present invention designs pass through external heating power supply and temperature indicating device, it is possible to achieve room temperature is applied to the arbitrary temp setting in 1400 degree Celsius ranges suitable for high-temperature electrochemistry research.
Description
Technical field
The present invention relates to high-temperature solid electrochemical reaction appts and preparation method thereof.
Background technology
Solid-state electrochemistry subject is an emerging cross discipline, is a branch of electrochemistry, and research object is mainly
The mixed conductor of solid ionic conductor and ion and electronics, research contents are mainly electrochemical reaction process and its phase in solid
Close material structure-activity relationship.Recently as going deep into for research, the research of the temperature effect in solid-state electrochemistry gradually causes people
Concern.But current general electrochemical reaction appts are usually normal temperature solution system, can not study more than 100 degrees Celsius of height
Warm electrochemical behavior, for the relevant nature of researching high-temperature solid-state electrochemistry, we specially devise a high-temperature solid electrification
Learn reaction unit and preparation method thereof.
The content of the invention
For current electrochemical reaction appts can not resistant to elevated temperatures problem, the invention provides a kind of electrochemical reaction dress
Put.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of electrochemical reaction appts, including reaction kettle body
The 1 reaction kettle cover 2 matched with reaction kettle body 1, the reaction kettle body 1 is made of superhigh temperature ceramic material, above embedded with three slabstones
Electrode ink 3 and three heating element heaters 4, the graphite electrode 3 is located at the isometry position of reaction kettle body 1 with heating element heater 4, and is reacting
Alternately it is uniformly distributed on the circumference of the isometry position of kettle 1, reaction kettle cover 2 center, which has, hangs down into graphite electrode 3 and heating
The temp probe 5 at the center of element 4, the heating element heater 4 are the Fe-based perovskite-like oxide of ceramic package, and the temp probe 5 is
Platinum rhodium thermocouple.
The invention also discloses the preparation method of above-mentioned electrochemical reaction appts, its step includes：
A, reaction kettle body base and reaction kettle cover base are made using superhigh temperature ceramic material, 6 is reserved on reaction kettle body base
Empty window is embedded in for graphite electrode and heating element heater；
B, reaction kettle body base is fired with reacting kettle cover base into ceramic reactor body and reaction kettle cover；
C, graphite electrode raw material is calcined in the case where completely cutting off air conditionses, then crushed；
D, the fragment for choosing suitable diameter adds other materials to be made into thickener；
E, after thickener precompressed, thickener is inserted into sky window position, reaction kettle body is put into press, makes the thickener inserted in sky window
It is compressing；
F, by protection medium of the reaction kettle body after die mould in heating furnace, roasted under conditions of air is completely cut off
Burn；
G, the reaction kettle body after roasting is put into graphitizing furnace and carries out graphitization；
H, heating element heater is embedded in；
I, in the reaction centre-drilling hole of kettle cover 2, and temp probe 5 is fixed under hole vertically.
Wherein the manufactured reaction kettle body fire damage temperature of superhigh temperature ceramic material than graphite electrode graphitization temperature extremely
It is few high 200 DEG C.Further, control thickener inserts the amount of sky window position so that the graphite electrode inner surface after compacting is higher than anti-
Kettle inner surface is answered, graphite electrode outer surface is higher than reaction kettle body outer surface, to add after graphitization in graphite electrode outer surface
Work goes out electric wire connection button.
Beneficial effects of the present invention：The electrochemical reaction appts that the present invention designs pass through external heating power supply and temperature display
Device, it is possible to achieve room temperature is applied to the arbitrary temp setting in 1400 degree Celsius ranges suitable for high-temperature electrochemistry research.Stone
Electrode ink is located at reaction kettle body isometry position and replaced on the circumference of reaction kettle body isometry position with heating element heater to be uniformly distributed,
Not only so that reaction kettle body is heated evenly, and cause three electrodes of electrochemistry to be in mutual equivalent position, avoid temperature
Influence of the factor such as distribution gradient or disturbance to electrode measurement, be advantageous to improve the accuracy of measurement.In addition, temp probe is straight
Connect and make it that measured temperature is more accurate positioned at the center of graphite electrode and heating element heater, also reduce further temp probe
Influence to electrode measurement.
Brief description of the drawings
Fig. 1 is the structural representation of the electrochemical reaction appts of the present invention.
Fig. 2 is the profile of the electrochemical reaction appts of the present invention.
Embodiments of the present invention are described further below in conjunction with the accompanying drawings.
Embodiment
Embodiment 1
This electrochemical reaction appts, including the reaction kettle cover 2 that reaction kettle body 1 matches with reaction kettle body 1, the reaction kettle body
1 is made of zirconium carbide superhigh temperature ceramic material with reaction kettle cover 2, above embedded with three graphite electrodes 3 and three heating element heaters 4,
The graphite electrode 3 is located at the isometry position of reaction kettle body 1 with heating element heater 4, and is submitted in the circumference of the isometry position of reaction kettle body 1
For being uniformly distributed, there is individual hang down into the temp probe to graphite electrode 3 and three centers of heating element heater 4 in reaction kettle cover 2 center
5, the heating element heater 4 is the Fe-based perovskite-like oxide of ceramic package, and the temp probe 5 is platinum rhodium thermocouple.Wherein it is carbonized
Reaction kettle body fire damage temperature is at 3200 DEG C or so made of zirconium ultrahigh temperature ceramic material.
Embodiment 2
This electrochemical reaction appts, including the reaction kettle cover 2 that reaction kettle body 1 matches with reaction kettle body 1, the reaction kettle body
1 is made of titanium carbide superhigh temperature ceramic material with reaction kettle cover 2, above embedded with three graphite electrodes 3 and three heating element heaters 4,
The graphite electrode 3 is located at the isometry position of reaction kettle body 1 with heating element heater 4, and is submitted in the circumference of the isometry position of reaction kettle body 1
For being uniformly distributed, there is individual hang down into the temp probe to graphite electrode 3 and three centers of heating element heater 4 in reaction kettle cover 2 center
5, the heating element heater 4 is the Fe-based perovskite-like oxide of ceramic package, and the temp probe 5 is platinum rhodium thermocouple.Wherein it is carbonized
Reaction kettle body fire damage temperature is at 3000 DEG C or so made of titanium superhigh temperature ceramic material.
Embodiment 3
The preparation method of the electrochemical reaction appts of embodiment 1, its step include：
A, reaction kettle body base and reaction kettle cover base are made using superhigh temperature ceramic material zirconium carbide, it is pre- on reaction kettle body base
6 empty windows are stayed to be embedded in for graphite electrode and heating element heater；
B, under the conditions of vacuum atmosphere, 1650 DEG C, pressure are 20MPa, 1.5 hours are incubated, fire reaction kettle body base with it is anti-
Kettle cover base is answered into ceramic reactor body and reaction kettle cover；
C, using petroleum coke, needle coke and coal tar pitch as graphite electrode raw material, the ratio of selection is：Petroleum coke 50%, needle-like
Jiao 40%, coal tar pitch 10%, in the case where completely cutting off air conditionses, 1400 DEG C of calcinings, are then crushed；
D, choose the fragment that particle size range is 0.3~1.0mm and 1.0~1.5mm to be mixed in 1: 3 ratio, do
The binding agent medium temperature modified coal tar pitch for accounting for siccative gross weight 25% is added after mixed 30 minutes, then thickener is made in 40 minutes in kneading, is going out paste
Add within first 8 minutes the additive stearic acid of siccative gross weight 0.4%；
E, by thickener in cooler it is cool to 110 DEG C, then precompressed 5 minutes in extruder are put into after being incubated 20 minutes, will pasted
Material inserts sky window position, and reaction kettle body is put into press, 125 DEG C, pressure 35Mpa of temperature, and the thickener for making to insert in sky window is suppressed
Shaping；
F, by protection medium of the reaction kettle body after die mould in heating furnace, roasted under conditions of air is completely cut off
Burn, parameter：400 DEG C first are warming up to by 70 DEG C/h speed, is kept for 6 minutes；Then 800 are warming up to according to 40 DEG C/h speed
DEG C, it is incubated 16 minutes；1200 degrees Celsius are warming up to according still further to 70 DEG C/h speed, is incubated 30 minutes；
G, the reaction kettle body after roasting is put into graphitizing furnace and carries out graphitization, graphitization temperature is 2800 DEG C；
H, heating element heater is embedded in；
I, in the reaction centre-drilling hole of kettle cover 2, and temp probe 5 is fixed under hole vertically.
Claims (4)
1. a kind of electrochemical reaction appts, including the reaction kettle cover that reaction kettle body matches with reaction kettle body, it is characterised in that：It is described
Reaction kettle body is made of superhigh temperature ceramic material, above embedded with three graphite electrodes and three heating element heaters, the graphite electrode
It is located at the isometry position of reaction kettle body with heating element heater, and is alternately uniformly distributed on the circumference of reaction kettle body isometry position, institute
State reaction kettle cover center and be provided with the temp probe to hang down into graphite electrode and heating element heater center, the heating element heater seals for ceramics
The Fe-based perovskite-like oxide of dress, the temp probe are platinum rhodium thermocouple.
2. the preparation method of the electrochemical reaction appts described in claim 1, its step includes：
A, reaction kettle body base and reaction kettle cover base are made using superhigh temperature ceramic material, 6 empty windows is reserved on reaction kettle body base
So that graphite electrode and heating element heater are embedded in；
B, reaction kettle body base is fired with reacting kettle cover base into ceramic reactor body and reaction kettle cover；
C, graphite electrode raw material is calcined in the case where completely cutting off air conditionses, then crushed；
D, the fragment for choosing suitable diameter adds other materials to be made into thickener；
E, after thickener precompressed, thickener is inserted into sky window position, reaction kettle body is put into press, and the thickener for making to insert in sky window is suppressed
Shaping；
F, by protection medium of the reaction kettle body after die mould in heating furnace, it is calcined under conditions of air is completely cut off；
G, the reaction kettle body after roasting is put into graphitizing furnace and carries out graphitization；
H, heating element heater is embedded in；
I, in the reaction centre-drilling hole of kettle cover 2, and temp probe 5 is fixed under hole vertically.
3. the preparation method of electrochemical reaction appts according to claim 2, it is characterised in that：Wherein superhigh temperature ceramics material
The manufactured reaction kettle body fire damage temperature of material is at least higher 200 DEG C than the graphitization temperature of graphite electrode.
4. the preparation method of electrochemical reaction appts according to claim 2, it is characterised in that：Control thickener inserts sky window
The amount of position so that the graphite electrode inner surface after compacting is higher than reaction kettle body inner surface, and graphite electrode outer surface is higher than reaction
Kettle outer surface, to process electric wire connection button in graphite electrode outer surface after graphitization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710797546.8A CN107638853A (en) | 2017-09-06 | 2017-09-06 | Electrochemical reaction appts and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710797546.8A CN107638853A (en) | 2017-09-06 | 2017-09-06 | Electrochemical reaction appts and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060429A (en) * | 1991-10-28 | 1992-04-22 | 郑军 | The hollow graphite electrode Processes and apparatus is produced in vibratory compaction |
| CN103585942B (en) * | 2013-11-12 | 2015-12-16 | 厦门福纳新材料科技有限公司 | Arc process fullerene High-efficient Production device |
| CN205821422U (en) * | 2016-07-08 | 2016-12-21 | 大余县东宏锡制品有限公司 | High-efficiency environment friendly refines high-purity tin device |
| CN107081119A (en) * | 2017-04-01 | 2017-08-22 | 航天神洁（北京）环保科技有限公司 | A kind of reactor of heat plasma volume array Coal Pyrolysis acetylene |
-
2017
- 2017-09-06 CN CN201710797546.8A patent/CN107638853A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060429A (en) * | 1991-10-28 | 1992-04-22 | 郑军 | The hollow graphite electrode Processes and apparatus is produced in vibratory compaction |
| CN103585942B (en) * | 2013-11-12 | 2015-12-16 | 厦门福纳新材料科技有限公司 | Arc process fullerene High-efficient Production device |
| CN205821422U (en) * | 2016-07-08 | 2016-12-21 | 大余县东宏锡制品有限公司 | High-efficiency environment friendly refines high-purity tin device |
| CN107081119A (en) * | 2017-04-01 | 2017-08-22 | 航天神洁（北京）环保科技有限公司 | A kind of reactor of heat plasma volume array Coal Pyrolysis acetylene |
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Application publication date: 20180130 |