CN117263164A - Preparation method of large-block carbon electrode with controllable micro-channel size and morphology - Google Patents
Preparation method of large-block carbon electrode with controllable micro-channel size and morphology Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000002028 Biomass Substances 0.000 claims abstract description 18
- 239000007772 electrode material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 230000002457 bidirectional effect Effects 0.000 claims abstract description 10
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 230000000149 penetrating effect Effects 0.000 claims abstract description 7
- 238000010000 carbonizing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000003763 carbonization Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 5
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920005610 lignin Polymers 0.000 claims description 3
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 2
- 241000723346 Cinnamomum camphora Species 0.000 claims description 2
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 claims description 2
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 claims description 2
- -1 butyraldehyde stearate Chemical compound 0.000 claims description 2
- 229930006739 camphene Natural products 0.000 claims description 2
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 claims description 2
- 229930008380 camphor Natural products 0.000 claims description 2
- 229960000846 camphor Drugs 0.000 claims description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims 1
- 238000012824 chemical production Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 7
- 235000017491 Bambusa tulda Nutrition 0.000 description 7
- 241001330002 Bambuseae Species 0.000 description 7
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 7
- 239000011425 bamboo Substances 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 5
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 4
- 235000011613 Pinus brutia Nutrition 0.000 description 4
- 241000018646 Pinus brutia Species 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000010902 straw Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention belongs to the technical field of preparation of electrode materials, and discloses a preparation method of a large carbon electrode with controllable micro-channel size and morphology, which comprises the following steps: firstly, delignifying biomass powder; then preparing a mixed suspension of biomass powder, a cross-linking agent and a solvent, and performing low-temperature treatment under different temperature gradients by using a controllable temperature refrigerating device so as to regulate and control the size of a micro-channel; simultaneously, a unidirectional, bidirectional or non-directional low-temperature treatment mode is carried out by utilizing a temperature-controllable refrigerating device so as to adjust the shape of the micro-channel; and finally carbonizing. The method can prepare the penetrating micro-channel carbon electrode with different apertures and micro-channel morphologies by adjusting preparation process parameters, is expected to be applied to various fields of chemical production, environmental protection and the like, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of carbon electrodes, and particularly relates to a preparation method of a large carbon electrode with controllable micro-channel size and morphology.
Background
Carbon materials are widely used in the fields of electrochemistry, adsorption, catalysis, etc. Common carbon materials include graphite, carbon felt, carbon nanotubes, activated carbon, biomass carbon, graphene, and the like. The carbon material has the advantages of stable chemical property, low cost, controllable morphology and the like. In electrochemical water treatment, however, powdered carbon is mainly mixed with a binder and then coated on a support to serve as a carbon electrode. However, a problem of carbon material falling off may occur in long-term operation, and the addition of the binder may affect the conductivity of the electrode material. Related patent (CN 108910859A) reports that a porous carbon material is prepared by taking a high molecular material as a precursor through a freeze-drying and high-temperature carbonization mode, but the pore canal of the carbon material prepared by the method is disordered, and the pore diameter and the pore canal morphology cannot be controlled. In addition, the existing pore-forming methods such as the ice template method are mostly used for preparing porous ceramics and high heat conduction composite materials, but are not applied to the field of large-scale carbon electrodes, and mainly the problems of poor electric conductivity and incapability of forming large-area electrodes are difficult to solve. Therefore, the carbon material is difficult to be industrially produced and practically utilized on a large scale.
Disclosure of Invention
The invention takes biomass powder material as raw material, and prepares the massive carbon electrode material with the through micron-sized channel by using a low-temperature freezing and high-temperature carbonization method. The carbon electrode materials with different pore diameters and pore appearances can be prepared by adjusting the content of solid powder, the low-temperature treatment temperature, the low-temperature treatment mode, the content of the cross-linking agent and the solvent composition. In actual production, biomass is an inexhaustible renewable resource in natural environment, and the preparation of the biomass as a carbon electrode material is the development and reuse of waste resources. Therefore, the large-block micro-channel carbon electrode prepared by the method has great potential in large-scale application.
The technical scheme of the invention is as follows:
a preparation method of a large carbon electrode with controllable micro-channel size and morphology comprises the following steps:
(1) Microchannel size and morphology adjustment: preparing suspension from biomass powder, a cross-linking agent and a solvent according to a certain proportion after lignin removal treatment, placing the treated suspension into a mould, performing unidirectional, bidirectional or unoriented low-temperature treatment under different temperature gradients by using a controllable temperature refrigerating device, and then drying and forming;
(2) Carbonizing the material: and (3) placing the dried and formed material in a high-temperature resistance furnace for carbonization treatment to obtain the micro-channel carbon electrode material with controllable size.
Preparing biomass powder subjected to lignin removal treatment in the step (1) and a cross-linking agent and a solvent into suspension, wherein the mass ratio of the biomass powder to the cross-linking agent to the solvent is 8-35%: 1-9%: 60-100%. Too much solid powder may result in the formation of channels and too little may result in too low mechanical strength of the material to be shaped.
The particle size of the biomass powder in the step (1) is 2-30 mu m. Too large particle size of the biomass powder can result in uncontrolled microchannel diameter and morphology, and too small particle size can result in carbonization which is difficult to shape.
The cross-linking agent in step (1) includes, but is not limited to, polyvinyl butyral (PVB), polyvinyl pyrrolidone (PVP), polyvinyl acid (PAA), glycerol.
Solvents in step (1) include, but are not limited to, camphor, camphene, dimethyl sulfoxide, t-butanol, water, formamide, and butyraldehyde stearate.
In the step (1), a controllable temperature refrigerating device is used for unidirectional, bidirectional or non-directional low-temperature treatment under different temperature gradients, and the temperature gradients and the treatment time procedures are as follows: for the penetrating micro-channel with the diameter of 70-200 mu m, firstly, the micro-channel is treated for 5-60 min at the low temperature of minus 10-minus 15 ℃ and then is treated for 5-60 min at the low temperature of minus 30-minus 35 ℃; for the penetrating micro-channel with the diameter of 20-80 mu m, firstly, treating for 5-60 min at the low temperature of minus 35-minus 40 ℃ and then treating for 5-60 min at the low temperature of minus 60-minus 65 ℃; for the penetrating micro-channel with the diameter of 4-30 mu m, the micro-channel is firstly treated for 5-60 min at the low temperature of minus 65-minus 70 ℃ and then treated for 5-60 min at the low temperature of minus 90-minus 95 ℃. The temperature gradient is a key factor causing the passage to penetrate, and changing the gradient cooling sequence can cause the passage to be closed and incapable of passing water.
In the step (1), a controllable temperature refrigerating device is used for unidirectional, bidirectional or non-directional low-temperature treatment under different temperature gradients, and the low-temperature treatment mode process comprises the following steps: when the low-temperature treatment mode is unidirectional, the shape of the micro-channel is that the aperture ratio of the two ends is 1.5:1 to 6:1, wherein the height range of the electrode is 5-35mm; when the low-temperature treatment mode is bidirectional, the shape of the micro-channel is a layered channel with the length of 0.1-70 mm, and the height range of the electrode is 5-70mm; when the low-temperature treatment mode is unoriented, the shape of the micro-channel is staggered.
In the step (2), under the vacuum condition that the vacuum degree is 1-100 Pa, heating is started at the heating rate of 8-10 ℃/min, and the temperature is kept for 0.5-2 h at the temperature of 200-400 ℃; then heating up at the heating rate of 4-5 ℃/min under the vacuum condition of 0.001-1 Pa, and preserving heat for 0.5-2 h at 400-600 ℃; finally, under the vacuum condition of 0.001-1 Pa, heating is started at the heating rate of 1-2 ℃/min, and the temperature is kept for 1-3 h at 600-900 ℃.
The invention has the beneficial effects that: the biomass powder material is used as a raw material, and the method of low-temperature freezing and high-temperature carbonization is used for preparing the massive carbon electrode material with the through micron-sized channels. The carbon electrode materials with different micro-channel diameters and morphologies can be prepared by adjusting the content of solid powder, the low-temperature treatment temperature, the low-temperature treatment mode, the content of the cross-linking agent and the solvent composition. The micro-channel structure limits the reaction process in the grid of the electrode, overcomes mutual repulsion of ions and the electrode under the action of electric field force, shortens the mass transfer distance, improves the reaction efficiency of the electrode and the utilization rate of active free radicals, and increases the effective reaction area of the electrode. The low-temperature freezing method has the advantages of simple preparation flow, low equipment requirement, low production cost, simple operation, easy regulation and control and easy realization of large-scale preparation and mass production. And the biomass is an inexhaustible renewable resource in the natural environment, and the preparation of the biomass as a carbon electrode material is the development and reuse of waste resources.
Drawings
FIG. 1 is a scanning electron microscope image of a microchannel carbon electrode prepared by unidirectional low temperature treatment.
FIG. 2 is a scanning electron microscope image of a microchannel carbon electrode prepared by a two-way low temperature treatment mode according to the invention.
FIG. 3 is a scanning electron microscope image of a microchannel carbon electrode prepared by the non-directional low temperature treatment method of the invention.
FIG. 4 is a scanning electron microscope image of a porous carbon electrode without microchannels.
Fig. 5 is a flow chart of the preparation of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples for further illustration of the invention, but they should not be construed as limiting the scope of the invention.
Example 1
(1) 60g of bamboo powder is weighed and placed in a 3mol/L NaOH aqueous solution, heated to boiling and kept for 5 hours, and after treatment, the bamboo powder is repeatedly washed by high-purity water until the bamboo powder is neutral. Then adding the washed bamboo powder and 5g of polyvinyl butyl ester into 200mL of dimethyl sulfoxide, and uniformly mixing to prepare a suspension.
(2) Pouring the treated suspension into a mould with the thickness of 170mm being 30mm, performing unidirectional low-temperature treatment by using a controllable temperature refrigerating device, performing low-temperature treatment for 50min at the temperature of minus 35 ℃ to minus 40 ℃, performing low-temperature treatment for 50min at the temperature of minus 60 ℃ to minus 65 ℃, and then drying and forming.
(3) Placing the dried green body in a carbonization furnace, wherein the carbonization furnace needs to reach a vacuum condition with the vacuum degree of 10Pa, heating up at the heating rate of 10 ℃/min, and preserving heat for 0.5h at 300 ℃; then heating at a heating rate of 5 ℃/min under a vacuum condition of 0.001Pa, and preserving heat for 2 hours at 600 ℃; finally, heating is started at a heating rate of 2 ℃/min under a vacuum condition of 0.001Pa, and the temperature is kept for 3 hours at 900 ℃, so that the green body can be completely carbonized, and the carbon electrode material with a micro-channel diameter of 20-80 mu m and a horn-shaped morphology is obtained, as shown in figure 1.
Example 2
(1) Weighing 60g of natural pine wood powder, placing in 5mol/L NaOH aqueous solution, heating to boil and maintaining for 8h, and repeatedly washing with high-purity water until the bamboo powder is neutral. Then adding the washed pine wood powder and 1g of polyvinyl acid into 200mL of water, and uniformly mixing to prepare a suspension.
(2) Pouring the treated suspension into a mould with the thickness of 170mm being 30mm, performing bidirectional low-temperature treatment by using a controllable temperature refrigerating device, performing low-temperature treatment for 30min at the temperature of minus 35 ℃ to minus 40 ℃, performing low-temperature treatment for 30min at the temperature of minus 60 ℃ to minus 65 ℃, and then drying and forming.
(3) Placing the dried green body in a carbonization furnace, wherein the carbonization furnace needs to reach a vacuum condition with the vacuum degree of 10Pa, heating up at the heating rate of 10 ℃/min, and preserving heat for 0.5h at 300 ℃; then heating at a heating rate of 5 ℃/min under a vacuum condition of 0.001Pa, and preserving heat for 2 hours at 600 ℃; finally, heating is started at a heating rate of 2 ℃/min under a vacuum condition of 0.001Pa, and the temperature is kept for 3 hours at 900 ℃, so that the green body can be completely carbonized, and the carbon electrode material with 20-80 mu m micro-channel diameter and lamellar morphology is obtained, as shown in figure 2.
Example 3
(1) 60g of straw powder is weighed and placed in 1.5mol/L NaOH aqueous solution, heated to boiling and kept for 3 hours, and after treatment, the straw powder is repeatedly washed by high-purity water until the bamboo powder is neutral. And then adding the washed straw powder and 2g of polyvinylpyrrolidone into 200mL of tertiary butanol, and uniformly mixing to prepare a suspension.
(2) Pouring the treated suspension into a mould with the thickness of 170mm being 30mm, carrying out non-directional low-temperature treatment by using a controllable temperature refrigerating device, carrying out low-temperature treatment for 20min at the temperature of minus 35 ℃ to minus 40 ℃, carrying out low-temperature treatment for 20min at the temperature of minus 60 ℃ to minus 65 ℃, and then drying and forming.
(3) Placing the dried green body in a carbonization furnace, wherein the carbonization furnace needs to reach a vacuum condition with the vacuum degree of 10Pa, heating up at the heating rate of 10 ℃/min, and preserving heat for 0.5h at 300 ℃; then heating at a heating rate of 5 ℃/min under a vacuum condition of 0.001Pa, and preserving heat for 2 hours at 600 ℃; finally, heating is started at a heating rate of 2 ℃/min under a vacuum condition of 0.001Pa, and the temperature is kept for 3 hours at 900 ℃, so that the green body can be completely carbonized, and the carbon electrode material with the micro-channel diameter of 20-80 mu m and staggered morphology is obtained, as shown in figure 3.
Comparative example 1
(1) Weighing 80g of natural pine wood powder, placing in 5mol/L NaOH aqueous solution, heating to boil and keeping for 8 hours, and repeatedly washing with high-purity water until the bamboo powder is neutral. Then adding the washed pine wood powder and 1g of polyvinyl acid into 100mL of water, and uniformly mixing to prepare a suspension.
(2) Pouring the treated suspension into a mould with the thickness of 170mm being 30mm, performing unidirectional low-temperature treatment by using a controllable temperature refrigerating device, performing low-temperature treatment for 20min at the temperature of minus 35 ℃ to minus 40 ℃, performing low-temperature treatment for 20min at the temperature of minus 60 ℃ to minus 65 ℃, and then drying and forming.
(3) Placing the dried green body in a carbonization furnace, wherein the carbonization furnace needs to reach a vacuum condition with the vacuum degree of 10Pa, heating up at the heating rate of 10 ℃/min, and preserving heat for 0.5h at 300 ℃; then heating at a heating rate of 5 ℃/min under a vacuum condition of 0.001Pa, and preserving heat for 2 hours at 600 ℃; finally, heating is started at a heating rate of 2 ℃/min under a vacuum condition of 0.001Pa, and the temperature is kept at 900 ℃ for 3 hours, so that the green body can be completely carbonized, and the micro-channel-free porous carbon electrode material is obtained, as shown in fig. 4. Since the mass fraction of the biomass powder is 80% which is far greater than in the examples, the micro-channels of the carbon electrode material cannot be formed.
Claims (8)
1. A preparation method of a large carbon electrode with controllable micro-channel size and morphology is characterized by comprising the following steps:
(1) Microchannel size and morphology adjustment: preparing biomass powder into suspension with a cross-linking agent and a solvent according to a proportion after lignin removal treatment, placing the suspension into a die, performing unidirectional, bidirectional or unoriented low-temperature treatment on the die under different temperature gradients by using a controllable temperature refrigerating device, and then drying and forming;
(2) Carbonizing the material: and (3) placing the dried and formed material in a high-temperature resistance furnace for carbonization treatment to obtain the micro-channel carbon electrode material with controllable size.
2. The method for preparing a bulk carbon electrode according to claim 1, wherein in the step (1), the mass ratio of the biomass powder subjected to delignification treatment, the cross-linking agent and the solvent is 8-35%: 1-9%: 60-100%.
3. The method for producing a bulk carbon electrode according to claim 1, wherein in the step (1), the biomass powder has a particle size of 2 to 30. Mu.m.
4. The method for producing a bulk carbon electrode according to claim 1, wherein in the step (1), the crosslinking agent comprises polyvinyl butyl ester, polyvinyl pyrrolidone, polyvinyl acid, glycerin.
5. The method for producing a bulk carbon electrode according to claim 1, wherein in the step (1), the solvent comprises camphor, camphene, dimethyl sulfoxide, t-butanol, water, formamide, and butyraldehyde stearate.
6. The method for preparing a bulk carbon electrode according to claim 1, wherein in the step (1), the mold is subjected to unidirectional, bidirectional or non-directional low-temperature treatment under different temperature gradients by using a temperature-controllable refrigerating device, and the temperature gradient and the treatment time are as follows: for the penetrating micro-channel with the diameter of 70-200 mu m, firstly, the micro-channel is treated for 5-60 min at the low temperature of minus 10-minus 15 ℃ and then is treated for 5-60 min at the low temperature of minus 30-minus 35 ℃; for the penetrating micro-channel with the diameter of 20-80 mu m, firstly, treating for 5-60 min at the low temperature of minus 35-minus 40 ℃ and then treating for 5-60 min at the low temperature of minus 60-minus 65 ℃; for the penetrating micro-channel with the diameter of 4-30 mu m, the micro-channel is firstly treated for 5-60 min at the low temperature of minus 65-minus 70 ℃ and then treated for 5-60 min at the low temperature of minus 90-minus 95 ℃.
7. The method for preparing a bulk carbon electrode according to claim 1, wherein in the step (1), the mold is subjected to unidirectional, bidirectional or non-directional low-temperature treatment under different temperature gradients by using a controllable temperature refrigerating device, and the low-temperature treatment process is as follows: when the low-temperature treatment mode is unidirectional, the shape of the micro-channel is that the aperture ratio of the two ends is 1.5:1 to 6:1, wherein the height range of the micro-channel carbon electrode is 5-35mm; when the low-temperature treatment mode is bidirectional, the shape of the micro-channel carbon electrode is a layered channel with the length of 0.1-70 mm, and the height range of the micro-channel carbon electrode is 5-70mm; when the low-temperature treatment mode is unoriented, the shape of the micro-channel in the micro-channel carbon electrode is staggered.
8. The method for producing a bulk carbon electrode according to claim 1, wherein in the step (2), the carbonization treatment is performed under a vacuum condition of a vacuum degree of 1 to 100Pa, the temperature is raised at a temperature raising rate of 8 to 10 ℃/min, and the temperature is kept at 200 to 400 ℃ for 0.5 to 2 hours; then heating up at the heating rate of 4-5 ℃/min under the vacuum condition of 0.001-1 Pa, and preserving heat for 0.5-2 h at 400-600 ℃; finally, under the vacuum condition of 0.001-1 Pa, heating is started at the heating rate of 1-2 ℃/min, and the temperature is kept for 1-3 h at 600-900 ℃.
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