CN116462508A - Preparation method of high-conductivity graphite electrode - Google Patents
Preparation method of high-conductivity graphite electrode Download PDFInfo
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- CN116462508A CN116462508A CN202310290916.4A CN202310290916A CN116462508A CN 116462508 A CN116462508 A CN 116462508A CN 202310290916 A CN202310290916 A CN 202310290916A CN 116462508 A CN116462508 A CN 116462508A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000010439 graphite Substances 0.000 title claims abstract description 93
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 142
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 36
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 239000002006 petroleum coke Substances 0.000 claims abstract description 19
- 239000010426 asphalt Substances 0.000 claims abstract description 17
- 230000003111 delayed effect Effects 0.000 claims abstract description 16
- 238000009987 spinning Methods 0.000 claims abstract description 15
- 239000011258 core-shell material Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 63
- 238000005245 sintering Methods 0.000 claims description 53
- 238000001816 cooling Methods 0.000 claims description 51
- 238000007598 dipping method Methods 0.000 claims description 46
- 239000011230 binding agent Substances 0.000 claims description 44
- 239000000843 powder Substances 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 24
- 239000011280 coal tar Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 21
- 238000004898 kneading Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000011294 coal tar pitch Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 235000011837 pasties Nutrition 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 2
- 230000002618 waking effect Effects 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 16
- 238000007254 oxidation reaction Methods 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 12
- 238000005086 pumping Methods 0.000 description 9
- 238000007599 discharging Methods 0.000 description 8
- 238000005553 drilling Methods 0.000 description 6
- 238000000576 coating method Methods 0.000 description 3
- 239000011246 composite particle Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 2
- 239000011331 needle coke Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-conductivity graphite electrode, which adopts delayed petroleum coke as a main raw material, conductive carbon black and boron carbide as a first layer coating agent, adopts spinning asphalt as a second layer coating agent to form a three-layer core-shell structure, and adopts the process of briquetting and granulating to modify a material, change the microstructure of the material and improve the density, homogeneity, conductivity and oxidation resistance of the material. The composite forming density and the current density of the graphite electrode can be further improved, the conductivity and the oxidation resistance are improved, the energy consumption is reduced, the service life is prolonged, the crack resistance is good, and particularly the replacement times of the medium-sized and large-sized graphite electrode are reduced. The volume density of the prepared graphite electrode blank is less than 1.78g/cm 3 The resistivity is less than 4.2 mu omega-m, is suitable for graphite electrodes of various specifications and models, and solves the problems of the graphite electrodes in the prior artThe conductivity and the service life are limited by the characteristics of the raw materials, and the index is difficult to improve.
Description
Technical Field
The invention belongs to the technical field of graphite electrode preparation, and particularly relates to a preparation method of a high-conductivity graphite electrode.
Background
In industrial production, graphite electrodes are used as conductive materials in the metallurgical industry, heating furnaces, lithium batteries and other industries. For example, the high-temperature electric furnace conductive electrode is characterized in that electric energy is input into the electric furnace through a graphite electrode, and the high temperature generated by arc initiation between the electrode end and the furnace burden is used as a heat source, so that the purpose of heating the furnace burden is achieved. However, with the continuous improvement of the technical level of industry, the scale of various electric furnace heating furnaces is continuously enlarged, and the high requirement for reducing energy consumption is also continuously put forward higher performance requirements on the specification and the electric conductivity of graphite electrodes in industry.
At present, graphite electrodes are generally produced by adopting petroleum coke powder as a main material and using asphalt powder for bonding and through the technological processes of kneading, forming, roasting, dipping, graphitizing, machining and the like, and the preparation process is relatively mature. This results in a graphite electrode having a greater restriction on the conductivity properties of the raw materials and the mature process, and a less breakthrough in performance improvement, especially for larger graphite electrodes. For example, patent CN110615680a discloses a graphite electrode with ultra-large specification of GHP phi 960-phi 1420mm and a production method thereof, which adopts needle coke raw material extrusion molding, prepares a hollow electrode by water-cooling drilling, improves electrical conductivity and thermal conductivity and reduces thermal expansion performance by high-quality needle coke raw material extrusion molding, and is suitable for the graphite electrode with ultra-large specification. However, the conductivity of the electrode is limited by the characteristics of needle petroleum coke raw materials, and the oxidation resistance service life of the large-sized electrode is also a problem to be considered, so that the replacement of the electrode needs to consume larger cost; therefore, it is still necessary to further improve the properties of graphite electrodes from the aspects of raw material compounding and process improvement.
Disclosure of Invention
Aiming at the problems that the existing graphite electrode prepared by taking various petroleum cokes as raw materials has performance limitation and the conductivity and oxidation resistance of the electrode are to be improved, the invention provides a preparation method of the high-conductivity graphite electrode. The specific technical scheme is as follows:
a preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 300-800 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 3 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of less than 6 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B (1.5-8), and then adding the adhesive C according to the mass ratio of the main material A to the adhesive C (0.5-2) to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 900-1000 ℃ to obtain carbonized blocks, naturally cooling, crushing the carbonized blocks into particles with the median granularity of 1-6 mm, and obtaining a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the coal tar=100 (10-25) (5-10) at 150-250 ℃, and then cooling to 90-100 ℃ for proofing paste for 20-40 min to obtain a paste material F;
s5: extruding the pasty material F to form an electrode green body, then carrying out primary sintering treatment on the electrode green body, wherein the sintering maximum temperature is 1200-1300 ℃, preserving heat for 24-48 h, and naturally cooling to obtain a carbonized electrode green body;
s6: placing the carbonized electrode blank into a high-pressure dipping tank, pumping negative pressure of 0.08-0.09 MPa, keeping the negative pressure for 1-2 h, then adding a dipping agent for dipping, pressurizing to 2.5-3 MPa, dipping at 200-250 ℃ for 2-3 h, and cooling to obtain the dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 1-5%;
s7: carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 2800-3200 ℃, preserving heat for 24-48 hours, and cooling to obtain a graphite electrode blank;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
In the step S5 of the technical scheme, drilling the electrode green body or the carbonized electrode green body to prepare a hollow electrode green body or a carbonized electrode green body; or the electrode green body or the carbonized electrode green body is not drilled, and a solid electrode green body or a solid carbonized electrode green body is prepared;
in the above technical scheme S5, the volume density of the electrode green compact is more than 1.75g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The resistivity of the carbonized electrode blank is less than 55 mu omega-m;
in the S7 of the technical scheme, the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m.
Compared with the prior art, the preparation method of the high-conductivity graphite electrode has the beneficial effects that:
1. according to the invention, the delayed petroleum coke is used as a main material, the particle size difference of the main material and the auxiliary material is designed, so that the conductive carbon black and the boron carbide are mixed and embedded on the surface of the delayed petroleum coke particles as a coating agent, the surface defect is overcome, and the conductivity and the oxidation resistance of the material can be improved.
2. The method of the invention utilizes the self-cohesiveness of the delayed petroleum coke after being heated to achieve the effect of particle binding and granulating, and assists a small amount of spinning asphalt, so that conductive carbon black and boron carbide can be firmly embedded on the surface and defect of the delayed petroleum coke particles, the particles after coating modification are divided into a delayed petroleum coke base layer, an auxiliary material layer and a spinning asphalt layer, the coating granulation performance of the spinning asphalt is better, sintering is carried out at 900-1000 ℃, crushing and granulating are carried out, the microscopic properties of material particles can be improved, the conductivity and oxidation resistance of composite particles are improved, and the stability and firmness of granulating are improved.
3. The granulating process can ensure the homogeneity of auxiliary materials, optimize the particle morphology, reduce the gaps generated by defects, make up the gaps by conductive carbon black, boron carbide and spinning asphalt, and can effectively improve the density of the material after compression. Compared with simple mixing, the method can save the consumption of conductive carbon black and boron carbide, and can achieve better conductive and antioxidation effects.
4. The method of the invention carries out composite modification on the material, can substantially improve the properties of the base material particles and achieve higher homogeneity, so that the subsequent dry mixing is not needed, and the wet mixing and kneading are directly carried out; only the modified material E, namely the solid particle material, is kneaded, so that the kneading quality is more uniform, and the phenomenon of non-uniformity in kneading and dispersion does not occur, so that layering or non-uniform agglomeration of heterogeneous particles does not occur even if coal tar is added; the addition of coal tar can improve the kneading effect, reduce the consumption of asphalt, has better conductivity, and is easier to extrude and form electrode green bodies with higher density; in addition, the composite particles are stable in material quality, and compared with a simple mixing process, the composite particles are better in crack resistance after being pressed.
5. According to the method, the electrode green body is carbonized at 1200-1300 ℃, so that the microscopic interlayer structure of the material can be well changed, and the conductivity is improved; then the mixture is placed in a high-pressure dipping tank for dipping, and the dipping agent is coal tar pitch melt liquid added with conductive carbon black and boron carbide, so that the conductivity and the oxidation resistance of the surface of the carbonized electrode blank can be improved.
6. The method of the invention carries out secondary sintering treatment on the carbonized electrode blank after impregnation, the sintering maximum temperature is 2800-3200 ℃, the microstructure of the material is further changed, graphitized materials are formed, and the conductivity is improved.
In conclusion, the method adopts the procedures of coating, bonding, briquetting and granulating, improves the homogeneity and density of materials, and the addition of auxiliary materials can also improve the contact conductivity between particles, improve the oxidation resistance of the particles, prolong the service life and have good crack resistance, in particular reduce the replacement times of medium-and-large-sized graphite electrodes. The volume density of the prepared graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega-m, is suitable for graphite electrodes of various specifications and models, and solves the problem that the technical indexes of the conductivity and the service life of the graphite electrode in the prior art are difficult to improve.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples and comparative examples were either commercially available from conventional sources or may be obtained by prior art methods unless specifically indicated. Unless otherwise indicated, assays or testing methods are routine in the art.
Example 1
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 326 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 2.5 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of below 3.2 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:1.5, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:0.5 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 900 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 2mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:20:8, at 160 ℃, and then cooling to 90 ℃ for 30min to wake up paste to obtain a pasty material F;
s5: extruding the paste F to form an electrode green compact with a volume density of 1.782g/cm 3 Drilling a hole to make the electrode green compact into a hollow, then performing primary sintering treatment on the electrode green compact, wherein the sintering maximum temperature is 1250 ℃, preserving heat for 26 hours, and naturally cooling to obtain a carbonized electrode blank, wherein the resistivity of the carbonized electrode blank is 52 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.08MPa, keeping the negative pressure for 1h, adding a dipping agent for dipping, pressurizing to 2.5MPa, dipping at 200 ℃ for 2h, and discharging from the tank and cooling to obtain a dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 3%;
s7: carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering maximum temperature is 3000 ℃, preserving heat for 24 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 2
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: pulverizing delayed petroleum coke into particles with a median particle diameter of 430 μm to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 1.5 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of below 2.3 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:2.5, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:0.6 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 900 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 1mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:25:5 at 180 ℃, and then cooling to 100 ℃ for carrying out paste proofing for 40min to obtain a paste material F;
s5: extruding the paste F to form an electrode green compact with a volume density of 1.76g/cm 3 Then sintering the electrode green body for one time, wherein the sintering maximum temperature is 1200 ℃, preserving heat for 30 hours, naturally cooling to obtain a carbonized electrode green body, drilling holes to prepare the carbonized electrode green body into a hollow body, and the resistivity of the carbonized electrode green body is 54 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.09MPa, keeping the negative pressure for 2 hours, adding a dipping agent for dipping, pressurizing to 3MPa, dipping at 250 ℃ for 2.5 hours, and discharging from the tank for cooling to obtain a dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 2.5 percent;
s7: performing secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 2800 ℃, preserving heat for 26 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 3
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 537 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 1 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of less than 1.5 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:5.5, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:1.2 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 950 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 4mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:10:10, at 200 ℃, and then cooling to 95 ℃ for carrying out paste proofing for 35min to obtain a paste material F;
s5: extruding the paste F to form an electrode green body, wherein the volume density of the electrode green body is more than 1.775g/cm 3 Then sintering the electrode green body for one time, wherein the sintering maximum temperature is 1300 ℃, preserving heat for 32 hours, and naturally cooling to obtain a carbonized electrode green body, wherein the resistivity of the carbonized electrode green body is 53 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.08MPa, keeping the negative pressure for 1.5 hours, adding a dipping agent for dipping, pressurizing to 2.8MPa, dipping at 230 ℃ for 3 hours, and discharging from the tank and cooling to obtain a dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 4%;
s7: carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 3200 ℃, preserving heat for 28 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 4
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: pulverizing delayed petroleum coke into particles with median particle diameter of 673 μm to obtain main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 0.8 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of less than 1.2 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:6, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:1.4 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 900 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 4.5mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:15:8 at 150 ℃, and then cooling to 90 ℃ for 25min to wake up paste to obtain a pasty material F;
s5: paste F is subjected toExtruding to form electrode green compact with volume density of 1.762g/cm 3 Then sintering the electrode green body for one time, wherein the sintering maximum temperature is 1250 ℃, the heat preservation is carried out for 40 hours, and the carbonized electrode green body is obtained after natural cooling, and the resistivity of the carbonized electrode green body is 51 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.08MPa, keeping the negative pressure for 2 hours, adding a dipping agent for dipping, pressurizing to 2.6MPa, dipping at 220 ℃ for 2 hours, and discharging from the tank and cooling to obtain the dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 1 percent;
s7: carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 3100 ℃, preserving heat for 40 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 5
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 750 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 0.6 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of less than 1.6 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:7, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:1.8 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 950 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 3.5mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:18:10, at the temperature of 250 ℃, and then cooling to the temperature of 95 ℃ for 20min to prepare paste material F;
s5: extruding the paste F to form an electrode green compact with a volume density of 1.765g/cm 3 Drilling a hole to make the electrode green body into a hollow, then performing primary sintering treatment on the electrode green body, wherein the sintering maximum temperature is 1250 ℃, preserving heat for 45 hours, and naturally cooling to obtain a carbonized electrode blank, wherein the resistivity of the carbonized electrode blank is 50 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.09MPa, keeping the negative pressure for 1h, then adding a dipping agent for dipping, pressurizing to 2.8MPa, dipping at 200 ℃ for 2h, and discharging from the tank and cooling to obtain a dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 3.5 percent;
s7: performing secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 2800 ℃, preserving heat for 48 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 6
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 386 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 3 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of less than 6 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:4, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:1 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 900 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 5mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:22:6 at 240 ℃, and then cooling to 100 ℃ for proofing for 40min to obtain a pasty material F;
s5: extruding the paste F to form an electrode green compact with a volume density of 1.763g/cm 3 Then sintering the electrode green body for one time, wherein the sintering maximum temperature is 1300 ℃, preserving heat for 24 hours, naturally cooling to obtain a carbonized electrode green body, drilling holes to prepare the carbonized electrode green body into a hollow body, and the resistivity of the carbonized electrode green body is 53 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.09MPa, keeping the negative pressure for 1.5 hours, adding a dipping agent for dipping, pressurizing to 2.6MPa, dipping at 240 ℃ for 3 hours, and discharging from the tank and cooling to obtain a dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 1.5 percent;
s7: carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 2850 ℃, preserving heat for 46h, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 7
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 300 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 2.4 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of below 4.2 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:3.5, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:0.8 to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 950 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 2.5mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:21:5 at 190 ℃, and then cooling to 95 ℃ for carrying out paste proofing for 30min to obtain a paste material F;
s5: extruding the paste F to form an electrode green compact with a volume density of 1.781g/cm 3 Then sintering the electrode green body for one time, wherein the sintering maximum temperature is 1200 ℃, preserving heat for 48 hours, and naturally cooling to obtain a carbonized electrode green body, wherein the resistivity of the carbonized electrode green body is 54 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.09MPa, keeping the negative pressure for 2 hours, adding a dipping agent for dipping, pressurizing to 2.5MPa, dipping at 250 ℃ for 2.5 hours, and discharging from the tank and cooling to obtain the dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 1.8 percent;
s7: performing secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering maximum temperature is 2950 ℃, preserving heat for 36 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
Example 8
A preparation method of a high-conductivity graphite electrode comprises the following steps:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 800 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 1.2 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of below 2.8 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B=100:8, and then adding the binder C according to the mass ratio of the main material A to the binder C=100:2, and continuously uniformly mixing to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 1000 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks into particles with the granularity of 6mm to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the binder C, namely coal tar=100:18:6 at 180 ℃, and then cooling to 95 ℃ for carrying out paste proofing for 35min to obtain a pasty material F;
s5: extruding the paste F to form an electrode green compact with a volume density of 1.768g/cm 3 Then sintering the electrode green body for one time, wherein the sintering maximum temperature is 1250 ℃, preserving heat for 35 hours, and naturally cooling to obtain a carbonized electrode green body, wherein the resistivity of the carbonized electrode green body is 52 mu omega m;
s6: placing the carbonized electrode blank in a high-pressure dipping tank, pumping negative pressure of 0.09MPa, keeping the negative pressure for 1.5 hours, adding a dipping agent for dipping, pressurizing to 2.8MPa, dipping at 210 ℃ for 2 hours, and discharging from the tank and cooling to obtain a dipped carbonized electrode blank;
the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 2.6 percent;
s7: carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 3100 ℃, preserving heat for 30 hours, and cooling to obtain a graphite electrode blank, and the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m;
s8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
The graphite electrode of the embodiment has high density and volume density of 1.78g/cm 3 The above material has good crack resistance, uniform quality, good conductivity and resistivity below 4.2 mu omega-m; and has good oxidation resistance and long service life.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-conductivity graphite electrode is characterized by comprising the following steps of:
s1: crushing the delayed petroleum coke into particles with the median particle diameter of 300-800 mu m to prepare a main material A; respectively crushing conductive carbon black and boron carbide into powder with the median particle diameter of less than 3 mu m, and then uniformly mixing the two powder by air flow to prepare an auxiliary material B; crushing the spinning asphalt into powder with the median particle diameter of less than 6 mu m to prepare a binder C;
s2: uniformly mixing the main material A and the auxiliary material B according to the mass ratio of the main material A to the auxiliary material B (1.5-8), and then adding the adhesive C according to the mass ratio of the main material A to the adhesive C (0.5-2) to continuously uniformly mix to obtain a composite material D with a three-layer core-shell structure;
s3: briquetting the composite material D, sintering at 900-1000 ℃ to obtain carbonized blocks, naturally cooling, and crushing the carbonized blocks to obtain a granulated modified material E;
s4: uniformly kneading the modified material E, the molten liquid of the binder C and the coal tar according to the mass ratio of the modified material E to the coal tar=100 (10-25) to the coal tar (5-10) at 150-250 ℃, and then cooling to 90-100 ℃ for proofing paste to obtain a paste material F;
s5: extruding the pasty material F to form an electrode green body, then carrying out primary sintering treatment on the electrode green body, wherein the sintering maximum temperature is 1200-1300 ℃, preserving heat for 24-48 h, and naturally cooling to obtain a carbonized electrode green body;
s6: placing the carbonized electrode blank into a high-pressure dipping tank, adding a dipping agent for dipping, and cooling the carbonized electrode blank after dipping;
s7: and (3) carrying out secondary sintering treatment on the impregnated carbonized electrode blank, wherein the sintering highest temperature is 2800-3200 ℃, preserving heat for 24-48 hours, and cooling to obtain the graphite electrode blank.
2. The method for preparing a highly conductive graphite electrode according to claim 1, further comprising S8: and carrying out mechanical processing post-treatment on the graphite electrode blank to obtain the graphite electrode.
3. The method for preparing a highly conductive graphite electrode according to claim 1, wherein in S5, the electrode green body or carbonized electrode blank is drilled to prepare a hollow electrode green body or carbonized electrode blank; or the electrode green body or the carbonized electrode green body is not drilled, and a solid electrode green body or a carbonized electrode green body is prepared.
4. The method for producing a highly conductive graphite electrode according to claim 1, wherein in S3, the carbonized mass is pulverized into particles having a median particle size of 1 to 6 mm.
5. The method for preparing a highly conductive graphite electrode according to claim 1, wherein in S4, the time for waking up the paste is 20 to 40 minutes.
6. The method for preparing a highly conductive graphite electrode according to claim 1, wherein in S6, the carbonized electrode blank is placed in a high-pressure dipping tank, then negative pressure is applied for 0.08-0.09 MPa, the negative pressure is maintained for 1-2 hours, and then dipping agent is added.
7. The method for preparing a highly conductive graphite electrode according to claim 1, wherein in S6, the impregnation is performed under a pressure of 2.5 to 3MPa at 200 to 250 ℃ for 2 to 3 hours.
8. The preparation method of the high-conductivity graphite electrode according to claim 1, wherein in the step S6, the impregnant is coal tar pitch melt liquid added with conductive carbon black and boron carbide, and the addition mass percentage of the conductive carbon black and the boron carbide is 1-5%.
9. The method for preparing a highly conductive graphite electrode according to claim 1, wherein in S5, the volume density of the electrode green body is > 1.75g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The resistivity of the carbonized electrode blank is less than 55 mu omega-m.
10. The method for manufacturing a highly conductive graphite electrode as claimed in claim 1The preparation method is characterized in that in S7, the volume density of the graphite electrode blank is more than 1.78g/cm 3 The resistivity is less than 4.2 mu omega.m.
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