WO2024082709A1 - 一种高强度石墨电极的制备方法 - Google Patents
一种高强度石墨电极的制备方法 Download PDFInfo
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- WO2024082709A1 WO2024082709A1 PCT/CN2023/104422 CN2023104422W WO2024082709A1 WO 2024082709 A1 WO2024082709 A1 WO 2024082709A1 CN 2023104422 W CN2023104422 W CN 2023104422W WO 2024082709 A1 WO2024082709 A1 WO 2024082709A1
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- graphite electrode
- raw materials
- roasting
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 239000010439 graphite Substances 0.000 title claims abstract description 99
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 48
- 238000001354 calcination Methods 0.000 claims abstract description 28
- 230000017525 heat dissipation Effects 0.000 claims abstract description 15
- 230000003064 anti-oxidating effect Effects 0.000 claims abstract description 14
- 238000004898 kneading Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 41
- 239000004615 ingredient Substances 0.000 claims description 31
- 239000003575 carbonaceous material Substances 0.000 claims description 24
- 238000001125 extrusion Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
- 239000011280 coal tar Substances 0.000 claims description 17
- 239000011331 needle coke Substances 0.000 claims description 17
- 239000002006 petroleum coke Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 13
- 238000000465 moulding Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 238000005470 impregnation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 6
- 239000010426 asphalt Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000011294 coal tar pitch Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000007580 dry-mixing Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 238000005087 graphitization Methods 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 2
- 239000002737 fuel gas Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract 4
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000003039 volatile agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012258 stirred mixture Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
- C04B2235/9684—Oxidation resistance
Definitions
- the invention relates to the technical field of graphite electrode preparation, in particular to a method for preparing a high-strength graphite electrode.
- Graphite electrodes are mainly made of petroleum coke and needle coke as raw materials, with coal tar as a binder, and are made through calcination, batching, kneading and other processing steps. Graphite electrodes are widely used in production and can be used as a conductive material.
- the publication number is CN114751747A, a graphite electrode and a preparation process thereof, the process comprising the following steps: S1: a first extruded bottom plate, a plurality of first disk bodies and a first extruded top plate are fixed to form a first graphite electrode; S2: a second extruded bottom plate, a plurality of second disk bodies, a reaming disk, a limiting disk and a second extruded top plate are fixed to form a second graphite electrode; S3: a conversion mechanism passes through the first graphite electrode and extends into the second graphite electrode to form a graphite electrode; a graphite electrode, comprising a first graphite electrode, a second graphite electrode and a conversion mechanism; the first graphite electrode comprises a first extruded bottom plate, a first disk body, a first extruded top plate, connecting pins I and II, and the second graphite electrode comprises a second extruded
- the publication number is CN209120506U, an arc furnace graphite electrode, including a graphite electrode unit, an electrode joint and an electrode end cap, wherein a through hole is arranged at the center of the graphite electrode unit, the graphite electrode units are combined to form a graphite electrode body, two adjacent graphite electrode units have through holes of different diameters, and the through holes in the existing arc furnace graphite electrode have the same upper and lower apertures for passing cooling gas to improve the service life of graphite.
- the arc furnace graphite electrode provided by the embodiment of the utility model increases the internal gas turbulence between different graphite electrode units by setting the diameter difference of the through holes in the graphite anode. Improve heat exchange efficiency and extend the overall service life of graphite electrodes.
- Such graphite electrodes have low strength and will have a large loss rate as the use time increases, thereby reducing the use effect of graphite electrodes;
- the object of the present invention is to provide a method for preparing a high-strength graphite electrode to solve the problem mentioned in the above background technology that the existing graphite electrodes have no anti-oxidation protection during use, which shortens the service life of the graphite electrodes, and the graphite electrodes themselves have low strength, and as the use time increases, a large loss rate will occur, thereby reducing the use effect of the graphite electrodes.
- a method for preparing a high-strength graphite electrode comprising:
- Step 1 Prepare the raw materials
- Step 2 First processing of raw materials
- Step 3 Second processing of raw materials
- crushed petroleum coke, needle coke and coal tar are ground and sieved after grinding to ensure the fineness of the raw materials;
- the raw materials are placed in a calcining furnace for heat treatment to discharge the contained moisture and volatile matter, and are cooled after calcination;
- the kneaded mixture is placed in a molding device, and an external force is applied to cause plastic deformation to form a green body with a certain shape, size, density and strength, and the green body is cooled after being formed;
- the green body cooled to a certain temperature is charged and placed into a press, and then pre-pressed, extruded and sheared;
- the green body is placed in a heating furnace under the protection of fillers for high-temperature heat treatment to carbonize the coal tar pitch in the green body and improve the mechanical strength;
- Step 11 Graphitization
- the carbon products are heated in a protective medium in a high-temperature furnace to improve the electrical and thermal conductivity of the carbon materials.
- Step 12 Hole processing
- Heat dissipation holes are opened on the surface of the graphite electrode to improve the heat dissipation speed when the graphite electrode is used.
- An anti-oxidation coating is sprayed on the outer surface of the graphite electrode to slow down the oxidation of the graphite electrode.
- step 1 there are 50 parts of petroleum coke, 40 parts of needle coke, and 20 parts of coal tar, and the crusher in step 2 is a jaw crusher, and the particle size after crushing is 0.5-20 mm.
- the raw materials in step 3 are ground and then sieved, and the aperture range of the sieve is 0.075-0.15 mm.
- the calcium oxide in step 4 is 4 parts
- the ferric oxide is 0.75 parts
- the carbon fiber is 30 parts
- the batching crusher in step 5 is a jaw crusher
- the crushing particle size is 0.5-20mm
- the batching is screened after crushing, and the aperture of the screen is 0.075-0.15mm.
- the raw material calcining furnace in step 6 uses fuel gas and its own volatile matter as heat sources for calcination, and the calcination temperature is 1250-1350°C.
- the kneading process in step 7 is: dry mixing for 20-35 minutes and wet mixing for 40-55 minutes, so that the solid carbonaceous materials of different particle sizes are evenly mixed and the density of the mixture is improved.
- the forming method in step 8 is molding, and the equipment used is a vertical hydraulic press.
- the extrusion process in step 9 is cooling, charging, pre-pressing, and extrusion.
- the kneaded carbonaceous material is cooled to an appropriate temperature in the range of 90-120°C.
- the pre-pressing pressure is 20-25MPa, and the pre-pressing time is 3-5min, and vacuum is drawn before extrusion.
- the extrusion pressure is 5-15MPa.
- the roasting in step 10 is divided into two times, and the time of the first roasting is 22-30 days, the maximum roasting temperature is 1250°C, and the time of the second roasting is 5-10 days, the maximum roasting temperature range is 700-800°C, and the second roasting is roasting again after the roasted product is impregnated.
- the secondary roasting and impregnation process in step 10 is to first clean the surface of the roasted billet, then preheat it, the preheating temperature is 260-380°C, and the preheating time is 6-10h, then put the roasted billet into the impregnation tank, vacuum it, the vacuum pressure is 8-9KPa, the time is 40-50min, then inject asphalt, the temperature is 180-200°C, and then pressurize it again, the pressure is 1.2-1.5MPa, the time is 3-4h, and finally cool it.
- the hole-drilling process in step 12 is to drill holes on the surface of the graphite electrode by a hole-drilling machine, and the heat dissipation holes are evenly spaced on the surface of the graphite electrode.
- the filtering method in step 9 is to allow the stirred mixture to flow out from the discharge port of the reactor and filter it using a filter, and the pore size of the filter is 1-5 mm.
- the present invention has the following beneficial effects:
- the preparation method of the high-strength graphite electrode is divided into two calcinations during the calcination process of the graphite electrode, and the carbonaceous material is impregnated before the second calcination, so that the mechanical strength of the carbonaceous material can be improved by impregnation, thereby increasing the strength during use in the later use, and also improving the thermal stability and chemical stability, effectively reducing the loss rate, and improving the use effect of the graphite electrode;
- the preparation method of the high-strength graphite electrode is to coat the outer surface of the graphite electrode with an anti-oxidation layer and to open heat dissipation holes on the surface of the graphite electrode. This allows the graphite electrode to increase air circulation through the heat dissipation holes when used for a long time, thereby transferring the internal temperature to the outside, thereby accelerating the heat dissipation of the graphite electrode.
- the anti-oxidation layer can protect the graphite electrode, effectively slowing down the oxidation rate of the graphite electrode and extending the service life of the graphite electrode.
- This embodiment 1 provides a method for preparing a high-strength graphite electrode, and the method is described in detail below.
- the raw materials are prepared first, that is, 50 parts of petroleum coke, 40 parts of needle coke, and 20 parts of coal tar. Then the raw materials are processed for the first time, and large pieces of petroleum coke, needle coke and coal tar are put into a crusher for crushing to make the particles of petroleum coke, needle coke and coal tar smaller.
- the crusher is a jaw crusher with a crushing particle size of 0.5-20mm.
- the raw materials are ground for a second time, and sieved after grinding, wherein the aperture range of the screen is 0.075-0.15mm.
- the ingredients are prepared, that is, 4 parts of calcium oxide, 0.75 parts of ferric oxide, and 30 parts of carbon fiber are prepared.
- the ingredients are put into a jaw crusher with a crushing particle size of 0.5-20mm.
- the ingredients are sieved after crushing, and the aperture range of the screen is 0.075-0.15mm. In this way, the uniformity of the raw materials and the ingredients can be guaranteed.
- the raw materials are calcined, and the raw materials are placed in a calcining furnace for heat treatment to discharge the moisture and volatiles contained therein.
- the raw material calcining furnace uses gas and its own volatiles as heat sources for calcination, and the calcination temperature is 1250-1350°C.
- the raw materials are cooled, and then the cooled raw materials and the ingredients are poured into a kneading machine for mixing to obtain a mixture.
- the kneading process is: first dry mixing for 20-35 minutes, and then wet mixing for 40-55 minutes, so that the solid carbonaceous materials of different particle sizes are evenly mixed to improve the density of the mixture.
- the kneaded mixture is put into the molding equipment, and external force is applied to make it produce plastic deformation to form a green body with a certain shape, size, density and strength.
- the molding method is molding, and the equipment used is a vertical hydraulic press. Then it is extruded.
- the extrusion process is cooling, charging, pre-pressing, and extrusion.
- the kneaded carbonaceous material is cooled to a suitable temperature, and the temperature range is 90-120°C. When charging, the carbonaceous material at a suitable temperature is put into the press and compacted with 4-10MPa, and then pre-pressed.
- the pre-pressing pressure is 20-25MPa, and the pre-pressing time is 3-5min, and vacuum is drawn, and then extrusion is performed.
- the extrusion pressure is 5-15MPa. After extrusion, the green body is protected by the filler and loaded into a heating furnace for high-temperature heat treatment to carbonize the coal tar in the green body and improve the mechanical strength.
- the carbonaceous material is extruded, it is roasted, and the roasting is divided into two times, and the time of each roasting is 22-30 days, the highest roasting temperature is 1250°C, and the secondary roasting time is 5-10 days, the highest roasting temperature range is 700-800°C, and the secondary roasting is the roasting again after the roasting product is impregnated, wherein the impregnation process is to first clean the surface of the roasted blank, and then preheat it, the preheating temperature is 260-380°C, and the preheating time is 6-10h, then put the roasted blank into the impregnation tank, vacuumize it, the vacuum pressure is 8-9KPa, the time is 40-50min, then inject asphalt, the temperature is 180-200°C, and then pressurize it again, the pressure is 1.2-1.5MPa, the time is 3-4h, and finally cool it.
- the impregnation process is to first clean the surface of the roasted blank, and then preheat it, the
- graphitization treatment is carried out.
- the carbon product is heated to above 2300°C in a protective medium in a high-temperature furnace to treat the graphite crystalline structure at high temperature, thereby improving the electrical and thermal conductivity of the carbon material.
- the chemical stability of the carbon material can be improved, and the carbon material has lubricity and wear resistance.
- the surface of the obtained graphite electrode is perforated by a perforator, and the heat dissipation holes are evenly distributed on the surface of the graphite electrode, and an anti-oxidation coating is sprayed on the outer surface of the graphite electrode to slow down the oxidation of the graphite electrode. In this way, when the graphite electrode is used in the later stage, it not only improves its own structural strength, but also has the function of heat dissipation and anti-oxidation, thereby extending the service life of the graphite electrode.
- This embodiment 2 provides a method for preparing a high-strength graphite electrode, and the method is described in detail below.
- the raw materials are prepared first, that is, 60 parts of petroleum coke, 50 parts of needle coke, and 30 parts of coal tar. Then the raw materials are processed for the first time, and large pieces of petroleum coke, needle coke and coal tar are put into a crusher for crushing to make the particles of petroleum coke, needle coke and coal tar smaller.
- the crusher is a jaw crusher with a crushing particle size of 0.5-20mm.
- the raw materials are ground for a second time, and screened after grinding, wherein the aperture range of the screen is 0.075-0.15mm.
- the ingredients are prepared, that is, 5 parts of calcium oxide, 1 part of ferric oxide, and 20 parts of carbon fiber are prepared.
- the ingredients are put into a jaw crusher with a crushing particle size of 0.5-20mm.
- the ingredients are screened after crushing, and the aperture range of the screen is 0.075-0.15mm. In this way, the uniformity of the raw materials and the ingredients can be guaranteed.
- the raw materials are calcined, and the raw materials are placed in a calcining furnace for heat treatment to discharge the moisture and volatiles contained therein.
- the raw material calcining furnace uses gas and its own volatiles as heat sources for calcination, and the calcination temperature is 1250-1350°C.
- the raw materials are cooled, and then the cooled raw materials and the ingredients are poured into a kneading machine for mixing to obtain a mixture.
- the kneading process is: first dry mixing for 20-35 minutes, and then wet mixing for 40-55 minutes, so that the solid carbonaceous materials of different particle sizes are evenly mixed to improve the density of the mixture.
- the kneaded mixture is put into the molding equipment, and external force is applied to make it produce plastic deformation to form a green body with a certain shape, size, density and strength.
- the molding method is molding, and the equipment used is a vertical hydraulic press. Then it is extruded.
- the extrusion process is cooling, charging, pre-pressing, and extrusion.
- the kneaded carbonaceous material is cooled to a suitable temperature, and the temperature range is 90-120°C. When charging, the carbonaceous material at a suitable temperature is put into the press and compacted with 4-10MPa, and then pre-pressed.
- the pre-pressing pressure is 20-25MPa, and the pre-pressing time is 3-5min, and vacuum is drawn, and then extrusion is performed.
- the extrusion pressure is 5-15MPa. After extrusion, the green body is protected by the filler and loaded into a heating furnace for high-temperature heat treatment to carbonize the coal tar in the green body and improve the mechanical strength.
- the carbonaceous material After the carbonaceous material is extruded, it is roasted, and the roasting is divided into two times.
- the time of the first roasting is 22-30 days, and the maximum roasting temperature is 1250°C.
- the time of the second roasting is 5-10 days, and the maximum roasting temperature range is 700-800°C.
- the second roasting is roasting again after the roasted product is impregnated.
- the impregnation process is to first clean the surface of the roasted blank, and then preheat it.
- the preheating temperature is 260-380°C, and the preheating time is 6-10h. Then the roasted blank is put into the impregnation tank for vacuum treatment.
- the vacuum pressure is 8- 9KPa, time is 40-50min, then asphalt is injected, the temperature is 180-200°C, and then pressurized again, the pressure is 1.2-1.5MPa, the time is 3-4h, and finally cooled. After impregnation cooling, graphitization treatment is carried out.
- the carbon product is heated to above 2300°C in the protective medium in the high-temperature furnace to make the graphite crystalline structure undergo high-temperature treatment, improve the electrical and thermal conductivity of the carbon material, and at the same time improve the chemical stability of the carbon material, so that the carbon material has lubricity and wear resistance, and then the surface of the obtained graphite electrode is processed by a hole opening machine Holes are opened, and heat dissipation holes are evenly spaced on the surface of the graphite electrode, and an anti-oxidation coating is sprayed on the outer surface of the graphite electrode to slow down the oxidation of the graphite electrode. This not only improves the structural strength of the graphite electrode during later use, but also has the function of heat dissipation and anti-oxidation, thereby extending the service life of the graphite electrode.
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Abstract
一种高强度石墨电极的制备方法,包括以下步骤:首先准备原材料和配料,且对原材料和配料进行精准称重,然后对原材料和配料进行破碎、研磨、筛分处理,保证后期制备时的均匀度,然后对原材料进行煅烧,且在煅烧冷却后与配料一起混捏处理,之后进行成型、挤压、焙烧,其中焙烧分为两次进行,焙烧结束后进行石墨化处理,最后对得到的石墨电极进行开孔和抗氧化层喷涂。该高强度石墨电极的制备方法可以使石墨电极在长时间使用时,通过散热孔增加空气流通,将内部温度向外传递,进而加快石墨电极的散热进度,而且在抗氧化层的作用下,可以对石墨电极进行保护,有效减缓石墨电极的氧化速度,延长石墨电极的使用寿命。
Description
本发明涉及石墨电极制备技术领域,具体为一种高强度石墨电极的制备方法。
石墨电极主要以石油焦、针状焦为原料,以煤沥青做结合剂,经过煅烧、配料、混捏等步骤加工而制成,石墨电极在生产中的应用比较广泛,可以作为导电材料。
如公开号为CN114751747A,一种石墨电极及其制备工艺,该工艺包括以下步骤:S1:第一挤压底板、多个第一盘体和第一挤压顶板之间固定形成第一石墨电极;S2:第二挤压底板、多个第二盘体、扩孔盘、限位盘和第二挤压顶板之间固定形成第二石墨电极;S3:转换机构穿过第一石墨电极伸入到第二石墨电极内形成石墨电极;一种石墨电极,包括第一石墨电极、第二石墨电极和转换机构;第一石墨电极包括第一挤压底板、第一盘体、第一挤压顶板、连接钉Ⅰ和连接钉Ⅱ,第二石墨电极包括第二挤压底板、第二盘体、扩孔盘、限位盘、第二挤压顶板、连接钉Ⅲ和连接钉Ⅳ;可以制备一种偏轴心传导的石墨电极,这样的石墨电极在使用时没有抗氧化保护,缩短了对石墨电极的使用寿命;
如公开号为CN209120506U,一种电弧炉石墨电极,包括石墨电极单元、电极接头和电极端盖,所述石墨电极单元中心设置有通孔,所述石墨电极单元组合形成石墨电极本体,相邻两个所述石墨电极单元具有不同直径的通孔,现有电弧炉石墨电极内通孔上下孔径相同用于通入冷却气体,提高石墨使用寿命,通过以上技术方案可知,本实用新型实施例提供的电弧炉石墨电极,通过设置石墨阳极内通孔直径差,增加不同石墨电极单元间内部气体湍流,
提高换热效率,延长石墨电极整体使用寿命,这样的石墨电极自身强度低,随着使用时间的增加会出现损耗率大的现象,从而降低了对石墨电极的使用效果;
所以我们提出了一种高强度石墨电极的制备方法,以便于解决上述中提出的问题。
发明内容
本发明的目的在于提供一种高强度石墨电极的制备方法,以解决上述背景技术中提出现有的石墨电极在使用时没有抗氧化保护,缩短了对石墨电极的使用寿命,而且石墨电极自身强度低,随着使用时间的增加会出现损耗率大的现象,从而降低了对石墨电极的使用效果的问题。
为实现上述目的,本发明提供如下技术方案:一种高强度石墨电极的制备方法,包括:
步骤1:准备原材料
对原材料进行称重存储,即准备石油焦40-60份,针状焦30-50份,煤沥青20-40份;
步骤2:对原料进行第一次处理
将大块的石油焦、针状焦和煤沥青放入破碎机中进行破碎,使石油焦、针状焦和煤沥青的颗粒变小;
步骤3:对原料进行第二次处理
将破碎后的石油焦、针状焦和煤沥青进行磨粉处理,且在磨粉后进行筛分,保证原材料的细腻度;
步骤4:准备配料
对配料进行称重,即准备氧化钙3-5份,三氧化二铁0.5-1份,碳纤维20-40份;
步骤5:对配料进行处理
将配料放入研磨机中进行研磨,使配料的颗粒减小,且对研磨后的配料进行筛分,保证配料的细腻度;
步骤6:对原料进行煅烧处理
将原材料放入煅烧炉中进行热处理,排出所含的水分和挥发份,且在煅烧后进行冷却;
步骤7:混捏处理
将冷却后的原材料和配料一起倒入混捏机中进行混合,得到混合物;
步骤8:成型处理
将混捏好的混合物放入成型设备中,施加外部作用力使其产生塑性变形,形成一定形状、尺寸、密度和强度的生坯,且在成型生坯后进行冷却;
步骤9:挤压
将冷却至一定温度的生坯进行装料,放入压机中,然后进行预压、挤压、剪切;
步骤10:焙烧
将生坯在填充料的保护下,装入加热炉内进行高温热处理,使生坯中的煤沥青碳化,提高机械强度;
步骤11:石墨化处理
在高温炉内保护介质中对炭制品加热,提高炭材料的导电、导热性。
步骤12:开孔处理
在石墨电极的表面开设散热孔,提高石墨电极使用时的散热进度。
步骤13:防氧化处理
在石墨电极的外表面喷涂防氧化涂层,减缓石墨电极的氧化。
优选的,所述步骤1中的石油焦50份,针状焦40份,煤沥青20份,且步骤2中的破碎机为颚式破碎机,并且破碎后的粒径为0.5-20mm。
优选的,所述步骤3中的原材料磨粉后筛分,且筛网的孔径范围为0.075-0.15mm。
优选的,所述步骤4中的氧化钙4份,三氧化二铁0.75份,碳纤维30份,且步骤5中的配料粉碎机为颚式破碎机,并且破碎粒径为0.5-20mm,同时配料破碎后进行筛分,而筛网的孔径为0.075-0.15mm。
优选的,所述步骤6中的原料煅烧炉采用燃气及自身挥发份作为热源进行煅烧,且煅烧的温度为1250-1350℃。
优选的,所述步骤7中的混捏过程为:干混20-35min,湿混40-55min,使不同粒度大小的固体炭质物料均匀的混合,提高混合料的密实度。
优选的,所述步骤8中的成型方法为模压,且采用的设备为立式液压机,所述步骤9中的挤压过程为凉料、装料、预压、挤压,将混捏后的炭质物料进行降温,且降至适宜温度,并且温度范围为90-120℃,装料时将适宜温度的炭质物料放入压机中,且用4-10MPa压实,然后进行预压,预压的压力为20-25MPa,且预压的时间为3-5min,并且抽真空,之后进行挤压,挤压的压力为5-15MPa。
优选的,所述步骤10中的焙烧分为2次,且一次焙烧的时间为22-30天,焙烧最高温度为1250℃,并且二次焙烧的时间为5-10天,焙烧最高温度范围为700-800℃,同时二次焙烧是焙烧品浸渍后再次焙烧。
优选的,所述步骤10中的二次焙烧浸渍过程为先对焙烧坯进行表面清理,然后进行预热,预热温度为260-380℃,且预热时间为6-10h,然后将焙烧坯装入浸渍罐,进行抽真空处理,抽真空的压力为8-9KPa,时间为40-50min,然后注沥青,温度为180-200℃,之后再次加压,压力为1.2-1.5MPa,时间为3-4h,最后进行冷却。
优选的,所述步骤12中的开孔处理是在石墨电极的表面通过开孔机进行开孔,且散热孔在石墨电极的表面等间距分布。
优选的,所述步骤9中的过滤方式为使搅拌后的混合物从反应釜的出料口流出,且使用滤网过滤,并且滤网的孔径为1-5mm。
与现有技术相比,本发明的有益效果是:
(1)该高强度石墨电极的制备方法,在制备过程中,对原材料和配料均采用了破碎和筛分的方式,这样可以使原材料和配料的粒径度更加持细腻,从而可以使后期混捏时得到的混合物更加均匀,有效防止出现原材料和配料粒度大小差距过大的现象,为石墨电极的制备提供了便捷条件;
(2)该高强度石墨电极的制备方法,在石墨电极煅烧过程中,分为两次煅烧,且二次煅烧前对炭质物料进行了浸渍,这样通过浸渍可以使炭质物料的机械强度更好,从而在后期使用时,可以增加使用时的强度,也可以提高热稳定性和化学稳定性,有效降低损耗率,提高对石墨电极的使用效果;
(3)该高强度石墨电极的制备方法,在石墨电极的外表面涂有抗氧化层,且在石墨电极的表面开设有散热孔,这样可以使石墨电极在长时间使用时,通过散热孔增加空气流通,将内部温度向外传递,进而加快石墨电极的散热进度,而且在抗氧化层的作用下,可以对石墨电极进行保护,有效减缓石墨电极的氧化速度,延长石墨电极的使用寿命。
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
本实施例1提供一种高强度石墨电极的制备方法,以下对上述方法进行详细介绍。
在制备前,先对原材料进行准备,即准备石油焦50份,针状焦40份,煤沥青20份,然后对原料进行第一次处理,将大块的石油焦、针状焦和煤沥青放入破碎机中进行破碎,使石油焦、针状焦和煤沥青的颗粒变小,其中破碎机为颚式破碎机,且破碎粒径为0.5-20mm,原材料破碎后,对原材料进行磨粉第二次处理,并且在磨粉后进行筛分,其中筛网的孔径范围为0.075-0.15mm,之后准备配料,即准备氧化钙4份,三氧化二铁0.75份,碳纤维30份,且在配料准备好后,将配料放入颚式破碎机,并且破碎粒径为0.5-20mm,同时配料破碎后进行筛分,而筛网的孔径为0.075-0.15mm,这样便可以使原材料和配料都保证均匀度,
然后对原料进行煅烧处理,将原材料放入煅烧炉中进行热处理,排出所含的水分和挥发份,原料煅烧炉采用燃气及自身挥发份作为热源进行煅烧,且煅烧的温度为1250-1350℃,且在煅烧后进行冷却,然后将冷却后的原材料和配料一起倒入混捏机中进行混合,得到混合物,混捏过程为:先干混20-35min,然后湿混40-55min,使不同粒度大小的固体炭质物料均匀的混合,提高混合料的密实度,
然后将混捏好的混合物放入成型设备中,施加外部作用力使其产生塑性变形,形成一定形状、尺寸、密度和强度的生坯,且在成型生坯后进行冷却,成型方法为模压,且采用的设备为立式液压机,之后进行挤压处理,挤压过程为凉料、装料、预压、挤压,将混捏后的炭质物料进行降温,且降至适宜温度,并且温度范围为90-120℃,装料时将适宜温度的炭质物料放入压机中,且用4-10MPa压实,然后进行预压,预压的压力为20-25MPa,且预压的时间为3-5min,并且抽真空,之后进行挤压,挤压的压力为5-15MPa,挤压后将生坯在填充料的保护下,装入加热炉内进行高温热处理,使生坯中的煤沥青碳化,提高机械强度,
在炭质物料挤压后,进行焙烧,且焙烧分为2次,一次焙烧的时间为22-30
天,焙烧最高温度为1250℃,并且二次焙烧的时间为5-10天,焙烧最高温度范围为700-800℃,同时二次焙烧是焙烧品浸渍后再次焙烧,其中浸渍过程为先对焙烧坯进行表面清理,然后进行预热,预热温度为260-380℃,且预热时间为6-10h,然后将焙烧坯装入浸渍罐,进行抽真空处理,抽真空的压力为8-9KPa,时间为40-50min,然后注沥青,温度为180-200℃,之后再次加压,压力为1.2-1.5MPa,时间为3-4h,最后进行冷却,浸渍冷却后进行石墨化处理,在高温炉内保护介质中把炭制品加热到2300℃以上,使石墨晶质结构进行高温处理,提高炭材料的导电、导热性,同时可以提高炭材料的化学稳定性,使炭材料具有润滑性和抗磨性,之后对得到的石墨电极表面通过开孔机进行开孔,且散热孔在石墨电极的表面等间距分布,并且在石墨电极的外表面喷涂防氧化涂层,减缓石墨电极的氧化,这样可以使石墨电极后期使用时,不仅提高了自身的结构强度,还具有散热抗氧化的功能,进而延长了石墨电极的使用寿命。
实施例2
本实施例2提供一种高强度石墨电极的制备方法,以下对上述方法进行详细介绍。
在制备前,先对原材料进行准备,即准备石油焦60份,针状焦50份,煤沥青30份,然后对原料进行第一次处理,将大块的石油焦、针状焦和煤沥青放入破碎机中进行破碎,使石油焦、针状焦和煤沥青的颗粒变小,其中破碎机为颚式破碎机,且破碎粒径为0.5-20mm,原材料破碎后,对原材料进行磨粉第二次处理,并且在磨粉后进行筛分,其中筛网的孔径范围为0.075-0.15mm,之后准备配料,即准备氧化钙5份,三氧化二铁1份,碳纤维20份,且在配料准备好后,将配料放入颚式破碎机,并且破碎粒径为0.5-20mm,同时配料破碎后进行筛分,而筛网的孔径为0.075-0.15mm,这样便可以使原材料和配料都保证均匀度,
然后对原料进行煅烧处理,将原材料放入煅烧炉中进行热处理,排出所含的水分和挥发份,原料煅烧炉采用燃气及自身挥发份作为热源进行煅烧,且煅烧的温度为1250-1350℃,且在煅烧后进行冷却,然后将冷却后的原材料和配料一起倒入混捏机中进行混合,得到混合物,混捏过程为:先干混20-35min,然后湿混40-55min,使不同粒度大小的固体炭质物料均匀的混合,提高混合料的密实度,
然后将混捏好的混合物放入成型设备中,施加外部作用力使其产生塑性变形,形成一定形状、尺寸、密度和强度的生坯,且在成型生坯后进行冷却,成型方法为模压,且采用的设备为立式液压机,之后进行挤压处理,挤压过程为凉料、装料、预压、挤压,将混捏后的炭质物料进行降温,且降至适宜温度,并且温度范围为90-120℃,装料时将适宜温度的炭质物料放入压机中,且用4-10MPa压实,然后进行预压,预压的压力为20-25MPa,且预压的时间为3-5min,并且抽真空,之后进行挤压,挤压的压力为5-15MPa,挤压后将生坯在填充料的保护下,装入加热炉内进行高温热处理,使生坯中的煤沥青碳化,提高机械强度,
在炭质物料挤压后,进行焙烧,且焙烧分为2次,一次焙烧的时间为22-30天,焙烧最高温度为1250℃,并且二次焙烧的时间为5-10天,焙烧最高温度范围为700-800℃,同时二次焙烧是焙烧品浸渍后再次焙烧,其中浸渍过程为先对焙烧坯进行表面清理,然后进行预热,预热温度为260-380℃,且预热时间为6-10h,然后将焙烧坯装入浸渍罐,进行抽真空处理,抽真空的压力为8-9KPa,时间为40-50min,然后注沥青,温度为180-200℃,之后再次加压,压力为1.2-1.5MPa,时间为3-4h,最后进行冷却,浸渍冷却后进行石墨化处理,在高温炉内保护介质中把炭制品加热到2300℃以上,使石墨晶质结构进行高温处理,提高炭材料的导电、导热性,同时可以提高炭材料的化学稳定性,使炭材料具有润滑性和抗磨性,之后对得到的石墨电极表面通过开孔机
进行开孔,且散热孔在石墨电极的表面等间距分布,并且在石墨电极的外表面喷涂防氧化涂层,减缓石墨电极的氧化,这样可以使石墨电极后期使用时,不仅提高了自身的结构强度,还具有散热抗氧化的功能,进而延长了石墨电极的使用寿命。
尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
- 一种高强度石墨电极的制备方法,包括:步骤1:准备原材料对原材料进行称重存储,即准备石油焦40-60份,针状焦30-50份,煤沥青20-40份;步骤2:对原料进行第一次处理将大块的石油焦、针状焦和煤沥青放入破碎机中进行破碎,使石油焦、针状焦和煤沥青的颗粒变小;步骤3:对原料进行第二次处理将破碎后的石油焦、针状焦和煤沥青进行磨粉处理,且在磨粉后进行筛分,保证原材料的细腻度;步骤4:准备配料对配料进行称重,即准备氧化钙3-5份,三氧化二铁0.5-1份,碳纤维20-40份;步骤5:对配料进行处理将配料放入研磨机中进行研磨,使配料的颗粒减小,且对研磨后的配料进行筛分,保证配料的细腻度;步骤6:对原料进行煅烧处理将原材料放入煅烧炉中进行热处理,排出所含的水分和挥发份,且在煅烧后进行冷却;步骤7:混捏处理将冷却后的原材料和配料一起倒入混捏机中进行混合,得到混合物;步骤8:成型处理将混捏好的混合物放入成型设备中,施加外部作用力使其产生塑性变形,形成一定形状、尺寸、密度和强度的生坯,且在成型生坯后进行冷却;步骤9:挤压将冷却至一定温度的生坯进行装料,放入压机中,然后进行预压、挤压、剪切;步骤10:焙烧将生坯在填充料的保护下,装入加热炉内进行高温热处理,使生坯中的煤沥青碳化,提高机械强度;步骤11:石墨化处理在高温炉内保护介质中对炭制品加热,提高炭材料的导电、导热性。步骤12:开孔处理在石墨电极的表面开设散热孔,提高石墨电极使用时的散热进度。步骤13:防氧化处理在石墨电极的外表面喷涂防氧化涂层,减缓石墨电极的氧化。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤1中的石油焦50份,针状焦40份,煤沥青20份,且步骤2中的破碎机为颚式破碎机,并且破碎后的粒径为0.5-20mm。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤3中的原材料磨粉后筛分,且筛网的孔径范围为0.075-0.15mm。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤4中的氧化钙4份,三氧化二铁0.75份,碳纤维30份,且步骤5中的配料粉碎机为颚式破碎机,并且破碎粒径为0.5-20mm,同时配料破碎后进行筛分,而筛网的孔径为0.075-0.15mm。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤6中的原料煅烧炉采用燃气及自身挥发份作为热源进行煅烧,且煅烧的温度为1250-1350℃。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤7中的混捏过程为:干混20-35min,湿混40-55min,使不同粒度大 小的固体炭质物料均匀的混合,提高混合料的密实度。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤8中的成型方法为模压,且采用的设备为立式液压机,所述步骤9中的挤压过程为凉料、装料、预压、挤压,将混捏后的炭质物料进行降温,且降至适宜温度,并且温度范围为90-120℃,装料时将适宜温度的炭质物料放入压机中,且用4-10MPa压实,然后进行预压,预压的压力为20-25MPa,且预压的时间为3-5min,并且抽真空,之后进行挤压,挤压的压力为5-15MPa。
- 根据权利要求1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤10中的焙烧分为2次,且一次焙烧的时间为22-30天,焙烧最高温度为1250℃,并且二次焙烧的时间为5-10天,焙烧最高温度范围为700-800℃,同时二次焙烧是焙烧品浸渍后再次焙烧。
- 根据权利要8所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤10中的二次焙烧浸渍过程为先对焙烧坯进行表面清理,然后进行预热,预热温度为260-380℃,且预热时间为6-10h,然后将焙烧坯装入浸渍罐,进行抽真空处理,抽真空的压力为8-9KPa,时间为40-50min,然后注沥青,温度为180-200℃,之后再次加压,压力为1.2-1.5MPa,时间为3-4h,最后进行冷却。
- 根据权利要1所述的一种高强度石墨电极的制备方法,其特征在于:所述步骤12中的开孔处理是在石墨电极的表面通过开孔机进行开孔,且散热孔在石墨电极的表面等间距分布。
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