CN108751993A - A kind of manufacturing process of UHP graphite electrodes - Google Patents
A kind of manufacturing process of UHP graphite electrodes Download PDFInfo
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- CN108751993A CN108751993A CN201810567113.8A CN201810567113A CN108751993A CN 108751993 A CN108751993 A CN 108751993A CN 201810567113 A CN201810567113 A CN 201810567113A CN 108751993 A CN108751993 A CN 108751993A
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Abstract
The invention discloses a kind of manufacturing process of UHP graphite electrodes, include the following steps：S100, dispensing, S200, molding, S300, roasting and dipping, S400, graphitization, S500, machining.Present invention process is simple, and manufacturing cost is relatively low, and end properties are not weaker than mainstream finished product in the market, even better than import finished product.Therefore, it is possible to bring the profit margin of bigger for enterprise, the competitiveness of enterprise is improved.
Description
Technical field
The present invention relates to a kind of graphite electrode manufacturing process, more particularly to a kind of manufacturing process of UHP graphite electrodes.
Background technology
Graphite electrode refers to using petroleum coke, pitch coke as aggregate, and coal tar pitch is adhesive, by raw material calcining, broken mill
Powder, dispensing, kneading, molding, roasting, dipping, graphitization and mechanical processing and a kind of manufactured high temperature resistant graphite conductive material.
It is widely used in：
(1) it is used for electrical arc furnace
Electric furnace steel making is the use rich and influential family of graphite electrode.China's electric furnace output of steel accounts for about 18% or so of crude steel yield, steel-making stone
Electrode ink accounts for the 70%~80% of the total dosage of graphite electrode.Electric furnace steel making is that electric current is imported into stove using graphite electrode, utilizes electricity
Extremely high temperature heat source caused by starting arc is smelted between portion and furnace charge.
(2) it is used for ore-smelting electric furnace
Ore-smelting electric furnace is mainly for the production of industrial silicon and yellow phosphorus etc., its main feature is that the lower part of conductive electrode is embedded in furnace charge, is expecting
Electric arc is formed in layer, and heats furnace charge using the thermal energy that the resistance of furnace charge itself is sent out, wherein requiring current density higher
Ore-smelting electric furnace need to use graphite electrode, such as often production 1t silicon need to consume graphite electrode about 100kg, often produce 1t yellow phosphorus need to consume
Graphite electrode about 40kg.
(3) it is used for resistance furnace
The electric furnace etc. for producing the graphitizing furnace of graphite product, the melting furnaces for melting glass and production silicon carbide belongs to resistance furnace,
Interior the filled material of stove is both heating resistor and by heating target, in general, conductive graphite electrode is embedded in resistance end furnace
In burner wall, discontinuously consumed for graphite electrode herein.
(4) special-shaped graphite products are used to prepare
The blank of graphite electrode is additionally operable to be processed into the special-shaped graphite products such as various crucibles, mold, boat and heater.For example,
In quartz glass industry, 1t electric smelting pipes are often produced, graphite electrode stock 10t need to be used；1t quartz bricks are often produced, graphite electricity need to be consumed
Pole blank 100kg.
The manufacturing process of graphite electrode is very ripe and diversified at present, and end properties are also relatively high, but each
The manufacturing process of producer belongs to confidential state or by patent protection, and therefore, it is necessary to enter the manufacturing field of graphite electrode to be just engaged in
Must design it is a kind of it is completely new, with the distinguishing manufacturing process of the prior art, but currently, the manufacturing process by designed, designed is wanted
Complex process, yield rate are low, cause cost increase so that enterprise loses competitiveness；Poor product quality so that enterprise is competing
It is poor to strive power.
Ultra high power graphite electrode (UHP) is current emerging graphite electrode, and market demand gradually increases, so research
The emerging preparation process of UHP graphite electrodes is also just very necessary.
Therefore, applicant proposes a kind of manufacturing process of UHP graphite electrodes, simple for process, and cost is relatively low, but at
Moral character can meet the needs of current.
Invention content
In view of the drawbacks described above of the prior art, technical problem to be solved by the invention is to provide a kind of UHP graphite electricity
The manufacturing process of pole.
To achieve the above object, the present invention provides a kind of manufacturing process of UHP graphite electrodes, include the following steps：
S100, dispensing
S110, raw material, petroleum coke, needle coke, modified coal asphalt, the petroleum coke are that low-sulfur is burnt；The needle coke uses
Coal-based needle coke；
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%；
S120, petroleum coke, needle coke are crushed, fine grinding, its grain size is made to be not more than 0.075 ㎜；
S130, S120 is crushed after petroleum coke, needle coke is uniformly mixed according to following weight part ratio：10-15:20-30 is mixed
First by two kinds of dry-mixed 10-20min of fines during closing, ethyl alcohol is then added and carries out wet mixing 30-40min；
S140, the mixed fineves of S130 are uniformly mixed with modified coal asphalt according to following weight part ratio：10-15：6-8；
S200, molding
S210, by S140, treated that raw material is stirred, and raw material is heated to 100-120 DEG C, stirs 1-2 hours；
S220, it mixed raw material in S210 is put into forcing press is compacted by 6-8MPa；
S230, by treated in S220, raw material is put into extruder, carries out extrusion forming by the pressure of 10-15MPa, then
Section is cut into according to preset requirement, the raw material after section is cut into and is put into temperature to be cooled down in 5-10 degrees Celsius of water；
S300, roasting and dipping
S310, primary roasting, the raw material cut off in S230 is put into roaster, is roasted by 1250 DEG C of high temperature, and fill
Enter to protect gas（Argon gas）, heating mode is as follows：
It 0-350 DEG C, 4.4 DEG C/h, is kept for 50 hours after reaching 350 DEG C；
It 350-400 DEG C, 1.7 DEG C/h, is kept for 30 hours after reaching 400 DEG C；
400-500 DEG C, 1.4 DEG C/h；It is kept for 70 hours after reaching 500 DEG C；
500-600 DEG C, 2.0 DEG C/h；It is kept for 50 hours after reaching 600 DEG C；
600-700 DEG C, 4.0 DEG C/h；It is kept for 25 hours after reaching 700 DEG C；
700-800 DEG C, 5.0 DEG C/h；It is kept for 20 hours after reaching 800 DEG C；
800-1000 DEG C, 8.0 DEG C/h；It is kept for 25 hours after reaching 1000 DEG C；
1000-1250 DEG C, 10.0 DEG C/h；It is kept for 54 hours after reaching 1250 DEG C；
After the completion of roasting, stops heating, be cooled to room temperature in roaster；
Coal tar pitch coking in roasting process in green compact, the fugitive constituent of discharge 10% or so, while volume generates the contraction of 2-3%,
Mass loss 8-10%.Significant changes also have occurred in the physicochemical property of charcoal base, since the porosity increases bulk density by 1.70g/
Cm3 is reduced to 1.60g/cm3, and 10000 μ Ω .m of resistivity or so are down to 40-50 μ Ω .m, and the mechanical strength for roasting base also greatly carries
It is high.
S310 treated raw materials are carried out removing surface, mainly remove flash removed, be then placed in dipping by S320, dipping
In tank, and it is preheated to 280-350 DEG C, is kept for 6-8 hours；
Then impregnating autoclave is vacuumized, and keeps 40-50min, then after coal tar pitch is heated to 350-450 DEG C, keep 10-12 small
When, it is then injected into impregnating autoclave so that raw material is completely immersed in coal tar pitch；
Then, protection gas is added in impregnating autoclave（Argon gas）, after air pressure reaches 1.2-1.5MPa, kept for 3-4 hours；
Last pressure release, is discharged coal tar pitch, and raw material is cooled to room temperature in impregnating autoclave, takes out and clear up surface；
S330, after baking, by S320, treated that raw material is placed again into roaster, is roasted again by 2100 DEG C of high temperature
It burns, and is filled with protection gas（Argon gas）, heating mode is as follows：
It 0-800 DEG C, 24-34 DEG C/h, is kept for 20 hours after reaching 800 degrees Celsius；
It 800-1600 DEG C, 38-52 DEG C/h, is kept for 20 hours after reaching 1600 DEG C；
It 1600-2100 DEG C, 10-15 DEG C/h, is kept for 50 hours after reaching 2100 DEG C, is then cooled to room temperature, takes in roaster
Go out to clear up surface；It is crackle in order to prevent to reduce heating rate herein.
After baking is roasted again after roasting product impregnates, the technique for making the pitch in immersion roasting product hole carbonize
Process.
S340, S320-S330 is repeated twice or more than twice；
S400, graphitization, by S340, treated that raw material is put into internal thermal serial (LWG) stove, is filled with protective gas and is heated to
It 2300-3000 DEG C, is kept for 100-200 hours, keeps its graphitization, specific heating mode as follows：
0-1200 DEG C, continuous 40-60 DEG C of two hourly averages temperature rise rate；
1200-2100 DEG C, continuous 10-30 DEG C of two hourly averages temperature rise rate；
2100-3000 DEG C, continuous 30-50 DEG C of two hourly averages temperature rise rate is kept for 100-200 hours after reaching 3000 DEG C；
Raw material can be made to reach following effect by this step：
1. the conduction of high Carbon Materials, thermal conductivity（Resistivity reduces 4-5 times, and thermal conductivity improves about 10 times）；
Performance and chemical stability 2. the heat resistanceheat resistant for improving Carbon Materials is shaken（Linear expansion coefficient reduces 50-80%）；
3. making Carbon Materials that there is lubricity and wear resistence；
4. impurity is discharged, the purity of Carbon Materials is improved（The ash content of product drops to 0.3% or so by 0.5-0.8%）.
S500, machining, by S400, treated that raw material is machined out, and until reaching pre-set dimension, that is, produces stone
Electrode ink.
The beneficial effects of the invention are as follows：Present invention process is simple, and manufacturing cost is relatively low, and end properties are not weaker than in the market
Mainstream finished product, even better than import finished product.Therefore, it is possible to bring the profit margin of bigger for enterprise, the competition of enterprise is improved
Power.
Specific implementation mode
With reference to embodiment, the invention will be further described：
Embodiment one
A kind of manufacturing process of UHP graphite electrodes, includes the following steps：
S100, dispensing
S110, raw material, petroleum coke, needle coke, modified coal asphalt, the petroleum coke are that low-sulfur is burnt；The needle coke uses
Coal-based needle coke；
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%；
S120, petroleum coke, needle coke are crushed, fine grinding, its grain size is made to be not more than 0.075 ㎜；
S130, S120 is crushed after petroleum coke, needle coke is uniformly mixed according to following weight part ratio：10:30, it mixed
Then two kinds of dry-mixed 10-20min of fines are added ethyl alcohol and carry out wet mixing 30-40min by Cheng Zhongxian；
S140, the mixed fineves of S130 are uniformly mixed with modified coal asphalt according to following weight part ratio： 15：8；
S200, molding
S210, by S140, treated that raw material is stirred, and raw material is heated to 100-120 DEG C, stirs 1-2 hours；
S220, it mixed raw material in S210 is put into forcing press is compacted by 6-8MPa；
S230, by treated in S220, raw material is put into extruder, carries out extrusion forming by the pressure of 10-15MPa, then
Section is cut into according to preset requirement, the raw material after section is cut into and is put into temperature to be cooled down in 5-10 degrees Celsius of water；
S300, roasting and dipping
S310, primary roasting, the raw material cut off in S230 is put into roaster, is roasted by 1250 DEG C of high temperature, and fill
Enter to protect gas（Argon gas）, heating mode is as follows：
It 0-350 DEG C, 4.4 DEG C/h, is kept for 50 hours after reaching 350 DEG C；
It 350-400 DEG C, 1.7 DEG C/h, is kept for 30 hours after reaching 400 DEG C；
400-500 DEG C, 1.4 DEG C/h；It is kept for 70 hours after reaching 500 DEG C；
500-600 DEG C, 2.0 DEG C/h；It is kept for 50 hours after reaching 600 DEG C；
600-700 DEG C, 4.0 DEG C/h；It is kept for 25 hours after reaching 700 DEG C；
700-800 DEG C, 5.0 DEG C/h；It is kept for 20 hours after reaching 800 DEG C；
800-1000 DEG C, 8.0 DEG C/h；It is kept for 25 hours after reaching 1000 DEG C；
1000-1250 DEG C, 10.0 DEG C/h；It is kept for 54 hours after reaching 1250 DEG C；
After the completion of roasting, stops heating, be cooled to room temperature in roaster；
S310 treated raw materials are carried out removing surface, mainly remove flash removed, be then placed in impregnating autoclave by S320, dipping,
And 300 DEG C are preheated to, it is kept for 8 hours；
Then impregnating autoclave is vacuumized, and keeps 50min, then after coal tar pitch is heated to 380 DEG C, kept for 10 hours, then noted
Enter in impregnating autoclave so that raw material is completely immersed in coal tar pitch；
Then, protection gas is added in impregnating autoclave（Argon gas）, after air pressure reaches 1.2-1.5MPa, kept for 3-4 hours；
Last pressure release, is discharged coal tar pitch, and raw material is cooled to room temperature in impregnating autoclave, takes out and clear up surface；
S330, after baking, by S320, treated that raw material is placed again into roaster, is roasted again by 2100 DEG C of high temperature
It burns, and is filled with protection gas（Argon gas）, heating mode is as follows：
It 0-800 DEG C, 28 DEG C/h, is kept for 20 hours after reaching 800 degrees Celsius；
It 800-1600 DEG C, 42 DEG C/h, is kept for 20 hours after reaching 1600 DEG C；
It 1600-2100 DEG C, 10 DEG C/h, is kept for 50 hours after reaching 2100 DEG C, is then cooled to room temperature in roaster, taken out clear
Manage surface；
S340, S320-S330 is repeated twice or more than twice；
S400, graphitization, by S340, treated that raw material is put into internal thermal serial (LWG) stove, is filled with protective gas and is heated to
It 2300-3000 DEG C, is kept for 150 hours, keeps its graphitization, specific heating mode as follows：
0-1200 DEG C, continuous 40 DEG C of two hourly averages temperature rise rate；
1200-2100 DEG C, continuous 20 DEG C of two hourly averages temperature rise rate；
2100-3000 DEG C, continuous 50 DEG C of two hourly averages temperature rise rate is kept for 150 hours after reaching 3000 DEG C；
S500, machining, by S400, treated that raw material is machined out, and until reaching pre-set dimension, that is, produces graphite electricity
Pole.
Embodiment two
A kind of manufacturing process of UHP graphite electrodes, includes the following steps：
S100, dispensing
S110, raw material, petroleum coke, needle coke, modified coal asphalt, the petroleum coke are that low-sulfur is burnt；The needle coke uses
Coal-based needle coke；
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%；
S120, petroleum coke, needle coke are crushed, fine grinding, its grain size is made to be not more than 0.075 ㎜；
S130, S120 is crushed after petroleum coke, needle coke is uniformly mixed according to following weight part ratio：12:28, mixed process
It is middle first by two kinds of dry-mixed 10-20min of fines, ethyl alcohol is then added and carries out wet mixing 30-40min；
S140, the mixed fineves of S130 are uniformly mixed with modified coal asphalt according to following weight part ratio：14：7；
S200, molding
S210, by S140, treated that raw material is stirred, and raw material is heated to 100-120 DEG C, stirs 1-2 hours；
S220, it mixed raw material in S210 is put into forcing press is compacted by 6-8MPa；
S230, by treated in S220, raw material is put into extruder, carries out extrusion forming by the pressure of 10-15MPa, then
Section is cut into according to preset requirement, the raw material after section is cut into and is put into temperature to be cooled down in 5-10 degrees Celsius of water；
S300, roasting and dipping
S310, primary roasting, the raw material cut off in S230 is put into roaster, is roasted by 1250 DEG C of high temperature, and fill
Enter to protect gas（Argon gas）, heating mode is as follows：
It 0-350 DEG C, 4.4 DEG C/h, is kept for 50 hours after reaching 350 DEG C；
It 350-400 DEG C, 1.7 DEG C/h, is kept for 30 hours after reaching 400 DEG C；
400-500 DEG C, 1.4 DEG C/h；It is kept for 70 hours after reaching 500 DEG C；
500-600 DEG C, 2.0 DEG C/h；It is kept for 50 hours after reaching 600 DEG C；
600-700 DEG C, 4.0 DEG C/h；It is kept for 25 hours after reaching 700 DEG C；
700-800 DEG C, 5.0 DEG C/h；It is kept for 20 hours after reaching 800 DEG C；
800-1000 DEG C, 8.0 DEG C/h；It is kept for 25 hours after reaching 1000 DEG C；
1000-1250 DEG C, 10.0 DEG C/h；It is kept for 54 hours after reaching 1250 DEG C；
After the completion of roasting, stops heating, be cooled to room temperature in roaster；
S310 treated raw materials are carried out removing surface, mainly remove flash removed, be then placed in impregnating autoclave by S320, dipping,
And it is preheated to 280-350 DEG C, it is kept for 6-8 hours；
Then impregnating autoclave is vacuumized, and keeps 40-50min, then after coal tar pitch is heated to 350-450 DEG C, keep 10-12 small
When, it is then injected into impregnating autoclave so that raw material is completely immersed in coal tar pitch；
Then, protection gas is added in impregnating autoclave（Argon gas）, after air pressure reaches 1.2-1.5MPa, kept for 3-4 hours；
Last pressure release, is discharged coal tar pitch, and raw material is cooled to room temperature in impregnating autoclave, takes out and clear up surface；
S330, after baking, by S320, treated that raw material is placed again into roaster, is roasted again by 2100 DEG C of high temperature
It burns, and is filled with protection gas（Argon gas）, heating mode is as follows：
It 0-800 DEG C, 24-34 DEG C/h, is kept for 20 hours after reaching 800 degrees Celsius；
It 800-1600 DEG C, 38-52 DEG C/h, is kept for 20 hours after reaching 1600 DEG C；
It 1600-2100 DEG C, 10-15 DEG C/h, is kept for 50 hours after reaching 2100 DEG C, is then cooled to room temperature, takes in roaster
Go out to clear up surface；It is crackle in order to prevent to reduce heating rate herein.
After baking is roasted again after roasting product impregnates, the technique for making the pitch in immersion roasting product hole carbonize
Process.
S340, S320-S330 is repeated twice or more than twice；
S400, graphitization, by S340, treated that raw material is put into internal thermal serial (LWG) stove, is filled with protective gas and is heated to
It 2300-3000 DEG C, is kept for 180 hours, keeps its graphitization, specific heating mode as follows：
0-1200 DEG C, continuous 50 DEG C of two hourly averages temperature rise rate；
1200-2100 DEG C, continuous 10 DEG C of two hourly averages temperature rise rate；
2100-3000 DEG C, continuous 50 DEG C of two hourly averages temperature rise rate is kept for 180 hours after reaching 3000 DEG C；
S500, machining, by S400, treated that raw material is machined out, and until reaching pre-set dimension, that is, produces graphite electricity
Pole.
Place is not described in detail by the present invention, is the known technology of those skilled in the art.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that those skilled in the art without
It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical solution, all should be in the protection domain being defined in the patent claims.
Claims (4)
1. a kind of manufacturing process of UHP graphite electrodes, which is characterized in that include the following steps：
S100, dispensing
S110, raw material, petroleum coke, needle coke, modified coal asphalt, the petroleum coke are that low-sulfur is burnt；The needle coke uses
Coal-based needle coke；
The softening point of the modified coal asphalt is 100-120 DEG C, and coking value is >=55%, ash content≤0.15%；
S120, petroleum coke, needle coke are crushed, fine grinding, its grain size is made to be not more than 0.075 ㎜；
S130, S120 is crushed after petroleum coke, needle coke is uniformly mixed according to following weight part ratio：10-15:20-30 is mixed
First by two kinds of dry-mixed 10-20min of fines during closing, ethyl alcohol is then added and carries out wet mixing 30-40min；
S140, the mixed fineves of S130 are uniformly mixed with modified coal asphalt according to following weight part ratio：10-15：6-8；
S200, molding
S210, by S140, treated that raw material is stirred, and raw material is heated to 100-120 DEG C, stirs 1-2 hours；
S220, it mixed raw material in S210 is put into forcing press is compacted by 6-8MPa；
S230, by treated in S220, raw material is put into extruder, carries out extrusion forming by the pressure of 10-15MPa, then
Section is cut into according to preset requirement, the raw material after section is cut into and is put into temperature to be cooled down in 5-10 degrees Celsius of water；
S300, roasting and dipping
S310, primary roasting, the raw material cut off in S230 is put into roaster, is roasted by 1250 DEG C of high temperature, and fill
Enter to protect gas；
S310 treated raw materials are carried out removing surface, mainly remove flash removed, be then placed in impregnating autoclave by S320, dipping,
And it is preheated to 280-350 DEG C, it is kept for 6-8 hours；
Then impregnating autoclave is vacuumized, and keeps 40-50min, then after coal tar pitch is heated to 350-450 DEG C, keep 10-12 small
When, it is then injected into impregnating autoclave so that raw material is completely immersed in coal tar pitch；
Then, protection gas is added in impregnating autoclave, after air pressure reaches 1.2-1.5MPa, is kept for 3-4 hours；
Last pressure release, is discharged coal tar pitch, and raw material is cooled to room temperature in impregnating autoclave, takes out and clear up surface；
S330, after baking, by S320, treated that raw material is placed again into roaster, is roasted again by 2100 DEG C of high temperature
It burns, and is filled with protection gas；
S340, S320-S330 is repeated twice or more than twice；
S400, graphitization, by S340, treated that raw material is put into internal thermal serial stove, is filled with protective gas and is heated to 2300-
It 3000 DEG C, is kept for 100-200 hours, makes its graphitization；
S500, machining, by S400, treated that raw material is machined out, and until reaching pre-set dimension, that is, produces graphite electricity
Pole.
2. manufacturing process as described in claim 1, which is characterized in that heating mode is as follows in S310：
It 0-350 DEG C, 4.4 DEG C/h, is kept for 50 hours after reaching 350 DEG C；
It 350-400 DEG C, 1.7 DEG C/h, is kept for 30 hours after reaching 400 DEG C；
400-500 DEG C, 1.4 DEG C/h；It is kept for 70 hours after reaching 500 DEG C；
500-600 DEG C, 2.0 DEG C/h；It is kept for 50 hours after reaching 600 DEG C；
600-700 DEG C, 4.0 DEG C/h；It is kept for 25 hours after reaching 700 DEG C；
700-800 DEG C, 5.0 DEG C/h；It is kept for 20 hours after reaching 800 DEG C；
800-1000 DEG C, 8.0 DEG C/h；It is kept for 25 hours after reaching 1000 DEG C；
1000-1250 DEG C, 10.0 DEG C/h；It is kept for 54 hours after reaching 1250 DEG C；
After the completion of roasting, stops heating, be cooled to room temperature in roaster.
3. manufacturing process as described in claim 1, which is characterized in that heating mode is as follows in S330：
It 0-800 DEG C, 24-34 DEG C/h, is kept for 20 hours after reaching 800 degrees Celsius；
It 800-1600 DEG C, 38-52 DEG C/h, is kept for 20 hours after reaching 1600 DEG C；
It 1600-2100 DEG C, 10-15 DEG C/h, is kept for 50 hours after reaching 2100 DEG C, is then cooled to room temperature, takes in roaster
Go out to clear up surface.
4. manufacturing process as described in claim 1, which is characterized in that heating mode is as follows in S400：
0-1200 DEG C, continuous 40-60 DEG C of two hourly averages temperature rise rate；
1200-2100 DEG C, continuous 10-30 DEG C of two hourly averages temperature rise rate；
2100-3000 DEG C, continuous 30-50 DEG C of two hourly averages temperature rise rate is kept for 100-200 hours after reaching 3000 DEG C.
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