CN108892136A - A kind of manufacturing process of high-heat resistance shock resistant graphite electrode - Google Patents
A kind of manufacturing process of high-heat resistance shock resistant graphite electrode Download PDFInfo
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- CN108892136A CN108892136A CN201810716095.5A CN201810716095A CN108892136A CN 108892136 A CN108892136 A CN 108892136A CN 201810716095 A CN201810716095 A CN 201810716095A CN 108892136 A CN108892136 A CN 108892136A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/20—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein the material is extruded
- B28B3/26—Extrusion dies
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Abstract
The invention discloses a kind of manufacturing process of high-heat resistance shock resistant graphite electrode, include the following steps：S100, ingredient, S200, molding, S300, machining, by S220, treated that adobe is machined out, and until reaching pre-set dimension, that is, produces graphite electrode.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, bigger profit margin can be brought for enterprise, improves the competitiveness of enterprise.Finished product thermal shock resistance of the invention simultaneously is higher.
Description
Technical field
The present invention relates to one kind, more particularly to a kind of manufacturing process of high-heat resistance shock resistant graphite electrode.
Background technique
Graphite electrode refers to that coal tar pitch is adhesive using petroleum coke, pitch coke as aggregate, by raw material calcining, broken mill
Powder, ingredient, kneading, molding, roasting, dipping, graphitization and machining 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, and stone is used in steel-making
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 furnace using graphite electrode, utilizes electricity
High temperature heat source caused by starting arc is smelted between extreme 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 issued, wherein requiring current density higher
Ore-smelting electric furnace need to use graphite electrode, such as every production 1t silicon need to consume graphite electrode about 100kg, and every production 1t yellow phosphorus needs to consume
Graphite electrode about 40kg.
(3) it is used for resistance furnace
It produces the graphitizing furnace of graphite product, the melting furnaces for melting glass and the electric furnace for producing silicon carbide etc. and belongs to resistance furnace,
Filled material is both heating resistor and is heated object in furnace, in general, conductive graphite electrode insertion 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 also used to be processed into the special-shaped graphite products such as various crucibles, mold, boat and heater.For example,
In quartz glass industry, every production 1t electric smelting pipe need to use graphite electrode stock 10t；Every production 1t quartz brick need to consume graphite electricity
Pole blank 100kg.
And existing graphite electrode the phenomenon that being easy to appear cracking, chip off-falling in smelting process, falling off and fracture, this can shadow
Ring the effect smelted, the reason that mainly its thermal shock resistance is poor of tracing it to its cause.
Therefore, applicant proposes a kind of manufacturing process of high-heat resistance shock resistant graphite electrode, can effectively improve finished product
Thermal shock resistance.
Summary of the invention
In view of the above drawbacks of the prior art, technical problem to be solved by the invention is to provide a kind of high-heat resistance shock resistants
The manufacturing process of graphite electrode.
To achieve the above object, the present invention provides a kind of manufacturing process of high-heat resistance shock resistant graphite electrode, including it is as follows
Step：
S100, ingredient
S110, raw material, petroleum coke, needle coke, coal tar pitch, acetylene black, PVDF（Polyvinyladine floride）,NMP（N- crassitude
Ketone）, molybdenum disulfide；
The petroleum coke is that low-sulfur is burnt；
The needle coke uses coal-based needle coke；
The softening point of the modified coal asphalt is 90-100 DEG C, and coking value is >=55%, and ash content≤0.20%, fineness exists when room temperature
90-100 mesh；
Molybdenum disulfide fineness is in 90-100 mesh；
S120, petroleum coke, needle coke are put into calcining furnace, are passed through protection gas（Argon gas）, it is then heated to 1250-1350 DEG C,
It is kept for 0.5-1 hours, is calcined；
Calcined petroleum coke real density is not less than 2.07g/cm3, and resistivity is not more than 550 μ Ω .m；Needle coke real density is not small
In 2.12g/cm3, resistivity is not more than 500 μ Ω .m；
S130, petroleum coke calcined in S120, needle coke are crushed, fine grinding, make its partial size no more than 0.075 ㎜；
S140, by following components according to parts by weight than uniformly mixing, after S130 treated petroleum coke 10-12, S130 processing
Needle coke 4-8, modified coal asphalt 8-10.Wet mixing can be used when mixing, i.e., ethyl alcohol is added in mixing, until being uniformly mixed
It air-dries afterwards.This mode can be quick and be comprehensively uniformly mixed it.
S150, by S140, treated that raw material is stirred, and material temperature is increased to 200-300 DEG C, and stirring 1-2 is small
When；
S160, raw material mixed in S150 is put into press machine through 4-10MPa compacting；Squeeze time 180-220s, in advance
Bulk density is in 1.66g/cm after pressure3Left and right；
S170, by the raw material being compacted in S160 by the pressure compaction of 15-20MPa, keep 3-5min, vacuumize simultaneously；It compresses
Afterwards, bulk density is in 1.68g/cm3Left and right, S160 and the common compression ratio of S170 are controlled in 3-5；
S180, by treated in S170, raw material is put into extruder, the pressure for being heated to 150-180 DEG C and passing through 30-35MPa
It is squeezed, then cuts into section according to preset requirement and obtain green compact, be put into the water that temperature is 5-10 degrees Celsius after cutting into section
In cooled down, extrusion speed control in 120-180s/ root, green volume density is in 1.68g/cm3Left and right；
S190, the green compact in S180 are put into roaster, are filled with protection gas（Argon gas）, and the high-temperature roasting of 3000 DEG C of progress,
Specific heating mode is as follows：
- 400 DEG C of room temperature, 5 DEG C/h；
400-800 DEG C, 7 DEG C/h；
800-1300 DEG C, 5 DEG C/h；
1300-1600 DEG C, 3 DEG C/h；It is kept for 20-30 hours after reaching 1600 DEG C；
1600-2300,10 DEG C/h；
It 2300-3000 DEG C, freely heating up, control is being no more than 15 DEG C/h, it is kept for 100-120 hours after reaching 3000 DEG C,
Obtain graphite base.Can green compact be graphitized in this way, to reduce resistivity.
S200, molding
S210, the graphite base of S190 is crushed to the graphite base fine powder that partial size is not more than 0.07 ㎜, then by graphite base fine powder, second
Acetylene black, PVDF, NMP, molybdenum disulfide are uniformly mixed according to following weight fraction ratio：80-85：8-10：5-8：2-4：1-2；Then
It is put into graphite jig and is heated to 120-160 DEG C, after being kept for 2-4 hours, by the pressure pre-molding of 10-15MPa, obtain brick
Base；
The S210 adobe prepared is put into the mold of large molded machine, is heated to 150-200 DEG C, kept for 2-4 hours by S220
Afterwards, pass through the further compression moulding of 30-45Mpa pressure.Wherein S210 and S220 common compression ratio controls between 4-5.
S300, machining, by S220, treated that adobe is machined out, and until reaching pre-set dimension, that is, produces stone
Electrode ink.
Since the graphited temperature such as petroleum coke, pitch, needle coke is often at 2700 DEG C or more, but reach this temperature
A large amount of hole can be generated in graphite base afterwards, this undoubtedly will cause cracked inside graphite base and stress concentrate, after this is also
The main reason for its thermal shock resistance of phase is not high.
However if graphite base is difficult to be graphitized using 2700 DEG C of temperature below again, cause resistivity high, so that finished product
It is serious not up to standard.
Therefore, graphite base is graphitized by applicant by existing, and the mode being then pressed and molded can reach preferable
Finished product, and its thermal shock resistance is also relatively high.Meanwhile the adobe made before molding using acetylene black as conductive agent,
PVDF can effectively avoid as binder and also need repeated calcination, graphited process when making binder using pitch, while at
Product resistivity is also up to standard（National standard）.
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, bigger profit margin can be brought for enterprise, improves the competition of enterprise
Power.
Specific embodiment
Below with reference to embodiment, the invention will be further described：
Embodiment one
A kind of manufacturing process of high-heat resistance shock resistant graphite electrode, includes the following steps：
S100, ingredient
S110, raw material, petroleum coke, needle coke, coal tar pitch, acetylene black, PVDF（Polyvinyladine floride）,NMP（N- crassitude
Ketone）, molybdenum disulfide；
The petroleum coke is that low-sulfur is burnt；
The needle coke uses coal-based needle coke；
The softening point of the modified coal asphalt is 90-100 DEG C, and coking value is >=55%, and ash content≤0.20%, fineness exists when room temperature
90-100 mesh；
Molybdenum disulfide fineness is in 90-100 mesh；
S120, petroleum coke, needle coke are put into calcining furnace, are passed through protection gas（Argon gas）, 1300 DEG C are then heated to, is kept
It 0.5-1 hours, is calcined；
Calcined petroleum coke real density is not less than 2.07g/cm3, and resistivity is not more than 550 μ Ω .m；Needle coke real density is not small
In 2.12g/cm3, resistivity is not more than 500 μ Ω .m；
S130, petroleum coke calcined in S120, needle coke are crushed, fine grinding, make its partial size no more than 0.075 ㎜；
S140, by following components according to parts by weight than uniformly mixing, S130 treated petroleum coke 10, S130 treated needle
Shape coke 6, modified coal asphalt 9.Wet mixing can be used when mixing, i.e., ethyl alcohol is added in mixing, until air-drying after mixing i.e.
It can.This mode can be quick and be comprehensively uniformly mixed it.
S150, by S140, treated that raw material is stirred, and material temperature is increased to 260 DEG C, stirs 1-2 hours；
S160, raw material mixed in S150 is put into press machine through 8MPa compacting；Squeeze time 190s, volume after precompressed
Density is in 1.66g/cm3Left and right；
S170, by the raw material being compacted in S160 by the pressure compaction of 16MPa, keep 4min, vacuumize simultaneously；After compression, body
Product density is in 1.68g/cm3Left and right, S160 and the common compression ratio of S170 are controlled in 3-5；
S180, by treated in S170, raw material is put into extruder, is heated to 180 DEG C and is squeezed by the pressure of 30MPa
Then pressure cuts into section according to preset requirement and obtains green compact, be put into temperature after cutting into section to carry out in 5-10 degrees Celsius of water
Cooling, extrusion speed is controlled in 120-180s/ root, and green volume density is in 1.68g/cm3Left and right；
S190, the green compact in S180 are put into roaster, are filled with protection gas（Argon gas）, and the high-temperature roasting of 3000 DEG C of progress,
Specific heating mode is as follows：
- 400 DEG C of room temperature, 5 DEG C/h；
400-800 DEG C, 7 DEG C/h；
800-1300 DEG C, 5 DEG C/h；
1300-1600 DEG C, 3 DEG C/h；It is kept for 20-30 hours after reaching 1600 DEG C；
1600-2300,10 DEG C/h；
It 2300-3000 DEG C, 5 DEG C/h, is kept for 100 hours after reaching 3000 DEG C, obtains graphite base.It can make in this way
Green compact graphitization, to reduce resistivity.
S200, molding
S210, the graphite base of S190 is crushed to the graphite base fine powder that partial size is not more than 0.07 ㎜, then by graphite base fine powder, second
Acetylene black, PVDF, NMP, molybdenum disulfide are uniformly mixed according to following weight fraction ratio：82：9：7：3：1.4；It is then placed in graphite mo(u)ld
It is heated to 150 DEG C in tool, after being kept for 3 hours, by the pressure pre-molding of 15MPa, obtains adobe；
The S210 adobe prepared is put into the mold of large molded machine, is heated to 200 DEG C, after being kept for 4 hours, passes through by S220
The further compression moulding of 40Mpa pressure.Wherein S210 and S220 common compression ratio controls between 4-5.
S300, machining, by S220, treated that adobe is machined out, and until reaching pre-set dimension, that is, produces stone
Electrode ink.
Embodiment two
A kind of manufacturing process of high-heat resistance shock resistant graphite electrode, includes the following steps：
S100, ingredient
S110, raw material, petroleum coke, needle coke, coal tar pitch, acetylene black, PVDF（Polyvinyladine floride）,NMP（N- crassitude
Ketone）, molybdenum disulfide；
The petroleum coke is that low-sulfur is burnt；
The needle coke uses coal-based needle coke；
The softening point of the modified coal asphalt is 90-100 DEG C, and coking value is >=55%, and ash content≤0.20%, fineness exists when room temperature
90-100 mesh；
Molybdenum disulfide fineness is in 90-100 mesh；
S120, petroleum coke, needle coke are put into calcining furnace, are passed through protection gas（Argon gas）, 1350 DEG C are then heated to, keeps 1
Hour, it is calcined；
Calcined petroleum coke real density is not less than 2.07g/cm3, and resistivity is not more than 550 μ Ω .m；Needle coke real density is not small
In 2.12g/cm3, resistivity is not more than 500 μ Ω .m；
S130, petroleum coke calcined in S120, needle coke are crushed, fine grinding, make its partial size no more than 0.075 ㎜；
S140, by following components according to parts by weight than uniformly mixing, S130 treated petroleum coke 11, S130 treated needle
Shape coke 5, modified coal asphalt 8.Wet mixing can be used when mixing, i.e., ethyl alcohol is added in mixing, until air-drying after mixing i.e.
It can.This mode can be quick and be comprehensively uniformly mixed it.
S150, by S140, treated that raw material is stirred, and material temperature is increased to 300 DEG C, stirs 2 hours；
S160, raw material mixed in S150 is put into press machine through 6MPa compacting；Squeeze time 200s, volume after precompressed
Density is in 1.66g/cm3Left and right；
S170, by the raw material being compacted in S160 by the pressure compaction of 18MPa, keep 3min, vacuumize simultaneously；After compression, body
Product density is in 1.68g/cm3Left and right, S160 and the common compression ratio of S170 are controlled in 3-5；
S180, by treated in S170, raw material is put into extruder, the pressure for being heated to 150-180 DEG C and passing through 30-35MPa
It is squeezed, then cuts into section according to preset requirement and obtain green compact, be put into the water that temperature is 5-10 degrees Celsius after cutting into section
In cooled down, extrusion speed control in 120-180s/ root, green volume density is in 1.68g/cm3Left and right；
S190, the green compact in S180 are put into roaster, are filled with protection gas（Argon gas）, and the high-temperature roasting of 3000 DEG C of progress,
Specific heating mode is as follows：
- 400 DEG C of room temperature, 5 DEG C/h；
400-800 DEG C, 7 DEG C/h；
800-1300 DEG C, 5 DEG C/h；
1300-1600 DEG C, 3 DEG C/h；It is kept for 25 hours after reaching 1600 DEG C；
1600-2300,10 DEG C/h；
It 2300-3000 DEG C, 15 DEG C/h, is kept for 110 hours after reaching 3000 DEG C, obtains graphite base.It can make in this way
Green compact graphitization is obtained, to reduce resistivity.
S200, molding
S210, the graphite base of S190 is crushed to the graphite base fine powder that partial size is not more than 0.07 ㎜, then by graphite base fine powder, second
Acetylene black, PVDF, NMP, molybdenum disulfide are uniformly mixed according to following weight fraction ratio：84：8： 8：2：1；It is then placed in graphite jig
In be heated to 160 DEG C, after being kept for 4 hours, pass through the pressure pre-molding of 15MPa, obtain adobe；
The S210 adobe prepared is put into the mold of large molded machine, is heated to 180 DEG C, after being kept for 4 hours, passes through by S220
The further compression moulding of 45Mpa pressure.Wherein S210 and S220 common compression ratio controls between 4-5.
S300, machining, by S220, treated that adobe is machined out, and until reaching pre-set dimension, that is, produces stone
Electrode ink.
Place is not described in detail by the present invention, is the well-known technique 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 within the scope of protection determined by the claims.
Claims (5)
1. a kind of manufacturing process of high-heat resistance shock resistant graphite electrode, which is characterized in that include the following steps：
S100, ingredient
S110, raw material, petroleum coke, needle coke, coal tar pitch, acetylene black, PVDF, NMP, molybdenum disulfide；
S120, petroleum coke, needle coke are put into calcining furnace, are passed through protection gas, be then heated to 1250-1350 DEG C, kept
It 0.5-1 hours, is calcined；
S130, petroleum coke calcined in S120, needle coke are crushed, fine grinding, make its partial size no more than 0.075 ㎜；
S140, by following components according to parts by weight than uniformly mixing, after S130 treated petroleum coke 10-12, S130 processing
Needle coke 4-8, modified coal asphalt 8-10；
S150, by S140, treated that raw material is stirred, and material temperature is increased to 200-300 DEG C, stirs 1-2 hours；
S160, raw material mixed in S150 is put into press machine through 4-10MPa compacting；Squeeze time 180-220s, in advance
Bulk density is in 1.66g/cm after pressure3Left and right；
S170, by the raw material being compacted in S160 by the pressure compaction of 15-20MPa, keep 3-5min, vacuumize simultaneously；It compresses
Afterwards, bulk density is in 1.68g/cm3Left and right, S160 and the common compression ratio of S170 are controlled in 3-5；
S180, by treated in S170, raw material is put into extruder, the pressure for being heated to 150-180 DEG C and passing through 30-35MPa
It is squeezed, then cuts into section according to preset requirement and obtain green compact, be put into the water that temperature is 5-10 degrees Celsius after cutting into section
In cooled down, extrusion speed control in 120-180s/ root, green volume density is in 1.68g/cm3Left and right；
S190, the green compact in S180 are put into roaster, are filled with protection gas, and carry out 3000 DEG C of high-temperature roasting, obtain stone
Black base；
S200, molding
S210, the graphite base of S190 is crushed to the graphite base fine powder that partial size is not more than 0.07 ㎜, then by graphite base fine powder, second
Acetylene black, PVDF, NMP, molybdenum disulfide are uniformly mixed according to following weight fraction ratio：80-85：8-10：5-8：2-4：1-2；Then
It is put into graphite jig and is heated to 120-160 DEG C, after being kept for 2-4 hours, by the pressure pre-molding of 10-15MPa, obtain brick
Base；
The S210 adobe prepared is put into the mold of large molded machine, is heated to 150-200 DEG C, kept for 2-4 hours by S220
Afterwards, by the further compression moulding of 30-45Mpa pressure, wherein S210 and S220 common compression ratio is controlled between 4-5；
S300, machining, by S220, treated that adobe 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 each ingredient requirement is as follows in S110：The petroleum coke
For low-sulfur coke；
The needle coke uses coal-based needle coke；
The softening point of the modified coal asphalt is 90-100 DEG C, and coking value is >=55%, and ash content≤0.20%, fineness exists when room temperature
90-100 mesh；
Molybdenum disulfide fineness is in 90-100 mesh.
3. manufacturing process as described in claim 1, which is characterized in that in S120, calcined petroleum coke real density is not less than
2.07g/cm3 resistivity is not more than 550 μ Ω .m；Needle coke real density is not less than 2.12g/cm3, and resistivity is not more than 500 μ
Ω.m。
4. manufacturing process as described in claim 1, which is characterized in that in S140, ethyl alcohol is added in mixing, until mixing is equal
It is air-dried after even.
5. manufacturing process as described in claim 1, which is characterized in that in S190, the heating mode of roasting is as follows：
- 400 DEG C of room temperature, 5 DEG C/h；
400-800 DEG C, 7 DEG C/h；
800-1300 DEG C, 5 DEG C/h；
1300-1600 DEG C, 3 DEG C/h；It is kept for 20-30 hours after reaching 1600 DEG C；
1600-2300,10 DEG C/h；
It 2300-3000 DEG C, freely heats up, control is being no more than 15 DEG C/h, is kept for 100-120 hours after reaching 3000 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761609A (en) * | 2019-02-13 | 2019-05-17 | 合肥炭素有限责任公司 | A kind of manufacturing process and its process units of high-heat resistance shock resistant graphite electrode |
| CN110054495A (en) * | 2019-02-13 | 2019-07-26 | 合肥炭素有限责任公司 | A kind of novel graphite resistor rod manufacturing process and its manufacturing equipment |
| CN113241425A (en) * | 2021-06-03 | 2021-08-10 | 贵州民族大学 | Molybdenite electrode and preparation method thereof |
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| CN104119108A (en) * | 2014-08-08 | 2014-10-29 | 苏州宏久航空防热材料科技有限公司 | Method for preparing composite ceramic graphite electrode |
| CN108046803A (en) * | 2017-11-01 | 2018-05-18 | 大同新成新材料股份有限公司 | A kind of high strength graphite product and method for adding pitch coke production |
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