CN107311662A - A kind of graphite electrode nipple and preparation method thereof - Google Patents

A kind of graphite electrode nipple and preparation method thereof Download PDF

Info

Publication number
CN107311662A
CN107311662A CN201710372060.XA CN201710372060A CN107311662A CN 107311662 A CN107311662 A CN 107311662A CN 201710372060 A CN201710372060 A CN 201710372060A CN 107311662 A CN107311662 A CN 107311662A
Authority
CN
China
Prior art keywords
thickener
graphite electrode
carbon fiber
petroleum coke
electrode nipple
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710372060.XA
Other languages
Chinese (zh)
Inventor
张桂兰
杨远继
杨勇
武爱云
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fangda Carbon New Materials Technology Co Ltd
Original Assignee
Fangda Carbon New Materials Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fangda Carbon New Materials Technology Co Ltd filed Critical Fangda Carbon New Materials Technology Co Ltd
Priority to CN201710372060.XA priority Critical patent/CN107311662A/en
Publication of CN107311662A publication Critical patent/CN107311662A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B7/00—Heating by electric discharge
    • H05B7/02—Details
    • H05B7/10—Mountings, supports, terminals or arrangements for feeding or guiding electrodes
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • 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
    • 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

Abstract

A kind of graphite electrode nipple, it is made up of thickener and carbon fiber, thickener is formed by raw material petroleum coke with the binding agent liquid coal tar pitch kneading for accounting for the 34wt% of raw material petroleum coke 32, wherein raw material petroleum coke is divided into graphite electrode nipple powder petroleum coke and Graphite nipple petroleum coke aggregate, a part of binding agent liquid coal tar pitch is first obtained graphite electrode nipple thickener by the preparation method of thickener to be existing with graphite electrode nipple powder petroleum coke kneading, then thickener is obtained after addition Graphite nipple petroleum coke aggregate and remaining binding agent liquid coal tar pitch kneading are uniform in electrode contact thickener, carbon fiber is added in graphite electrode nipple thickener, the addition of wherein carbon fiber accounts for 0.01 2wt% of thickener weight.The characteristics of present invention has simple technique, excellent performance；Carbon fiber ultra high power joint bulk density ＜ 1.83g/cm3Rupture strength ＞ 25MPa, modulus of elasticity reduces joint single-steeping and a roasting technique process between 15 20GPa, therefore the graphite electrode nipple reduces in cost or realizes performance on the premise of being held essentially constant and is substantially improved, and simplifies technological process.

Description

A kind of graphite electrode nipple and preparation method thereof
Technical field
The invention belongs to materials science field, and in particular to a kind of graphite electrode nipple and preparation method thereof.
Background technology
Graphite electrode nipple is a vital connection parts during graphite electrode use, and joint is made steel in electrode When play the key effect of connection, the quality of joint quality is directly connected to use of the electrode in electric furnace steel making.Graphite electrode Bonding pad with joint formation is position electric, that hot, mechanical load is larger and complicated, is also the position of common fracture.According to relevant Data shows, in electric furnace steel making, and more than 80% electrode is fractureed using accident by joint or loosening and releasing is caused, domestic Production of the outer carbon industry to graphite electrode nipple is especially paid attention to.
At present, domestic graphite electrode nipple quality will be less than external product, and tracing it to its cause, it is upper mainly to be used in quality raw materials Difference, foreign countries' production graphite electrode nipple uses the difference on high-quality needle coke, raw material to cause its product in structural behaviour index Upper is difficult to be compared favourably with foreign countries.Domestic import needle coke is limited by quality and quantity, and the grade of the import needle coke used is not Height, performance is not good, and the domestic needle coke performance of only a few families is also far away from import needle coke.
So, how on the basis of existing material performance, high-grade graphite electrode nipple is produced, it is necessary to separately ward off footpath Footpath.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of graphite electrode nipple for shortcoming of the prior art, Graphite electrode nipple bulk density ＜ 1.83g/cm3, rupture strength ＞ 27MPa, modulus of elasticity is between 15-20GPa.
It is a further object of the present invention to provide the preparation method of above-mentioned graphite electrode nipple.
A kind of graphite electrode nipple, is made up of thickener and carbon fiber, and thickener is by raw material petroleum coke and accounts for raw material petroleum coke 32- 34wt% binding agent liquid coal tar pitch kneading is formed, and wherein raw material petroleum coke is divided into graphite electrode nipple powder petroleum coke and stone Black joint petroleum coke aggregate, the preparation method of thickener is to show a part of binding agent liquid coal tar pitch elder generation and graphite electrode nipple powder Work stone oil coke kneading obtains graphite electrode nipple thickener, then in electrode contact thickener add Graphite nipple petroleum coke aggregate and Thickener is obtained after remaining binding agent liquid coal tar pitch kneading is uniform, carbon fiber is added in graphite electrode nipple thickener, and wherein carbon is fine The addition of dimension accounts for the 0.01-2wt% of thickener weight.
The preparation method of above-mentioned graphite electrode nipple, using petroleum coke as base material, liquid coal tar pitch is binding agent, and addition carbon is fine Dimension, specific step is as follows：
（1）Chopped carbon fiber is immersed in Small molecule organic solvents and soaks 2-4 hours, wherein chopped carbon fiber and organic solvent Mass ratio be 1:3-10, makes carbon fiber wire all spread out in organic solvent, forms monofilament or the thread states of 2-3, pull out, Drain, organic solvent volatilizees, and obtains material carbon fiber；
（2）- 0.075mm graphite electrode nipple powder petroleum coke is heated to 110-130 DEG C in kneading pot, 150- is added 180 DEG C of liquid coal tar pitch, liquid coal tar pitch addition is the 25-30wt % of graphite electrode nipple powder Petroleum Coke, and Stirring kneading makes it uniformly be mixed to get graphite electrode nipple thickener；
（3）By step（1）Obtained material carbon fiber is added to step（2）In the uniform graphite electrode nipple thickener of kneading, mix It is 155-175 DEG C to pinch temperature, compound stirring kneading 10-20min；
（4）In step（3）2-0.002mm Graphite nipple petroleum coke aggregates, kneading 5- are added in material after kneading 10-20min 10min, is supplemented addition liquid coal tar pitch and obtains thickener, wherein step（2）、（4）The total addition of liquid coal tar pitch is raw material stone The 32-34 wt % of oil coke, step（2）The addition of middle carbon fiber accounts for step（4）The 0.01-2wt% of middle thickener weight, continues Kneading 30-40min, 155-175 DEG C of kneading temperature；
（5）By step（4）Obtained material, extrusion forming is into all size graphite electrode nipple green compact；
（6）By step（5）Obtained graphite electrode nipple green compact, carry out once roasting, after baking, three roastings or once roast Burn, after baking or be once calcined, then obtain final graphite product after being handled through graphitizable high temperature；
The step（6）Once roasting carried out in 420 hours roasting circular furnaces, roasting maximum temperature be 1200-1270 DEG C, Baking profile is；
After baking and three roastings are carried out in 1270 DEG C of circular furnaces or bogie-type furnace, and Baking profile is：
The step（1）Middle carbon fiber is the fine base carbon fibre of polypropylene or asphalt base carbon fiber, the length of chopped carbon fiber For 2-15mm.
The step（1）Small molecular organic solvent is methanol or ethanol, and purity reaches more than 90%,
Institute x states petroleum coke for coal-based needle coke or oil system needle coke；Binding agent liquid coal tar pitch is medium temperature coal pitch, the modification of middle temperature Coal tar pitch or modified coal tar pitch.
The step（1）Middle organic solvent is evaporated into below 3 wt %.
The graphite electrode nipple that the present invention is provided, is 75-79wt%, carbon fiber 0.5-3wt% by petroleum coke, constitutes, outside Plus above-mentioned raw materials 25-34wt% binding agent liquid coal tar pitch is bonding agent.The present invention has that technique is simple, the spy of excellent performance Point；Prepared carbon fiber ultra high power joint bulk density ＜ 1.83g/cm3, rupture strength ＞ 25MPa, modulus of elasticity exists Between 15-20GPa, joint single-steeping and a roasting technique process are reduced, therefore the graphite electrode nipple is in cost reduction Or realize performance on the premise of being held essentially constant and be substantially improved, simplify technological process.
Embodiment
Below in conjunction with specific specific embodiment, technical scheme is further described, but the present invention is simultaneously It is not limited to these embodiments.
Embodiment 1
A kind of graphite electrode nipple, is made up of thickener and carbon fiber, and thickener is by raw material petroleum coke and accounts for raw material petroleum coke 32wt% Binding agent liquid medium temperature coal pitch kneading form, wherein raw material petroleum coke is divided into graphite electrode nipple powder petroleum coke and graphite Joint petroleum coke aggregate, the preparation method of thickener is now by a part of binding agent liquid medium temperature coal pitch elder generation and graphite electrode nipple Powder petroleum coke kneading obtains graphite electrode nipple thickener, and Graphite nipple petroleum coke aggregate is then added in electrode contact thickener With remaining binding agent liquid medium temperature coal pitch kneading it is uniform after obtain thickener, carbon fiber is added in graphite electrode nipple thickener, its The addition of middle carbon fiber accounts for the 1wt% of thickener weight.
The preparation method of above-mentioned graphite electrode nipple, using petroleum coke as base material, liquid medium temperature coal pitch is binding agent, addition Carbon fiber, specific step is as follows：
（1）Chopped carbon fiber is immersed in Small molecule organic solvents methanol and soaked 3 hours, methanol purity reaches more than 90%, its The mass ratio of middle chopped carbon fiber and organic solvent methanol is 1:8, carbon fiber wire is all spread out in organic solvent, shape Into monofilament state, wherein carbon fiber is the fine base carbon fibre of polypropylene, and the length of chopped carbon fiber is 10mm, pulls out, drains, organic Solvent volatilizees, and organic solvent is evaporated into 1 wt %, obtains material carbon fiber；
（2）- 0.075mm graphite electrode nipple powder petroleum coke is heated to 110 DEG C in kneading pot, 150 DEG C of liquid is added State medium temperature coal pitch, liquid medium temperature coal pitch addition is the 28wt % of graphite electrode nipple powder Petroleum Coke, and stirs Kneading makes it uniformly be mixed to get graphite electrode nipple thickener；
（3）By step（1）Obtained material carbon fiber is added to step（2）In the uniform graphite electrode nipple thickener of kneading, mix It is 155 DEG C to pinch temperature, compound stirring kneading 20min；
（4）In step（3）Addition 2-0.002mm Graphite nipple petroleum coke aggregates in material after kneading 20min, kneading 10min, It is supplemented addition liquid medium temperature coal pitch kneading and obtains thickener, wherein step（2）、（4）The middle total addition of liquid medium temperature coal pitch For 32 wt % of raw material petroleum coke, wherein step（2）The addition of middle material carbon fiber accounts for step（4）Middle thickener weight 1wt%, continues kneading 40min, 155 DEG C of kneading temperature；
（5）By step（4）Obtained material, extrusion forming is into all size graphite electrode nipple green compact；
（6）By step（5）Obtained graphite electrode nipple green compact, carry out once roasting, after baking, three roastings wherein once Roasting is carried out in 420 hours roasting circular furnaces, and roasting maximum temperature is 1200-1270 DEG C, and Baking profile is；
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
1270 23 Constant temperature
After baking and three roastings are carried out in 1270 DEG C of circular furnaces, and Baking profile is：
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
Embodiment 2
A kind of graphite electrode nipple, is made up of thickener and carbon fiber, and thickener is by raw material petroleum coke and accounts for raw material petroleum coke 34wt% The middle temperature modified coal asphalt kneading of binding agent liquid form, wherein raw material petroleum coke be divided into graphite electrode nipple powder petroleum coke and Graphite nipple petroleum coke aggregate, the preparation method of thickener is now by the middle temperature modified coal asphalt elder generation of a part of binding agent liquid and graphite Electrode contact powder petroleum coke kneading obtains graphite electrode nipple thickener, and Graphite nipple stone is then added in electrode contact thickener Thickener is obtained after oil coke aggregate and the middle temperature modified coal asphalt pitch kneading of remaining binding agent are uniform, carbon fiber adds graphite electrode and connect In head thickener, the addition of wherein carbon fiber accounts for the 0.5wt% of thickener weight.
The preparation method of above-mentioned graphite electrode nipple, using petroleum coke as base material, the middle temperature modified coal asphalt of liquid is binding agent, Carbon fiber is added, specific step is as follows：
（1）Chopped carbon fiber is immersed in Small molecule organic solvents ethanol and soaked 4 hours, purity of alcohol reaches more than 90%, its The mass ratio of middle chopped carbon fiber and organic solvent methanol is 1:10, carbon fiber wire is all spread out in organic solvent, The thread states of 2-3 are formed, wherein carbon fiber is the fine base carbon fibre of polypropylene, and the length of chopped carbon fiber is 15mm, pull out, drain, Organic solvent volatilizees, and organic solvent is evaporated into 2 wt %, obtains material carbon fiber；
（2）- 0.075mm graphite electrode nipple powder petroleum coke is heated to 130 DEG C in kneading pot, 180 DEG C of liquid is added The middle temperature modified coal asphalt of state, the middle temperature modified coal asphalt addition of liquid is the 30wt of graphite electrode nipple powder Petroleum Coke %, and stirring kneading makes it uniformly be mixed to get graphite electrode nipple thickener；
（3）By step（1）Obtained material carbon fiber is added to step（2）In the uniform graphite electrode nipple thickener of kneading, mix It is 155 DEG C to pinch temperature, compound stirring kneading 20min；
（4）In step（3）Addition 2-0.002mm Graphite nipple petroleum coke aggregates in material after kneading 20min, kneading 10min, It is supplemented addition liquid medium temperature coal pitch kneading and obtains thickener, wherein step（2）、（4）The middle total addition of liquid medium temperature coal pitch For 34 wt % of raw material petroleum coke, wherein step（2）The addition of middle material carbon fiber accounts for step（4）Middle thickener weight 0.5wt%, continues kneading 40min, 175 DEG C of kneading temperature；
（5）By step（4）Obtained material, extrusion forming is into all size graphite electrode nipple green compact；
（6）By step（5）Obtained graphite electrode nipple green compact, carry out once roasting, after baking, wherein being once calcined Carried out in 420 hours roasting circular furnaces, roasting maximum temperature is 1200-1270 DEG C, and Baking profile is；
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
1270 23 Constant temperature
After baking is carried out in 1270 DEG C of bogie-type furnaces, and Baking profile is：
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
Embodiment 3
A kind of graphite electrode nipple, is made up of thickener and carbon fiber, and thickener is by raw material petroleum coke and accounts for raw material petroleum coke 34wt% Binding agent liquid coal tar pitch kneading form, wherein raw material petroleum coke is divided into graphite electrode nipple powder petroleum coke and Graphite nipple Petroleum coke aggregate, the preparation method of thickener is to show a part of binding agent liquid coal tar pitch elder generation and graphite electrode nipple powder oil Burnt kneading obtains graphite electrode nipple thickener, and Graphite nipple petroleum coke aggregate is then added in electrode contact thickener and residue is viscous Obtain thickener after knot agent liquid coal tar pitch kneading is uniform, carbon fiber is added in graphite electrode nipple thickener, wherein carbon fiber plus Enter the 2wt% that amount accounts for thickener weight.
The preparation method of above-mentioned graphite electrode nipple, using petroleum coke as base material, the middle temperature modified coal asphalt of liquid is binding agent, Carbon fiber is added, specific step is as follows：
（1）Chopped carbon fiber is immersed in Small molecule organic solvents ethanol and soaked 4 hours, purity of alcohol reaches more than 90%, its The mass ratio of middle chopped carbon fiber and organic solvent methanol is 1:10, carbon fiber wire is all spread out in organic solvent, The thread states of 2-3 are formed, wherein carbon fiber is asphalt base carbon fiber, and the length of chopped carbon fiber is 2mm, pull out, drain, You Jirong Agent is volatilized, and organic solvent is evaporated into 3 wt %, is obtained material carbon fiber；
（2）- 0.075mm graphite electrode nipple powder petroleum coke is heated to 130 DEG C in kneading pot, 180 DEG C of liquid is added The middle temperature modified coal asphalt of state, the middle temperature modified coal asphalt addition of liquid is the 25wt of graphite electrode nipple powder Petroleum Coke %, and stirring kneading makes it uniformly be mixed to get graphite electrode nipple thickener；
（3）By step（1）Obtained material carbon fiber is added to step（2）In the uniform graphite electrode nipple thickener of kneading, mix It is 175 DEG C to pinch temperature, compound stirring kneading 10min；
（4）In step（3）Addition 2-0.002mm Graphite nipple petroleum coke aggregates in material after kneading 20min, kneading 5min, It is supplemented adding the middle temperature modified coal asphalt of liquid, wherein step（2）、（4）The middle total addition of temperature modified coal asphalt of liquid is raw material 34 wt % of petroleum coke, wherein step（2）The addition of middle material carbon fiber accounts for step（4）The 2wt% of middle thickener weight, continues Kneading 30min, 175 DEG C of kneading temperature；
（5）By step（4）Obtained material, extrusion forming is into all size graphite electrode nipple green compact；
（6）By step（5）Obtained graphite electrode nipple green compact, are once calcined, and are calcined wherein being once calcined at 420 hours Carried out in circular furnace, roasting maximum temperature is 1200-1270 DEG C, and Baking profile is；
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
1270 23 Constant temperature
Embodiment 4
A kind of graphite electrode nipple, is made up of thickener and carbon fiber, and thickener is by raw material petroleum coke and accounts for raw material petroleum coke 34wt% Binding agent modified coal tar pitch kneading form, wherein raw material petroleum coke is divided into graphite electrode nipple powder petroleum coke and Graphite nipple stone Oil coke aggregate, the preparation method of thickener first mixes a part of binding agent modified coal tar pitch to be existing with graphite electrode nipple powder petroleum coke Pinch and obtain graphite electrode nipple thickener, Graphite nipple petroleum coke aggregate and remaining binding agent are then added in electrode contact thickener Thickener is obtained after modified coal tar pitch kneading is uniform, carbon fiber is added in graphite electrode nipple thickener, and the addition of wherein carbon fiber is accounted for The 0.01wt% of thickener weight.
The preparation method of above-mentioned graphite electrode nipple, using petroleum coke as base material, liquid modified coal tar pitch is binding agent, adds carbon Fiber, specific step is as follows：
（1）Chopped carbon fiber is immersed in Small molecule organic solvents ethanol and soaked 4 hours, purity of alcohol reaches more than 90%, its The mass ratio of middle chopped carbon fiber and organic solvent methanol is 1:10, carbon fiber wire is all spread out in organic solvent, The thread states of 2-3 are formed, wherein carbon fiber is asphalt base carbon fiber, and the length of chopped carbon fiber is 2mm, pull out, drain, You Jirong Agent is volatilized, and organic solvent is evaporated into 3 wt %, is obtained material carbon fiber；
（2）- 0.075mm graphite electrode nipple powder petroleum coke is heated to 130 DEG C in kneading pot, 180 DEG C of liquid is added State modified coal tar pitch, liquid modified coal tar pitch addition is the 25wt % of graphite electrode nipple powder Petroleum Coke, and stirs kneading It is set uniformly to be mixed to get graphite electrode nipple thickener；
（3）By step（1）Obtained material carbon fiber is added to step（2）In the uniform graphite electrode nipple thickener of kneading, mix It is 175 DEG C to pinch temperature, compound stirring kneading 10min；
（4）In step（3）Addition 2-0.002mm Graphite nipple petroleum coke aggregates in material after kneading 20min, kneading 5min, It is supplemented adding liquid modified coal tar pitch, wherein step（2）、（4）The total addition of liquid modified coal tar pitch is 34 wt of raw material petroleum coke %, wherein step（2）The addition of middle material carbon fiber accounts for step（4）The 0.01wt% of middle thickener weight, continues kneading 30min, 175 DEG C of kneading temperature；
（5）By step（4）Obtained material, extrusion forming is into all size graphite electrode nipple green compact；
（6）By step（5）Obtained graphite electrode nipple green compact, carry out once roasting, after baking, three roastings wherein once Roasting is carried out in 420 hours roasting circular furnaces, and roasting maximum temperature is 1200-1270 DEG C, and Baking profile is；
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
1270 23 Constant temperature
After baking and three roastings are carried out in 1270 DEG C of circular furnaces, and Baking profile is：
Temperature range（℃） Duration（h） Average heating speed（℃/h）
130-300 60 3.7
350-550 140 1.5
500-800 125 1.8
800-1000 35 5.7
1000-1200 30 6.7
1200-1270 7 10
Properties of sample is tested after graphite electrode nipple graphitization:
Sample prepared by each embodiment, its performance parameter is as shown in the table：
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in the spirit and principles in the present invention Within any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection.

Claims (7)

1. a kind of graphite electrode nipple, it is characterised in that：It is made up of thickener and carbon fiber, thickener is by raw material petroleum coke and accounts for raw material Petroleum coke 32-34wt% binding agent liquid coal tar pitch kneading is formed, and wherein raw material petroleum coke is divided into graphite electrode nipple powder Petroleum coke and Graphite nipple petroleum coke aggregate, the preparation method of thickener is now by a part of binding agent liquid coal tar pitch elder generation and graphite Electrode contact powder petroleum coke kneading obtains graphite electrode nipple thickener, and Graphite nipple stone is then added in electrode contact thickener Thickener is obtained after oil coke aggregate and remaining binding agent liquid coal tar pitch kneading are uniform, carbon fiber adds graphite electrode nipple thickener In, the addition of wherein carbon fiber accounts for the 0.01-2wt% of thickener weight.
2. a kind of preparation method of graphite electrode nipple according to claim 1, it is characterised in that：Using petroleum coke as base Material, liquid coal tar pitch is binding agent, adds carbon fiber, and specific step is as follows：
（1）Chopped carbon fiber is immersed in Small molecule organic solvents and soaks 2-4 hours, wherein chopped carbon fiber and organic solvent Mass ratio be 1:3-10, makes carbon fiber wire all spread out in organic solvent, forms monofilament or the thread states of 2-3, pull out, Drain, organic solvent volatilizees, and obtains material carbon fiber；
（2）- 0.075mm graphite electrode nipple powder petroleum coke is heated to 110-130 DEG C in kneading pot, 150- is added 180 DEG C of liquid coal tar pitch, liquid coal tar pitch addition is the 25-30wt % of graphite electrode nipple powder Petroleum Coke, and Stirring kneading makes it uniformly be mixed to get graphite electrode nipple thickener；
（3）By step（1）Obtained material carbon fiber is added to step（2）In the uniform graphite electrode nipple thickener of kneading, mix It is 155-175 DEG C to pinch temperature, compound stirring kneading 10-20min；
（4）In step（3）2-0.002mm Graphite nipple petroleum coke aggregates, kneading 5- are added in material after kneading 10-20min 10min, is supplemented addition liquid coal tar pitch and obtains thickener, wherein step（2）、（4）The total addition of liquid coal tar pitch is raw material stone The 32-34 wt % of oil coke, step（2）The addition of middle carbon fiber accounts for step（4）The 0.01-2wt% of middle thickener weight, continues Kneading 30-40min, 155-175 DEG C of kneading temperature；
（5）By step（4）Obtained material, extrusion forming is into all size graphite electrode nipple green compact；
（6）By step（5）Obtained graphite electrode nipple green compact, carry out once roasting, after baking, three roastings or once roast Burn, after baking or be once calcined, then obtain final graphite product after being handled through graphitizable high temperature.
3. a kind of preparation method of graphite electrode nipple according to claim 2, it is characterised in that：The step（6）'s Once it is calcined and is carried out in 420 hours roasting circular furnaces, roasting maximum temperature is 1200-1270 DEG C, and Baking profile is；
Temperature range（℃） Duration（h） Average heating speed（℃/h） 130-300 60 3.7 350-550 140 1.5 500-800 125 1.8 800-1000 35 5.7 1000-1200 30 6.7 1200-1270 7 10 1270 23 Constant temperature
After baking and three roastings are carried out in 1270 DEG C of circular furnaces or bogie-type furnace, and Baking profile is：
Temperature range（℃） Duration（h） Average heating speed（℃/h） 130-300 60 3.7 350-550 140 1.5 500-800 125 1.8 800-1000 35 5.7 1000-1200 30 6.7 1200-1270 7 10 1270 23 Constant temperature
4. a kind of preparation method of graphite electrode nipple according to Claims 2 or 3, it is characterised in that：The step（1） Middle carbon fiber is the fine base carbon fibre of polypropylene or asphalt base carbon fiber, and the length of chopped carbon fiber is 2-15mm.
5. a kind of preparation method of graphite electrode nipple according to claim 4, it is characterised in that：The step（1）In Small molecule organic solvents are methanol or ethanol.
6. a kind of preparation method of graphite electrode nipple according to claim 2 or 5, it is characterised in that：The petroleum coke For coal-based needle coke or oil system needle coke；Binding agent liquid coal tar pitch is medium temperature coal pitch, middle temperature modified coal asphalt or modification drip It is blue or green.
7. a kind of preparation method of graphite electrode nipple according to claim 6, it is characterised in that：The step（1）In Organic solvent is evaporated into below 3 wt %.
CN201710372060.XA 2017-05-24 2017-05-24 A kind of graphite electrode nipple and preparation method thereof Pending CN107311662A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710372060.XA CN107311662A (en) 2017-05-24 2017-05-24 A kind of graphite electrode nipple and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710372060.XA CN107311662A (en) 2017-05-24 2017-05-24 A kind of graphite electrode nipple and preparation method thereof

Publications (1)

Publication Number Publication Date
CN107311662A true CN107311662A (en) 2017-11-03

Family

ID=60181577

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710372060.XA Pending CN107311662A (en) 2017-05-24 2017-05-24 A kind of graphite electrode nipple and preparation method thereof

Country Status (1)

Country Link
CN (1) CN107311662A (en)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108249923A (en) * 2017-12-22 2018-07-06 中国平煤神马集团开封炭素有限公司 A kind of graphite electrode nipple thickener and preparation method thereof
CN108264367A (en) * 2017-12-22 2018-07-10 中国平煤神马集团开封炭素有限公司 A kind of enhancing Delanium connector
CN108285356A (en) * 2017-12-22 2018-07-17 中国平煤神马集团开封炭素有限公司 A kind of enhancing artificial graphite material
CN108558425A (en) * 2017-12-22 2018-09-21 中国平煤神马集团开封炭素有限公司 A kind of preparation method of enhancing artificial graphite material
CN108558426A (en) * 2017-12-22 2018-09-21 中国平煤神马集团开封炭素有限公司 A kind of preparation method of enhancing artificial graphite connector
CN108585861A (en) * 2018-03-22 2018-09-28 合肥炭素有限责任公司 A kind of electrode contact and preparation method thereof
CN109020547A (en) * 2018-09-03 2018-12-18 大同宇林德石墨设备股份有限公司 A kind of preparation method of the graphite electrode nipple containing graphene
CN109574669A (en) * 2018-11-30 2019-04-05 大同新成新材料股份有限公司 A kind of electrode contact preparation method for material adding graphite cathode material
CN109942308A (en) * 2019-04-26 2019-06-28 大同宇林德石墨设备股份有限公司 A kind of high-strength carbon fiber graphite electrode
CN110668819A (en) * 2019-10-28 2020-01-10 焦作市中州炭素有限责任公司 Short-flow high-power graphite electrode and production process
CN110769539A (en) * 2019-10-28 2020-02-07 焦作市中州炭素有限责任公司 Graphite electrode joint bolt and preparation method thereof
CN112457014A (en) * 2020-10-21 2021-03-09 大同宇林德石墨新材料股份有限公司 Ultrahigh-power graphite electrode joint and preparation process thereof
CN113816741A (en) * 2021-09-18 2021-12-21 邯郸市高精新材料科技有限公司 High-strength graphite product, preparation method and application
CN113816743A (en) * 2021-07-30 2021-12-21 开封平煤新型炭材料科技有限公司 High-strength graphite electrode joint preparation device and process
CN114751749A (en) * 2022-05-12 2022-07-15 永安市鼎丰碳素科技有限公司 Technological method for optimizing kneading effect
CN116041064A (en) * 2023-01-09 2023-05-02 济南万瑞炭素有限责任公司 Aggregate pretreatment prebaked anode and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698945A (en) * 2009-11-03 2010-04-28 中国铝业股份有限公司 Carbon-fiber reinforced cathode carbon block and preparation method thereof
CN103260282A (en) * 2013-05-24 2013-08-21 河北顺天电极有限公司 Enhanced composite graphite electrode and manufacturing and using method thereof
CN106498717A (en) * 2016-11-08 2017-03-15 长春工业大学 A kind of method that carbon fiber surface plates multiple layer metal
CN106631084A (en) * 2016-11-18 2017-05-10 吉林炭素有限公司 Graphite electrode connector and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698945A (en) * 2009-11-03 2010-04-28 中国铝业股份有限公司 Carbon-fiber reinforced cathode carbon block and preparation method thereof
CN103260282A (en) * 2013-05-24 2013-08-21 河北顺天电极有限公司 Enhanced composite graphite electrode and manufacturing and using method thereof
CN104837233A (en) * 2013-05-24 2015-08-12 河北顺天电极有限公司 Preparation method of enhanced type composite graphite electrode
CN106498717A (en) * 2016-11-08 2017-03-15 长春工业大学 A kind of method that carbon fiber surface plates multiple layer metal
CN106631084A (en) * 2016-11-18 2017-05-10 吉林炭素有限公司 Graphite electrode connector and preparation method thereof

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108249923A (en) * 2017-12-22 2018-07-06 中国平煤神马集团开封炭素有限公司 A kind of graphite electrode nipple thickener and preparation method thereof
CN108264367A (en) * 2017-12-22 2018-07-10 中国平煤神马集团开封炭素有限公司 A kind of enhancing Delanium connector
CN108285356A (en) * 2017-12-22 2018-07-17 中国平煤神马集团开封炭素有限公司 A kind of enhancing artificial graphite material
CN108558425A (en) * 2017-12-22 2018-09-21 中国平煤神马集团开封炭素有限公司 A kind of preparation method of enhancing artificial graphite material
CN108558426A (en) * 2017-12-22 2018-09-21 中国平煤神马集团开封炭素有限公司 A kind of preparation method of enhancing artificial graphite connector
CN108585861A (en) * 2018-03-22 2018-09-28 合肥炭素有限责任公司 A kind of electrode contact and preparation method thereof
CN109020547A (en) * 2018-09-03 2018-12-18 大同宇林德石墨设备股份有限公司 A kind of preparation method of the graphite electrode nipple containing graphene
CN109574669A (en) * 2018-11-30 2019-04-05 大同新成新材料股份有限公司 A kind of electrode contact preparation method for material adding graphite cathode material
CN109942308A (en) * 2019-04-26 2019-06-28 大同宇林德石墨设备股份有限公司 A kind of high-strength carbon fiber graphite electrode
CN110668819A (en) * 2019-10-28 2020-01-10 焦作市中州炭素有限责任公司 Short-flow high-power graphite electrode and production process
CN110769539A (en) * 2019-10-28 2020-02-07 焦作市中州炭素有限责任公司 Graphite electrode joint bolt and preparation method thereof
CN112457014A (en) * 2020-10-21 2021-03-09 大同宇林德石墨新材料股份有限公司 Ultrahigh-power graphite electrode joint and preparation process thereof
CN113816743A (en) * 2021-07-30 2021-12-21 开封平煤新型炭材料科技有限公司 High-strength graphite electrode joint preparation device and process
CN113816741A (en) * 2021-09-18 2021-12-21 邯郸市高精新材料科技有限公司 High-strength graphite product, preparation method and application
CN114751749A (en) * 2022-05-12 2022-07-15 永安市鼎丰碳素科技有限公司 Technological method for optimizing kneading effect
CN116041064A (en) * 2023-01-09 2023-05-02 济南万瑞炭素有限责任公司 Aggregate pretreatment prebaked anode and preparation method thereof
CN116041064B (en) * 2023-01-09 2023-08-29 济南万瑞炭素有限责任公司 Aggregate pretreatment prebaked anode and preparation method thereof

Similar Documents

Publication Publication Date Title
CN107311662A (en) A kind of graphite electrode nipple and preparation method thereof
CN104528725B (en) A kind of preparation method of magnetic carbon SiClx ceramic nanoparticle
CN110330350B (en) Preparation method of fiber-toughened alumina ceramic
CN103254440B (en) Method of preparing liquid anaerobic polyferrocarbosilane
CN101445233A (en) Manufacturing method of ultra high power graphite electrode with diameter no less than 550mm
CN107602125A (en) A kind of fine grained, high density, the preparation method of high purity graphite material
CN103086364A (en) Method for preparing high-strength ultra-high power graphite electrode
CN110511050A (en) A kind of polycrystalline silicon ingot or purifying furnace carbon fiber and graphite material and preparation method thereof
CN103396653A (en) Preparation method of graphene nanoplatelet/epoxy resin nanocomposite material
CN101602604A (en) A kind of blast furnace mud and method of manufacturing technology thereof
CN106757161A (en) Modified prebaked anode and preparation method thereof
CN108441244A (en) A kind of preparation method of mesocarbon microspheres and mesophase pitch
CN113788678A (en) Preparation method of high-strength prebaked anode
Fang et al. Improving the self-sintering of mesocarbon-microbeads for the manufacture of high performance graphite-parts
CN103014918B (en) Method for preparing coal-series general asphalt carbon fiber
CN105655003B (en) A kind of modified electrode paste and preparation method thereof
CN112694332B (en) Coal tar pitch quality-dividing treatment method for preparing nuclear graphite material
CN110204349A (en) A kind of carbon nano-tube modification enhancing graphite electrode and preparation method thereof
CN102260884B (en) Method for preparing blocky graphite anode with high density and low resistivity in short process
CN111548810A (en) Coke and preparation method and application thereof
CN116082041A (en) Graphite material with low thermal expansion coefficient and production method thereof
CN114853488B (en) Silicon carbide-based furnace eye repairing material and production process thereof
CN111960731B (en) Novel asphalt concrete and preparation process thereof
CN106403579B (en) A kind of method that mesophase pitch prepares high-quality needle coke electrode material
CN103849413B (en) Asphalt additive, modified pitch, and preparation method thereof, the preparation method of application and pitch carbide

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20171103