CN102364989A - Ultra-high power graphite electrode nipple with diameter of 318mm and production method thereof - Google Patents

Ultra-high power graphite electrode nipple with diameter of 318mm and production method thereof Download PDF

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Publication number
CN102364989A
CN102364989A CN2011101828044A CN201110182804A CN102364989A CN 102364989 A CN102364989 A CN 102364989A CN 2011101828044 A CN2011101828044 A CN 2011101828044A CN 201110182804 A CN201110182804 A CN 201110182804A CN 102364989 A CN102364989 A CN 102364989A
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high power
graphite electrode
roasting
weight
coal
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陈文来
季耀明
贾庆远
刘运平
李明杰
娄卫江
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Zhongping Energy & Chemical Group Of Kaifeng Carbon Co Ltd
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Zhongping Energy & Chemical Group Of Kaifeng Carbon Co Ltd
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Abstract

The invention relates to an ultra-high power graphite electrode nipple with the diameter of 318mm and a production method thereof. The ultra-high power graphite electrode nipple with the diameter of 318mm can be produced by using domestic coal series needle cokes with low main physical and chemical index true density and high thermal expansion coefficient and sulfur content to match with a large-size ultra-high power graphite electrode with the diameter of 600mm for use. Experiments prove that the volume density, rupture strength, resistivity and thermal expansion coefficient of the product can reach an international standard, and the problem that the domestic coal series needle cokes cannot be used for producing the large-size ultra-high power graphite electrode because the main physical and chemical index of the domestic coal series needle cokes is low is solved, therefore, the localization of main raw materials of the ultra-high power graphite electrode nipple is realized. According to the invention, production cost can be reduced and economic benefit is improved.

Description

A kind of diameter 318mm ultra high power graphite electrode joint and production method thereof
Technical field
The present invention relates to a kind of graphite electrode nipple and production method thereof, particularly diameter 318mm ultra high power graphite electrode joint and production method thereof.
Technical background
Ultra high power graphite electrode is similar with producing, and the primary raw material of ultra high power graphite electrode joint is a needle coke, and needle coke is divided into coal-based needle coke and oil is a needle coke.With oil is that needle coke is compared, and the nitrogenous sulfur content of coal-based needle coke is high, in the later stage high-temperature process, in 1400 ℃ to 2100 ℃ intervals, causes the product inflatable easily, cracks waste product; Because thermal coefficient of expansion is higher, the product thermal shock resistance there is considerable influence simultaneously.
Low owing to the coal-based needle coke granule strength except that above-mentioned reason; Mix pinch with the die mould process in each grain grade proportion of filling a prescription destroyed easily; Thereby the intensity to final products exerts an influence, and causes product the cracking and the phenomenon that fractures in following process and use, to occur.
In the world; Have only Japan to adopt big specification ultra high power graphite electrode of coal-based needle coke production and joint; With homemade coal-based needle coke contrast; It is burnt that Japan's producing coal is that the main physical and chemical index of needle coke is better than homemade coal measures, and its physical and chemical index reaches or is the relevant parameter of needle coke near oil to a certain extent.
In sum, the raw material needle coke has become the principal element that restriction China produces ultra high power graphite electrode and joint.
Summary of the invention
The object of the present invention is to provide a kind of diameter 318mm ultra high power graphite electrode joint and production method thereof; It can overcome the restriction of existing factor; Utilize main physical and chemical index real density on the low side; The homemade coal-based needle coke that thermal coefficient of expansion and sulfur-bearing nitrogen content are higher is produced ultra high power graphite resistor rod with 600 mm diameter with diameter 318mm graphite electrode nipple.The present invention can effectively reduce production costs, and increases economic efficiency, and the actual needs that use are satisfied in the requirement that product quality indicator is met international standards.
Product diameter 318mm ultra high power graphite electrode joint of the present invention is a raw material with homemade coal-based needle coke; Its concrete prescription comprises: 2mm-1mm granularity coal-based needle coke; 1mm-0.5mm the granularity coal-based needle coke, the siccative component that-0.075mm coal-based needle coke fine powder is formed; Binding agent modified coal tar pitch in order to bonding above-mentioned siccative component; The stearic acid of supplement production and brown iron oxide (Fe 2O 3) additive formed.This formula combination is if calculate by weight percentage; If above-mentioned siccative component total weight is 100%; Then the shared percentage by weight of 2mm-1mm granularity coal-based needle coke is 20%; 1mm-0.5mm the shared percentage by weight of granularity coal-based needle coke is 10%, the shared percentage by weight of-0.075mm coal-based needle coke fine powder is 70%, and binding agent modified coal tar pitch and its weight of siccative component contrast are the 40%-50% of siccative composition weight; Stearic acid weight in the additive is the 0.5%-1% of siccative composition weight, brown iron oxide (Fe 2O 3) weight is 0.5% of siccative composition weight.
Product processes of the present invention comprises following processing step:
1) the die mould stage:
With raw material coal-based needle coke crushing and screening to obtain required each the specification siccative component of filling a prescription; Get into after siccative is heated to 180-200 ℃ to mix and pinch pot; Add binding agent modified coal tar pitch, stearic acid and brown iron oxide additive; Under 180-200 ℃ of temperature, mix and pinch and kept 15 minutes, water spray is cooled to 130-140 ℃ and wakes up and stuck with paste 5 minutes, gets into press then.Press material cylinder temperature remains 120 ± 5 ℃, at this temperatures machine the entering material is vacuumized and makes firm by ramming, and vacuum degree≤22mmHg makes pressure 1100-1300 ton firm by ramming, and pumpdown time ≮ 3 minute are made pressure hold time ≮ 10 second firm by ramming.After making end firm by ramming material is extruded, squeeze pressure should maintain 900-1100 ton, extrusion speed ≯ 5mm/s.This stage resulting product is a raw product, and bulk density is not less than 1.78g/cm 3
2) the roasting stage
Above-mentioned raw product is carried out roasting heat through baking furnace handle, process comprises bakes to burn the article, single-steeping, after baking, double-steeping, three roastings, three dippings, four roastings.Said each roasting process all automatically performs according to each roasting curve; Roasting finishes the back product and is cooled to 300 ℃ and comes out of the stove, and after the shot-blasting machine Shot Blasting, gets into impregnation tank, through impregnating pitch after high temperature impregnation process under the 10-15bar pressure; Get into next roasting process, finish until four roastings.This stage resulting product is a roasting product.
3) the graphitization stage
Above-mentioned roasting product is handled through flush end, packed in the internal thermal serial formula graphitizing furnace with the mode of four post bundlings, send electric graphitization processing according to the power-supply curve of setting behind the covering and heat insulating material according to end to end principle.This stage resulting product is the graphitization article.
4) process segment
The finished product of regulatory specifications is processed in the specification requirement measurement according to the rules of above-mentioned graphitization article, and according to the rules coupling requires to assemble in advance, pack, put in storage with the ultra high power graphite electrode finished product again after quality index and size index detect.
Said roasting stage bakes to burn the article curve is following:
The bakes to burn the article curve
Figure BSA00000528964700021
Said roasting stage after baking, three roastings, four times the roasting curve is following:
Secondary, three times and four roasting curves
Figure BSA00000528964700022
Said graphitization stage graphitization curve is following:
The graphitization power-supply curve
Figure BSA00000528964700023
The present invention adopts technique scheme; The homemade coal-based needle coke that main physical and chemical index real density capable of using is on the low side, thermal coefficient of expansion and sulfur-bearing nitrogen content are higher is produced the big specification ultra high power graphite electrode of Φ 318mm and is used electrode nipple; Through detecting, the bulk density of this electrode nipple is 1.84g/cm 3, rupture strength is 11.70MPa, and modulus of elasticity is 7.56GPa, and resistivity is 4.5 μ Ω m, and thermal coefficient of expansion is 1.42X10 -6/ ℃, meet international standards.Thereby can solve that homemade coal-based needle coke is on the low side because of main physical and chemical index real density, thermal coefficient of expansion and the higher difficult problem that can't produce big specification ultra high power graphite electrode with electrode nipple of sulfur-bearing nitrogen content; And can realize of the production domesticization of big specification ultra high power graphite electrode with the primary raw material needle coke of electrode nipple; Simultaneously, China be can also solve effectively and China's carbon industry ultra high power graphite electrode production capacity and scale expansion problem seriously restricted because of the long-term dependence on import of raw material needle coke.Can reduce production costs, increase economic efficiency.
Product of the present invention is tested on probation on stove, non-cracking and other quality problems.
Description of drawings
Accompanying drawing is the process chart of diameter 318mm ultra high power graphite electrode with electrode nipple and production method thereof.
Embodiment
Specifically describe embodiment of the present invention in detail below in conjunction with instance.
Product of the present invention is to utilize the homemade coal-based needle coke of 100% Shanxi Hong Te to be raw material; Microstructure, real density, thermal coefficient of expansion, tap density, crushing strength according to this raw material; And the oil absorbency of this coal-based needle coke, design the prescription of satisfactory ultra high power graphite electrode with electrode nipple.This prescription comprises 2mm-1mm granularity coal-based needle coke, 1mm-0.5mm granularity coal-based needle coke, the siccative component that-0.075mm coal-based needle coke fine powder is formed; Binding agent modified coal tar pitch in order to bonding above-mentioned siccative component; The stearic acid of supplement production and brown iron oxide (Fe 2O 3) additive formed.This prescription counts 100% with needle coke siccative component; Then calculate 2mm-1mm granularity coal-based needle coke 20% then, 1mm-0.5mm granularity coal-based needle coke 10% according to percentage by weight;-0.075mm coal-based needle coke fine powder 70%; Binding agent modified coal tar pitch 40%-50%, stearic acid 0.5%-1%, brown iron oxide (Fe 2O 3) 0.5%.
Production method of the present invention comprises following processing step:
1) the die mould stage
The raw material coal-based needle coke is broken through jaw crusher, biconjugate roll crusher and Suspension roller flour mill, the required 2mm-1mm granularity coal-based needle coke that obtains after the screening filling a prescription, 1mm-0.5mm granularity coal-based needle coke;-0.075mm coal-based needle coke fine powder is sent into automatic batching system according to formula rate each granularity coal-based needle coke after with above-mentioned screening again, carries out automatic mix to obtain siccative; This siccative is discharged into Ai Li permitted mixes and to pinch pot after preheater is heated to 180-200 ℃, add binding agent modified coal tar pitch and stearic acid and the brown iron oxide additive of formula ratio after the dissolving of formula ratio again, mixedly under 180-200 ℃ of temperature pinch and kept 15 minutes; Mix and pinch into thickener; Wake up after thickener water spray is cooled to 130-140 ℃ and stuck with paste 5 minutes, enter 3000 tons upright smashing to crouch squeeze hydraulic presses, this hydraulic press vacuumizes and makes firm by ramming in advance under the thermal thermal temperature of design; Vacuum degree≤22mmHg; Make pressure 1100-1300 ton firm by ramming, pumpdown time ≮ 3 minute are made pressure hold time ≮ 10 second firm by ramming.After making end firm by ramming material is extruded, squeeze pressure should maintain 900-1100 ton, extrusion speed ≯ 5mm/s.This stage resulting product is a raw product, and bulk density is not less than 1.78g/cm 3, raw product obtains to meet the electrode green compact of specification requirement after shearing.
2) the roasting stage
9 one on above-mentioned electrode green compact are assembled into special roasting pot; Inserts is laid in specification requirement according to inserts is laid in roasting pot; Reaching the purpose of secluding air and uniformly transfer heat, tinning finishes the back and is pushed by waggon and carry out roasting heat in the formula baking furnace at the bottom of the car and handle, and carries out according to setting the roasting curve in this heat treatment process; Intensification finishes to naturally cool to normal temperature after the back water spray is cooled to 300 ℃ comes out of the stove, and accomplishes the bakes to burn the article operation.Product carries out Shot Blasting through shot-blasting machine behind the bakes to burn the article; Send in the impregnation tank; Use impregnating pitch to carry out carrying out after baking according to the after baking curve after high-pressure impregnation is handled, then obtain the after baking product, after above-mentioned ball blast and impregnation process, carry out three again and burn operations at 10-15bar; Finish until four calcining process by that analogy, the electrode that obtains to conform to quality requirements is joined the burning article.
3) the graphitization stage
Above-mentioned electrode baking article are handled the back through flush end packs in the internal thermal serial graphitized stove of " П " shape with the form of four post bundlings according to end to end principle; Energising heats up behind the covering and heat insulating material; Power-supply curve according to setting carries out graphitization processing, and processing finishes after detect the graphitization article that obtain meeting technical specification.
4) process segment
Above-mentioned graphitization article through numerical control machine tool, are processed into diameter 318mm standard specification electrode nipple finished product, after index and size detection, require to assemble in advance, pack, put in storage according to required precision and index coupling with diameter 600mm electrode body.
The present invention is through the inner detection of industry, and the bulk density of said electrode nipple is 1.84g/cm 3, rupture strength is 11.70MPa, and modulus of elasticity is 7.56GPa, and resistivity is 4.5 μ Ω m, and thermal coefficient of expansion is 1.42X10 -6/ ℃, meet international standards.

Claims (5)

1. a diameter 318mm ultra high power graphite electrode joint comprises 2mm-1mm granularity coal-based needle coke, 1mm-0.5mm granularity coal-based needle coke, the siccative component that-0.075mm coal-based needle coke fine powder is formed; Binding agent modified coal tar pitch in order to bonding above-mentioned siccative component; The stearic acid of supplement production and brown iron oxide (Fe 2O 3) additive formed.This formula combination is if calculate by weight percentage; If above-mentioned siccative component total weight is 100%; Then the shared percentage by weight of 2mm-1mm granularity coal-based needle coke is 20%; 1mm-0.5mm the shared percentage by weight of granularity coal-based needle coke is 10%, the shared percentage by weight of-0.075mm coal-based needle coke fine powder is 70%, and binding agent modified coal tar pitch and its weight of siccative component contrast are the 40%-50% of siccative composition weight; Stearic acid weight in the additive is the 0.5%-1% of siccative composition weight, brown iron oxide (Fe 2O 3) weight is 0.5% of siccative composition weight.
2. the production method of diameter 318mm ultra high power graphite electrode joint as claimed in claim 1 is characterized in that this production method comprises following processing step:
1) the die mould stage: with raw material coal-based needle coke crushing and screening to obtain according to claim 1 a specification granularity siccative component; By the said percentage by weight prescription of claim 1 the siccative component is prepared burden in automatic batching system; Be discharged into after then the siccative component being heated to 180-200 ℃ to mix and pinch pot, add binding agent modified coal tar pitch, stearic acid and brown iron oxide (Fe 2O 3) additive formed, under 180-200 ℃ of temperature, mix pinch and keep 15 minutes then water spray be cooled to 130-140 ℃ and wake up and stuck with paste 5 minutes, get into press afterwards.Press material cylinder temperature remains 120 ± 5 ℃, at this temperatures machine the entering material is vacuumized and makes firm by ramming, and vacuum degree≤22mmHg makes pressure 1100-1300 ton firm by ramming, and pumpdown time ≮ 3 minute are made pressure hold time ≮ 10 second firm by ramming.After making end firm by ramming material is extruded, squeeze pressure should maintain 900-1100 ton, extrusion speed ≯ 5mm/s.This stage resulting product is a raw product, and bulk density is not less than 1.78g/cm 3
2) the roasting stage: above-mentioned raw product is carried out roasting heat through baking furnace handle, process comprises bakes to burn the article, single-steeping, after baking, double-steeping, three roastings, three dippings, four roastings.Said each roasting process all automatically performs according to each roasting curve; Roasting finishes the back product and is cooled to 300 ℃ and comes out of the stove, and after the shot-blasting machine Shot Blasting, gets into impregnation tank, through impregnating pitch after high temperature impregnation process under the 10-15bar pressure; Get into next roasting process, finish until four roastings.This stage resulting product is a roasting product.
3) the graphitization stage: above-mentioned roasting product is handled through flush end, packed in the internal thermal serial formula graphitizing furnace with the mode of four post bundlings, send electric graphitization processing according to the power-supply curve of setting behind the covering and heat insulating material according to end to end principle.This stage resulting product is the graphitization article.
4) process segment: the finished product of regulatory specifications is processed in the specification requirement measurement according to the rules of above-mentioned graphitization article, and according to the rules coupling requires to assemble in advance, pack, put in storage with the ultra high power graphite electrode finished product again after quality index and size index detect.
3. the production method of diameter 318mm ultra high power graphite electrode joint as claimed in claim 2 is characterized in that described bakes to burn the article curve is following:
The bakes to burn the article curve
4. the production method of diameter 318mm ultra high power graphite electrode joint as claimed in claim 2 is characterized in that described after baking, and three roastings and four roasting curves are following:
Secondary, three times and four roasting curves
Figure FSA00000528964600021
5. the production method of diameter 318mm ultra high power graphite electrode joint as claimed in claim 2 is characterized in that described graphitization power-supply curve is following:
The graphitization power-supply curve
Figure FSA00000528964600022
CN2011101828044A 2011-07-01 2011-07-01 Ultra-high power graphite electrode nipple with diameter of 318mm and production method thereof Pending CN102364989A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103043656A (en) * 2012-12-19 2013-04-17 中国平煤神马集团开封炭素有限公司 Method for manufacturing ultra-high power graphite electrode joint by using asphalt additive
CN106744919A (en) * 2017-01-17 2017-05-31 韩俊培 A kind of production technology of polycrystalline silicon base plate special graphite
CN107846744A (en) * 2017-11-24 2018-03-27 吉林炭素有限公司 A kind of graphite electrode nipple method for determining dimension based on normal temperature processing, applied at elevated temperature
CN107986269A (en) * 2017-12-22 2018-05-04 中国平煤神马集团开封炭素有限公司 A kind of internal thermal serial graphitized technique of ultrahigh power graphite electrode joint
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
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
CN111943187A (en) * 2020-08-21 2020-11-17 合肥炭素有限责任公司 Ultrahigh-power graphite electrode 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
CN113372118A (en) * 2020-04-14 2021-09-10 吉林市高科特种炭素材料有限责任公司 Preparation method of special graphite material
CN113860874A (en) * 2021-08-23 2021-12-31 吉林炭素有限公司 Design method for dry material grain composition in graphite electrode joint formula
CN116253566A (en) * 2023-03-14 2023-06-13 山东亿维新材料有限责任公司 Needle-shaped Jiao Jipei formula for preparing high-quality graphite electrode and preparation method

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103043656A (en) * 2012-12-19 2013-04-17 中国平煤神马集团开封炭素有限公司 Method for manufacturing ultra-high power graphite electrode joint by using asphalt additive
CN106744919A (en) * 2017-01-17 2017-05-31 韩俊培 A kind of production technology of polycrystalline silicon base plate special graphite
CN107846744A (en) * 2017-11-24 2018-03-27 吉林炭素有限公司 A kind of graphite electrode nipple method for determining dimension based on normal temperature processing, applied at elevated temperature
CN107986269A (en) * 2017-12-22 2018-05-04 中国平煤神马集团开封炭素有限公司 A kind of internal thermal serial graphitized technique of ultrahigh power graphite electrode joint
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
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
CN113372118A (en) * 2020-04-14 2021-09-10 吉林市高科特种炭素材料有限责任公司 Preparation method of special graphite material
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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
CN113860874A (en) * 2021-08-23 2021-12-31 吉林炭素有限公司 Design method for dry material grain composition in graphite electrode joint formula
CN116253566A (en) * 2023-03-14 2023-06-13 山东亿维新材料有限责任公司 Needle-shaped Jiao Jipei formula for preparing high-quality graphite electrode and preparation method

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Application publication date: 20120229