CN100590231C - Preparation method for moulding fine structure graphite anode - Google Patents
Preparation method for moulding fine structure graphite anode Download PDFInfo
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- CN100590231C CN100590231C CN200710090789A CN200710090789A CN100590231C CN 100590231 C CN100590231 C CN 100590231C CN 200710090789 A CN200710090789 A CN 200710090789A CN 200710090789 A CN200710090789 A CN 200710090789A CN 100590231 C CN100590231 C CN 100590231C
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Abstract
The invention discloses a method for preparing a moulding fine-texture graphite anode. The main technological process is as follows: high-quality calcined petroleum coke is selected; the compositionsof superfine abrasive dust and small particles are adopted; after dry mixing of graphite scraps and the calcined petroleum coke, high-quality medium coal tar pitch is added; under certain temperatureand pressure, cold compression moulding forming is performed in a special die by utilization of a double-sided press machine after kneading, flaking and secondary milling; roasting is then performed and a manufactured product is guaranteed to have no crack; the density of the product is improved through dipping treatment of the coal tar pitch and then a finished product is obtained through reduction of the specific resistance and purification treatment during the graphitizing process. The graphite anode produced by the preparation method has high density, low specific resistance, low anisotropism ratio, a compact and uniform internal structure, low porosity and low ash content, and has certain mechanical strength and thermal shock resistance.
Description
Technical field
The present invention relates to a kind of preparation method of graphite anode, refer in particular to the preparation method of the graphite anode that uses in the re metal electrolyzing stove.
Background technology
Smelt rare earth special graphite anode and belong to nonmetal field new tool material, be mainly used in and make anode in the electrolytic furnace of electrolysis rare earth metal and use.The re metal electrolyzing stove is to add the iron cover by a plumbago crucible to make, put into rare-earth oxide in the crucible, insert the tungsten bar energising above and make negative electrode, the arc graphite product that four quadrntnt tubes of crucible wall suspension surround plays conduction and reductive action as anode, it makes, and carbon atom reacts in Sauerstoffatom in the rare-earth oxide and the graphite anode, displaces rare earth metal simple substance or alloy.So, smelt rare earth special graphite anode and belong to a kind of continuous consumption material.Require in smelting that graphite anode impurity is few, long service life, unit consumption is few, output is big, so that with the lower high-quality rare earth metal of cost output.Like this, for graphite anode, just require higher density, lower than resistance, anisotropy ratio is little, internal structure is fine and closely woven evenly, void content is little, ash content lacks, have characteristics such as certain physical strength and heat-shock resistance.
The smelting rare earth special graphite anode of Chu Shouing mostly is waste and old electrode greatly and processes through mechanical cutting in the market, its quality instability, particles of aggregates is big, redox reaction is incomplete, consumption is big, the final product carbon residue content often exceeds standard, and other impurity also may exceed standard.Another part graphite anode is the extrusion molding product, and its internal structure is inhomogeneous, than big, and torsional deformation, not anti-consumption easily also need mechanical workout and cause cost to strengthen to abnormity for each.In addition, the arc graphite anode two-end thickness made from above-mentioned way is identical, embeds suspension system one end, can making wherein in electrolytic solution too early, the iron tool exposes, monoblock anodic lower end can't be re-used because of having little time that redox reaction takes place, cause waste, increased consumption.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of moulding fine structure graphite anode, this preparation method consumes the characteristics designing mould according to the type of furnace of smelting the rare earth electrolytic furnace and anodic oxidation, make product inlay suspension system one end and under the situation that does not influence internal structure, do suitably thickening, adopt super fine powder, fine particle prescription, two-sided compression molding method compression moulding and add soak once, again through greying and purifying technique, make product reach high-purity, highly dense, finestructure, low resistivity, low consumed target.
The technical problem to be solved in the present invention is realized by following scheme: the preparation method of moulding fine structure graphite anode is characterized in that: with true density 2.08g/cm
3More than, broken in the after-smithing petroleum coke warp of ash content below 0.5%, make 0.8mm-0.5mm behind the super fine powder, 0.5mm-0.15mm, 0.15mm-0.075mm the superfine powder that the pellet of three grades and 0.075mm are following, make its purity reach 65%-80%, the weight ratio of four grades of above-mentioned after-smithing petroleum coke is accounted for 13%-15% by 0.8mm-0.5mm, 0.5mm-0.15mm account for 9%-11%, 0.15mm-0.075mm account for 18%-20%, 0.075mm following superfine powder accounts for the 54%-60% proportioning, mix with broken the doing of graphite through 20 minutes-30 minutes, be heated to 100 ℃-120 ℃ and become siccative, the broken weight of graphite accounts for 10%-20% in the siccative, after-smithing petroleum coke weight accounts for 80%-90%, add siccative weight 30%-40% again, softening temperature is at 80 ℃-90 ℃ medium temperature coal pitch, carrying out under 160 ℃-180 ℃ pressurizeed to mix in 20 minutes-30 minutes pinches, carry out secondary then and roll sheet, the powder of regrinding becomes the following particle weight of 0.075mm to account for the homogenous superfine powder of 60%-80%, by the compression moulding of match plate pattern pressing machine, guarantee that the volume density of stampings reaches 1.55g/cm
3More than, per hour heating up 2 ℃-3 ℃ at crucial warm area during roasting, the highest flame temperature roasting to 1250 ℃ guarantees that roasting product is indeformable, does not ftracture, and makes volume density reach 1.52g/cm
3More than, be controlled at below the 40 μ Ω m than resistance, again with coal-tar pitch dipping, guarantee the pickled product weightening finish more than 18%, roasting to 1250 ℃ again guarantees the close 1.70g/cm that reaches of re-baking product volume
3More than, under 2500 ℃ of temperature, make carbon goods greying and purification through graphitizing furnace, make the graphite anode product.Small product size density reaches 1.68g/cm
3More than, be controlled at below the 7 μ Ω m than resistance.
Advantage of the present invention is:
1, in the design process of this preparation method processing route, selects the high-quality after-smithing petroleum coke for use and the medium temperature coal pitch ash content is little, density is high, graphitization characteristic is good, the product purity height of producing, every good physical and chemical properties.Adopt super fine powder, small-particle prescription, make the not super 0.8mm of largest particle, smallest particles is below 0.075mm, and pinch through full and uniform mix of pressurizeing with coal-tar pitch, can make goods internal structure homogeneous, densification, defective is little, intergranular crack pore is few, gas permeability is low, and anisotropy ratio is little, density height, anti-consumption.
2, adopt two-sided compression molding method, guaranteed that the goods internal density is even; According to type of furnace designing mould, make final product not need the mechanical workout operation, provide cost savings; When designing mould, make the suspended end thickening, prevented from the product lower end to be utilized fully because of suspension system is exposed to electrolysis liquid surface too early, cause waste and cost to increase.
When 3, formulating the roasting curve,, per hour heat up not super 2-3 ℃ in the fugitive constituent discharge phase, making coal-tar pitch even charing in goods is net distribution, and is combined into valence bond with after-smithing petroleum coke, and graphite microcrystal is physically well developed, suppress built-in thermal stress simultaneously, prevent that crackle from producing.
4, flood and again roasting handle, can further reduce void content, improve product volume density, reduce than resistance enhance mechanical strength.
5, carry out graphitization processing, change the goods internal structure, promote graphite microcrystal to grow up, promote the product physicochemical property, reduce, realize that redox reaction is evenly abundant, reduce consuming, and can make product obtain purifying, increase carbon content than resistance.
This graphite anode product can use through behind the graphitization process, does not need mechanical workout, has reduced cost.This preparation method's innovative point is to adopt super fine powder, and the fine particle prescription carries out the cold forming moulding in special mould; Difficult point is to guarantee the after-smithing petroleum coke pellet, and powder and coal-tar pitch fully mix to be pinched evenly, guarantees stampings, and roasting product does not ftracture, the yield rate height.
The graphite anode performance index of product technologies that this preparation method produces can reach leading domestic level, through looking into new domestic beyond example, now the performance index of product technologies and domestic like product technical indicator is compared as follows:
The domestic similar advanced technical target of the product of this graphite anode product index
Purity: 〉=99% 〉=97%
Volume density: 〉=1.68g/cm
3〉=1.58g/cm
3
Than resistance :≤7 μ Ω m≤8.5 μ Ω m
Single cover elapsed time: 72 hours-80 hours 40 hours-50 hours
Description of drawings
Fig. 1 is this preparation method's a process flow sheet
Embodiment
One embodiment is described in detail in detail below: specification is 1/4 (φ 350mm-φ 180mm) * 400mm.True density is reached 2.08g/cm
3More than, the high-quality after-smithing petroleum coke of ash content below 0.5% through in make 0.8mm-0.5mm, 0.5mm-0.15mm, the pellet of three grades of 0.15mm-0.075mm and the superfine powder below the 0.075mm behind broken, the super fine powder, make its purity all reach 70%.According to the broken 130kg of the following graphite of 0.8mm, after-smithing petroleum coke 600kg proportioning.Wherein each grade of after-smithing petroleum coke is pressed 0.8mm-0.5mm 78kg, 0.5mm-0.15mm60kg, the following superfine powder 348kg proportioning of 0.15mm-0.075mm114kg, 0.075mm.Broken the doing through 30 minutes of each after-smithing petroleum coke and graphite mixed, and being heated to 120 ℃ becomes siccative.Add softening temperature again at 80 ℃-90 ℃ medium temperature coal pitch 270kg, under 170 ℃, carrying out pressurization in 20 minutes and mixing and pinches, carry out then that secondary rolls sheet, the powder of regrinding becomes the following particle of 0.075mm to account for 70% homogenous superfine powder, by the compression moulding of match plate pattern pressing machine.The volume density that guarantees stampings reaches 1.55g/cm
3More than, per hour heating up 2 ℃ at crucial warm area during roasting, the highest flame temperature roasting to 1250 ℃ guarantees that roasting product is indeformable, does not ftracture, and makes volume density reach 1.53g/cm
3More than, be controlled at below the 40 μ Ω m than resistance.With coal-tar pitch dipping, guarantee the pickled product weightening finish more than 18% again, roasting to 1250 ℃ again guarantees the close 1.70g/cm that reaches of re-baking product volume
3More than, under 2500 ℃ of temperature, make carbon goods greying and purification through graphitizing furnace, make the graphite anode product.Small product size density reaches 1.68g/cm
3More than, be controlled at below the 7 μ Ω m than resistance.An end external diameter 350mm in the die design, internal diameter 160mm, even transition is external diameter 350mm in 110mm length, internal diameter 180mm is until the other end.
Claims (1)
1, the preparation method of moulding fine structure graphite anode is characterized in that: with true density 2.08g/cm
3More than, broken in the after-smithing petroleum coke warp of ash content below 0.5%, make 0.8mm-0.5mm behind the super fine powder, 0.5mm-0.15mm, 0.15mm-0.075mm the superfine powder that the pellet of three grades and 0.075mm are following, make its purity reach 65%-80%, the weight ratio of four grades of above-mentioned after-smithing petroleum coke is accounted for 13%-15% by 0.8mm-0.5mm, 0.5mm-0.15mm account for 9%-11%, 0.15mm-0.075mm account for 18%-20%, 0.075mm following superfine powder accounts for the 54%-60% proportioning, mix with broken the doing of graphite through 20 minutes-30 minutes, be heated to 100 ℃-120 ℃ and become siccative, the broken weight of graphite accounts for 10%-20% in the siccative, after-smithing petroleum coke weight accounts for 80%-90%, add siccative weight 30%-40% again, softening temperature is at 80 ℃-90 ℃ medium temperature coal pitch, carrying out under 160 ℃-180 ℃ pressurizeed to mix in 20 minutes-30 minutes pinches, carry out secondary then and roll sheet, the powder of regrinding becomes the following particle weight of 0.075mm to account for the homogenous superfine powder of 60%-80%, by the compression moulding of match plate pattern pressing machine, guarantee that the volume density of stampings reaches 1.55g/cm
3More than, the crucial warm area in the fugitive constituent discharge phase during roasting per hour heats up 2 ℃-3 ℃, and the highest flame temperature roasting to 1250 ℃ guarantees that roasting product is indeformable, does not ftracture, and makes volume density reach 1.52g/cm
3More than, be controlled at below the 40 μ Ω m than resistance, again with coal-tar pitch dipping, guarantee the pickled product weightening finish more than 18%, roasting to 1250 ℃ again guarantees the close 1.70g/cm that reaches of re-baking product volume
3More than, under 2500 ℃ of temperature, make carbon goods greying and purification through graphitizing furnace, make the graphite anode product.
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| CN200710090789A CN100590231C (en) | 2007-04-09 | 2007-04-09 | Preparation method for moulding fine structure graphite anode |
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| CN200710090789A CN100590231C (en) | 2007-04-09 | 2007-04-09 | Preparation method for moulding fine structure graphite anode |
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| CN100590231C true CN100590231C (en) | 2010-02-17 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101748441B (en) * | 2010-01-25 | 2011-03-16 | 冯乃祥 | Method and device for preparing high-density aluminium cell anode carbon block green body |
| CN102260884B (en) * | 2010-07-12 | 2013-08-28 | 华东理工大学 | Method for preparing blocky graphite anode with high density and low resistivity in short process |
| CN102206080B (en) * | 2011-05-05 | 2012-06-06 | 大同新成新材料股份有限公司 | Graphite material for monocrystalline silicon growth thermal field in solar photovoltaic industry and production method thereof |
| CN102268697B (en) * | 2011-05-16 | 2013-11-27 | 方大炭素新材料科技股份有限公司 | Graphite anode for magnesium electrolysis and preparation method thereof |
| CN103397350A (en) * | 2013-08-06 | 2013-11-20 | 江西稀有金属钨业控股集团有限公司 | Special-shaped graphite anode |
| CN103482600A (en) * | 2013-09-06 | 2014-01-01 | 济南澳海炭素有限公司 | Quick temperature-rise heating method and device of carbon anode product dry materials |
| CN103820815A (en) * | 2013-12-12 | 2014-05-28 | 中国铝业股份有限公司 | Raw anode formula experiment method for increasing volume density of raw anode |
| CN108147404B (en) * | 2017-12-25 | 2020-02-07 | 大同新成新材料股份有限公司 | Graphite product with super-large specification and graphitization method thereof |
| CN117438129A (en) * | 2023-10-26 | 2024-01-23 | 重庆森仟烨新材料科技股份有限公司 | Regenerated graphite electrode and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5413689A (en) * | 1992-06-12 | 1995-05-09 | Moltech Invent S.A. | Carbon containing body or mass useful as cell component |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5413689A (en) * | 1992-06-12 | 1995-05-09 | Moltech Invent S.A. | Carbon containing body or mass useful as cell component |
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