CN102248580A - Molding method of fine grain graphite - Google Patents
Molding method of fine grain graphite Download PDFInfo
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- CN102248580A CN102248580A CN2010105967770A CN201010596777A CN102248580A CN 102248580 A CN102248580 A CN 102248580A CN 2010105967770 A CN2010105967770 A CN 2010105967770A CN 201010596777 A CN201010596777 A CN 201010596777A CN 102248580 A CN102248580 A CN 102248580A
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- powder
- petroleum coke
- fine grained
- forming method
- graphite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000010439 graphite Substances 0.000 title claims abstract description 52
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000000465 moulding Methods 0.000 title abstract description 6
- 239000002006 petroleum coke Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000010426 asphalt Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000002562 thickening agent Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 12
- 241001504664 Crossocheilus latius Species 0.000 claims description 8
- 239000002008 calcined petroleum coke Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000004898 kneading Methods 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 2
- 238000007599 discharging Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000004826 seaming Methods 0.000 description 7
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 238000005495 investment casting Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 239000002055 nanoplate Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910004349 Ti-Al Inorganic materials 0.000 description 1
- 229910004692 Ti—Al Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000006253 pitch coke Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
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Abstract
The invention provides a molding method of fine grain graphite, relating to graphite. The molding method of the fine grain graphite comprises the following steps of crushing and then pulverizing raw material petroleum coke so as to obtain petroleum coke powder; adding F3O2 powder to the petroleum coke powder so as to obtain a mixture of the petroleum coke powder and the F3O2 powder; putting the mixture of the petroleum coke powder and the F3O2 powder into a mixing kneading pot to be heated; and then adding liquid asphalt; discharging a paste out of the pot after mixing kneading of the mixture; putting the obtained paste on a heated tablet rolling machine to be rolled; cooling the rolled tablet in a natural environment to normal temperature; grinding the cooled rolled tablet so as to obtain the ground powder; filling the ground powder into a mold cylinder after preheating the ground powder; sealing the mold cylinder; vacuumizing to eliminate gas in the paste; pressurizing two ends of the mold cylinder; starting a vibrating platform; and releasing the mold and cooling to obtain a fine grain graphite product, wherein the dimension of the fine grain graphite product can reach phi 1000 mm*800 mm.
Description
Technical field
The present invention relates to a kind of graphite, especially relate to a kind of forming method of fine grained graphite goods.
Background technology
Be mainly used in the production of polysilicon, monocrystalline silicon Deng the graphite product of static pressure, can be used as the material of muff, heater, high temperature resistant member, also can be used for the mould of hot investment casting industry simultaneously.
Need adopt equal pressing equipment production routinely Deng the static pressure product, but the equipment price costliness especially produces large diameter product, equipment is bigger, and manufacturing cost is higher.
Along with the progress of industrial technology, novel carbon materials just is being applied to every field.The smelting of monocrystalline silicon, polysilicon, and industry such as hot investment casting to the demand of fine grained graphite with day increase severely.Existing fine grained graphite product mainly is the product of diameter less (ф 600mm is following), highly less (less than 500mm).Existing product does not satisfy the needs of maximization single crystal growing furnace far away, and ф 1000mm * 800mm fine grained graphite material that the large single crystal stove needs does not appear in the newspapers so far.
Chinese patent CN101654239 discloses a kind of isotropic graphite goods and preparation method thereof, its raw material comprises binding agent and aggregate, the mass ratio of binding agent and aggregate is (0.30～0.70): 1, wherein, purified natural micro crystal graphite accounts for 30%～100% of aggregate quality, and its clout is at least a in graphite returns, pitch coke, petroleum coke, secondary Jiao and the carbonaceous mesophase spherules; Its preparation method is by binding agent and aggregate are mixed, and again through overmolding, carries out roasting then, through dipping and after baking, carries out the step of graphitization processing at last and finishes again.
Chinese patent CN1505549 disclose a kind of in vacuum or low pressure inert atmosphere the various metal alloys of fusion such as nickel, cobalt and/or iron-based superalloy, stainless steel alloy, titanium alloy and Ti-Al alloy, in vacuum or low pressure inert atmosphere, melt is molded into the manufacturing process that graphite jig is shaped to engineering element afterwards.Mould is processed by high density ultra-fine grain shape isotropic graphite, and wherein graphite is with isobaric compacting or vibration formation method processing.
Chinese patent CN101348587 discloses a kind of preparation method of ultra-high molecular weight polyethylene/graphite nanoplate composite, comprises the steps: by the shared mass percent of each raw material to be: ultra-high molecular weight polyethylene 85%～99%, graphite 1%～15%; Join in the grinding pot, and add coupling agent according to the ratio of graphite quality 0.5%～1.5%; Add mill ball according to 1: 1～6: 1 ratios of grinding media to material; Rotating speed ball milling 1～4h with 350～580r/min; The dry materials that ball milling is good gets masterbatch; With masterbatch hot-press molding method moulding, get the ultra-high molecular weight polyethylene/graphite nanoplate composite.
Summary of the invention
The object of the present invention is to provide a kind of forming method of fine grained graphite.
The present invention adopts the graphite electrode make-up machine.
The present invention includes following steps:
1), gets petroleum coke powder with abrasive dust after the fragmentation of raw material petroleum coke;
In step 1), described petroleum coke can adopt calcined petroleum coke, and the ash content of described calcined petroleum coke is lower than 0.5%, and sulphur is lower than 0.3%; The granularity of described petroleum coke powder is preferably less than 100 orders.
2) in petroleum coke powder, add F
3O
2Powder gets petroleum coke powder and F
3O
2Mixture of powders;
In step 2) in, described adding F
3O
2The amount of powder can be 0.5%～1.5% of petroleum coke powder by mass percentage; Described F
3O
2The granularity of powder is less than 200 orders.
3) with petroleum coke powder and F
3O
2Mixture of powders is put into to mix and is pinched pot and heat, and adds liquid bitumen again, mix pinch after, thickener takes the dish out of the pot;
In step 3), the temperature of described heating can be 140～160 ℃; The amount of described adding liquid bitumen can be 26%～30% of material gross weight by mass percentage; The described mixed time of pinching can be 30min; For guaranteeing the plasticity of thickener, the temperature of described thickener can be 145～155 ℃.
4) thickener of step 3) gained is placed on the stone roller sheet machine of heating and grinds sheet, the slice, thin piece that ground is cooled to normal temperature in natural environment;
In step 4), the Controllable Temperature of described stone roller sheet machine is between 100～110 ℃.
5) cooled stone roller sheet is ground the powder after grinding;
In step 5), the powder after described the grinding is preferably less than 100 orders.
6) after the powder preheating after will grinding, in the mould tube of packing into, the sealing of mould tube vacuumizes, and gets rid of the gas in the thickener, the pressurization of mould tube two ends, the Vibration on Start-up platform, demoulding cooling, the fine grained graphite goods, its size can reach ф 1000mm * 800mm.
In step 6), the temperature of described preheating can be 90～100 ℃; The described vacuum that vacuumizes preferably is not less than-0.096MPa, and the time that vacuumizes preferably is not less than 40min; The specific pressure of described mould tube two ends pressurization is more preferably greater than 3MPa; The machine of described Vibration on Start-up platform shakes power more preferably greater than 400KN, and the time is preferably 10～6min.
Compare with the forming method of existing fine grained graphite goods, the present invention has following outstanding advantage:
Because make-up machine of the present invention (model is the make-up machine of CX-1400-800) is simple in structure, cost is low, and general needs 1,500,000 yuan; And adopt its price of equal pressing equipment of same specification to surpass 1,000 ten thousand yuan, once investment required for the present invention significantly reduces.
Adopt equipment depreciation of the present invention to reduce significantly.The cost of article of manufacture is well below the production cost that adopts the isostatic compaction machine.
This fine grained moulding green compact process, calcining process, the dipping operation, after graphitization process is handled, product after testing, its quality index is:
Bulk density: the requirement of overgauge YB/T119-1997 defined: 1.75～1.80g/cm
3
Compression strength: the requirement of overgauge GB/T1431-1985 defined: 20～30MPa;
Ash content: less than the requirement of standard GB/T1429-1985 defined: 0.5%.
The fine grained graphite goods of producing meet the G3 among the JB/T2750-2006 (seeing Table 1), the specification requirement of G4.
Table 1
The size of the prepared thin coccolith China ink goods of the present invention can reach ф 1000mm * 800mm.
Description of drawings
Fig. 1 forms schematic diagram for the embodiment of the invention adopts the structure of graphite electrode make-up machine.
Fig. 2 is that the side-looking structure of Fig. 1 is formed schematic diagram.
The specific embodiment
The present invention adopts graphite electrode make-up machine as illustrated in fig. 1 and 2, with the difference of the main technical detail of common vibrating forming machine is:
Specific pressure: common vibrating forming machine is 0.3～0.4MPa, and the specific pressure of this graphite electrode make-up machine is 2～3MPa;
Pressing mode: common vibrating forming machine is unidirectional pressurization, and this graphite electrode make-up machine is two-way pressurization, and its pressure reaches more than 200 tons;
The mode that applies of vibration source: common vibrating forming machine is to apply in the mold bottom vibration, and this graphite electrode make-up machine applies at the middle part.
This graphite electrode make-up machine is provided with electrode dolly 8, vacuum system 9, hydraulic system 10, electric-control system 11 and frame 13, also is provided with rubber spring support 1, mould 2, seaming chuck 3, cool material system 4, top dolly 5, stem stem and centre frame 6, switching mechanism 7, push-down head 12 and vibrating motor 14.
The rotating shaft of mould 2 is located on the rubber spring support 1, the thickener outlet of cold material system 4 connects mould 2 through belt feeder, seaming chuck 3 is connected with mould 2 with push-down head 12, top dolly 5 is located on the track of frame 13, seaming chuck 3, stem stem and centre frame 6 are located on the top dolly 5, vibrating motor 14 is as vibration source and be located at mould 2 both sides, vibrating motor 14 is arranged at the middle part of graphite electrode, be equipped with on seaming chuck 3 and the mould 2 and be connected tooth, be connected with mould 2 after seaming chuck 3 rotates 15 °, push-down head 12 is fixedly mounted on the bottom of mould 2; Switching mechanism 7 is connected with cool material system 4.Described cool material system 4 adopts the rotating disk coolers.Described vibrating motor 14 is located at mould 2 middle parts, makes the machine power of shaking more even in the axial distribution of shaped electrode.Described electric-control system 11 adopts programme-control treatment circuit (PLC), so whole operation can be controlled the realization operation automation by PLC.
Below provide production process:
1) reinforced: thickener joins in the mould behind the cool material of the cool material of rotating disk system, and after thickener added, the seaming chuck rotation was connected with mould and pins.
2) start vacuum system: the gas in the pumping mode tool, its vacuum reaches-0.93MPa.
3) start oil hydraulic system and vibration source, exert pressure and vibrate for thickener in the mould:
4) go out graphite electrode: mould lays down vacuum, release pressure after, open earlier and mention seaming chuck; Switching mechanism makes the mould rotation, and mould is the level of state; Graphite electrode is pushed and is poured on the electrode dolly.
5) then the graphite electrode upset is put on the electrode chill station.
Finished the forming process of a root graphite electrode, the gained graphite electrode can be large-size graphite electrode, and (ф 820～1400mm).
The whole operation process both can be manual, also can be controlled automatically by PLC and finish.
Below provide specific implementation method, may further comprise the steps:
1), gets petroleum coke powder with abrasive dust after the fragmentation of raw material petroleum coke; Described petroleum coke can adopt calcined petroleum coke, and the ash content of described calcined petroleum coke is lower than 0.5%, and sulphur is lower than 0.3%; The granularity of described petroleum coke powder is preferably less than 100 orders.
2) in petroleum coke powder, add F
3O
2Powder gets petroleum coke powder and F
3O
2Mixture of powders; Described adding F
3O
2The amount of powder is 0.5%～1.5% of petroleum coke powder by mass percentage; Described F
3O
2The granularity of powder is less than 200 orders.
3) with petroleum coke powder and F
3O
2Mixture of powders is put into to mix and is pinched pot and heat, and 140～160 ℃ of the temperature of heating add liquid bitumen again, mix and pinch 30min.Guarantee the plasticity of thickener, the temperature of thickener reaches about 150 ℃, and thickener takes the dish out of the pot.The amount of described adding pitch is 26%～30% (in the ratio of all material gross weights) by mass percentage.
4) thickener of step 3) gained is placed on the stone roller sheet machine of heating and grinds sheet, the temperature of grinding the sheet machine is controlled between 100-110 ℃, and the slice, thin piece that ground is cooled to normal temperature in natural environment.
5) cooled stone roller sheet is ground, the powder after must grinding is less than 100 orders.
6) powder after will grinding is preheating to 90～100 ℃, in the mould tube of packing into.
7) after the powder after grinding enters the mould tube, the sealing of mould tube.Vacuumize, vacuum is not less than-0.096Mpa, and the time that vacuumizes is not less than 40min, gets rid of the gas in the thickener; The pressurization of described mould tube two ends, specific pressure is greater than 3MPa.
8) Vibration on Start-up platform, machine shakes power more preferably greater than 400KN, and the time, demoulding cooling got the fine grained graphite goods at 10～6min, and its size reaches ф 1000mm * 800mm.
Claims (10)
1. the forming method of fine grained graphite is characterized in that may further comprise the steps:
1), gets petroleum coke powder with abrasive dust after the fragmentation of raw material petroleum coke;
2) in petroleum coke powder, add F
3O
2Powder gets petroleum coke powder and F
3O
2Mixture of powders;
3) with petroleum coke powder and F
3O
2Mixture of powders is put into to mix and is pinched pot and heat, and adds liquid bitumen again, mix pinch after, thickener takes the dish out of the pot;
4) thickener of step 3) gained is placed on the stone roller sheet machine of heating and grinds sheet, the slice, thin piece that ground is cooled to normal temperature in natural environment;
5) cooled stone roller sheet is ground the powder after grinding;
6) after the powder preheating after will grinding, in the mould tube of packing into, the sealing of mould tube vacuumizes, and gets rid of the gas in the thickener, the pressurization of mould tube two ends, the Vibration on Start-up platform, demoulding cooling, the fine grained graphite goods, its size can reach ф 1000mm * 800mm.
2. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 1), and described petroleum coke is a calcined petroleum coke, and the ash content of described calcined petroleum coke is lower than 0.5%, and sulphur is lower than 0.3%; The granularity of described petroleum coke powder is less than 100 orders.
3. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 2) in, described adding F
3O
2The amount of powder is 0.5%～1.5% of petroleum coke powder by mass percentage; Described F
3O
2The granularity of powder is less than 200 orders.
4. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 3), and the temperature of described heating is 140～160 ℃.
5. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 3), and the amount of described adding liquid bitumen is 26%～30% of material gross weight by mass percentage.
6. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 3), and the described mixed time of pinching is 30min; For guaranteeing the plasticity of thickener, the temperature of described thickener is 145～155 ℃.
7. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 4), and the temperature of described stone roller sheet machine is 100～110 ℃.
8. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 5), and the powder after described the grinding is less than 100 orders.
9. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 6), and the temperature of described preheating is 90～100 ℃; The described vacuum that vacuumizes is not less than-0.096MPa, and the time that vacuumizes is not less than 40min; The specific pressure of described mould tube two ends pressurization is greater than 3MPa.
10. the forming method of fine grained graphite as claimed in claim 1 is characterized in that in step 6), and the machine of described Vibration on Start-up platform shakes power greater than 400KN, and the time is 10～6min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105967770A CN102248580A (en) | 2010-12-20 | 2010-12-20 | Molding method of fine grain graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105967770A CN102248580A (en) | 2010-12-20 | 2010-12-20 | Molding method of fine grain graphite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102248580A true CN102248580A (en) | 2011-11-23 |
Family
ID=44976329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105967770A Pending CN102248580A (en) | 2010-12-20 | 2010-12-20 | Molding method of fine grain graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102248580A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105881711A (en) * | 2016-06-13 | 2016-08-24 | 索通发展股份有限公司 | Mould pressing forming process and mould pressing forming equipment for producing pre-baked anode green body |
| CN108218430A (en) * | 2017-12-05 | 2018-06-29 | 大同新成新材料股份有限公司 | A kind of isostatic pressing formed graphite product and preparation method thereof |
| CN114536843A (en) * | 2022-03-02 | 2022-05-27 | 中钢新型材料股份有限公司 | Vibration molding graphite preparation equipment for artware processing and process thereof |
-
2010
- 2010-12-20 CN CN2010105967770A patent/CN102248580A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105881711A (en) * | 2016-06-13 | 2016-08-24 | 索通发展股份有限公司 | Mould pressing forming process and mould pressing forming equipment for producing pre-baked anode green body |
| CN105881711B (en) * | 2016-06-13 | 2017-12-05 | 索通发展股份有限公司 | Compression molding produces the technique and its compression molding device of prebaked anode green body |
| CN108218430A (en) * | 2017-12-05 | 2018-06-29 | 大同新成新材料股份有限公司 | A kind of isostatic pressing formed graphite product and preparation method thereof |
| CN108218430B (en) * | 2017-12-05 | 2020-07-24 | 大同新成新材料股份有限公司 | Isostatic pressing graphite product and preparation method thereof |
| CN114536843A (en) * | 2022-03-02 | 2022-05-27 | 中钢新型材料股份有限公司 | Vibration molding graphite preparation equipment for artware processing and process thereof |
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Owner name: FUJIAN CHAOYANG SILICON MATERIALS CO., LTD. Free format text: FORMER OWNER: GONG BINGSHENG Effective date: 20111115 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20111115 Address after: 364211 Nanyang Industrial Zone, Nanyang Town, Shanghang County, Longyan, Fujian Applicant after: Fujian Xing the Zhaoyang Silicon Materials Co., Ltd. Address before: Nanyang town Longyan city Fujian province 364211 Ma Shanghang County Yang Dong River Road No. 1 Applicant before: Gong Bingsheng |
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Application publication date: 20111123 |