CN102730672A - Production technology of large-specification extraordinary isotropic graphite material - Google Patents
Production technology of large-specification extraordinary isotropic graphite material Download PDFInfo
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Abstract
A production technology of a large-specification extraordinary isotropic graphite material comprises the following steps: preparing coke powder with the average particle size of 6-20mum through utilizing airflow crushing, carrying out kneading, rolling and extrusion molding on the coke powder, rapidly charring, carrying out secondary kneading and rolling after charring, pre-molding the material subjected to the secondary kneading and rolling, and carrying out sequent processes of isopressing molding, dipping, roasting, graphitization and the like on pre-molded green body to prepare isopressed graphite; and carrying out cold molding and pressure holding stripping, and roasting and dipping many times to prepare the extraordinary isotropic graphite material. The extraordinary isotropic graphite material prepared through the method of the invention has the advantages of high mechanical strength, low porosity and excellent surface processing characteristic.
Description
Technical field
The present invention relates to machining graphite technology, be specially the production technique of the extraordinary same sex graphite material of a kind of big specification.
Background technology
Because of graphite material has characteristics such as high temperature resistant, corrosion-resistant, self-lubricating, obtained widespread use in a lot of fields.Along with development in science and technology, graphite material demands for higher performance such as each Application Areas.Graphite material adopt usually calcined coke as aggregate charcoal, modifying asphalt as sticker, make through mechanically mixing aftershaping, dipping and greying thermal treatment.But; In the above-mentioned technology; / 3rd above stickers decompose performance in roasting process; Cause the volumetric shrinkage difference between filler and the sticker, finally cause graphite material to have characteristics such as higher void content, the even structure degree is poor, the interface is obvious, cause the physical strength of final material to reduce.Drawbacks such as quality does not pass a test.
Thereby, need a kind of novel graphite material complete processing, in order to graphite material improve graphite material physical strength, reduce its void content, guarantee its fine in surface processing characteristics simultaneously.
Summary of the invention
The technical problem that the present invention solved is to provide the production technique of the extraordinary same sex graphite material of a kind of big specification, to solve the shortcoming in the above-mentioned background technology.
The technical problem that the present invention solved adopts following technical scheme to realize:
The production technique of the extraordinary same sex graphite material of big specification mainly comprises following operation steps:
Comminution by gas stream: calcined petroleum coke or pitch coke use micronizer mill that it is pulverized after coarse crushing, process the coke powder that median size is 6-20um.
Once mix and pinch, roll sheet: with the coke powder of 60:40 ~ 73:27 ratio and modifying asphalt under normal pressure the use kneading machine with its mixed pinching; Mix and pinch 0.35-2.6 hours time; 150 ~ 180 ℃ of temperature make it to become thickener, this thickener is mixed to pinch roll sheet while hot after finishing; Roll 130 ~ 170 ℃ of sheet temperature, roll the sheet number of times 1 ~ 10 time.
Extrusion molding: be crushed to below the 2mm after will rolling the thickener cooling behind the sheet, be squeezed into the elongated rods of 5 ~ 10mm with screw extrusion press.
Fast charring: elongated rods is inserted in the autoclave, under 550 ~ 650 ℃, 0.5 ~ 2.5MPa pressure, the pressurization charing, be 2 ~ 10 hours its pressure dwell, and the elongated rods after the charing is broken, screening, its broken fine and closely woven degree is being as the criterion through 80 ~ 200 mesh sieves.
Sheet is pinched, rolled to secondary mixing: the coke powder that sieves and modifying asphalt mixed in the carrying out with 60:40 ~ 73:27 ratio pinches, rolls sheet, and broken and cross 50 ~ 150 mesh sieves simultaneously, make press-powder.
Premolding: press-powder is packed in the steel die, and in press-powder, add 0.5 ~ 2wt% oleic acid, then at 100 ~ 200kg/cm
2Pressure condition under premolding; Perhaps adopt rubber coating vibration vacuum to decorate and carry out premolding.
Just processed isostatic pressing formed graphite behind the subsequent techniques such as the idiosome process isostatic pressing that premolding is good, dipping, roasting, greying.
In the present invention, treat hydrostatic profile after, must coldmoulding under 100 ~ 200Mpa pressure, pressurize demoulding after 10 minutes, the temperature rise rate with 10 ℃/hour under nitrogen protection of the idiosome behind the isostatic pressing is warming up to 850 ~ 1000 ℃, this is a bakes to burn the article; Cooling is come out of the stove the back under 265 ℃, 3.0Mpa pressure, adopts the mid-temperature pitch dipping 2.8 hours, and this is a single-steeping; Then, carry out re-baking, 800 ~ 900 ℃ of temperature: behind the idiosome naturally cooling behind the re-baking, going out time in temperature is that 320 ℃, pressure are under the condition of 33.5Mpa again, adopts the hard pitch dipping 4 hours, and this is a double-steeping; Then, carry out three roastings, 800 ~ 900 ℃ of temperature; Idiosome after three roastings places the graphitizing furnace of Frequency Induction Heating, and the temperature rise rate with 150 ℃/hour under the condition of argon shield is warming up to 2500 ℃, and constant temperature 1 hour makes finished product.
Compared with prior art, the present invention has the following advantages:
1. in that once to mix the time of carrying out charing after pinching shorter, temperature is lower, therefore still contains a certain amount of volatile matter.Can improve the wetting capacity with sticker, be very helpful improving the final mechanical property of product.
2. thickener still has certain shrink property through behind the fast charring.When roasting, aggregate coke and sticker have and shrink matching preferably, can effectively alleviate between aggregate coke and the sticker because of the excessive crackle that produces of volumetric shrinkage difference, improve its yield rate.
3. aggregate and caking agent colleague shrinks, and the caking agent that only has of comparing common process shrinks, and the finished product density will be done, and need not flood under the same case, has shortened the production cycle.
4. raw material (being coke powder) miniaturization; Mean particle size is 5 ~ 20; Cooperate special process processing again, making extraordinary carbon graphite material is static pressure isotropic graphite materials such as fine particle, compares with traditional coarse-grained graphite material; It has characteristics such as the meticulous densification of structure, good uniformity, mechanical property are excellent, wear-resisting, isotropy, mainly is to be particularly suitable for big products production.
5. coking under the employing pressure condition helps bonding (or cohering) component and infiltrates the filler endoporus, thereby has little high volume density and intensity.
Description of drawings
Fig. 1 is a product operational path block diagram of the present invention.
Embodiment
Give an actual example below and describe the present invention.
In the present embodiment, sticker is a modifying asphalt, and its main performance index is: carbon yield: 53%, and softening temperature: 79.5 ℃, fugitive constituent: 58.6%.
Soaker is mid-temperature pitch and hard pitch, and its salient features is following:
Mid-temperature pitch: carbon residue rate: 50.2%; Softening temperature: 79.5 ℃; Fugitive constituent: 58.6%;
Hard pitch: carbon yield: 56.6%; Softening temperature: 97.0 ℃; Fugitive constituent: 54.1%.
Filler is a calcined petroleum coke, and its main performance index is: ash content: 0.26%; Moisture: 0.38%.
Referring to Fig. 1, this production technique is carried out according to the following steps:
One, comminution by gas stream: calcined petroleum coke or pitch coke use micronizer mill that it is pulverized after coarse crushing, process the coke powder that median size is 6-20um.
Two, once mix and pinch, roll sheet: in the ratio of 3:2 coke powder is mixed it with modifying asphalt use kneading machine under normal pressure and pinch, mixing the time of pinching is two hours, and temperature is 160 ℃, and thickener is mixed to be pinched and roll sheet while hot after finishing, and rolls 160 ℃ of sheet temperature, and rolling the sheet number of times is 10 times.
Three, extrusion molding: be crushed to below the 2mm after the thickener cooling, be squeezed into the elongated rods of 8mm with screw extrusion press.
Four, fast charring: the elongated rods of extrusion molding is inserted in the autoclave, under 600 ℃, 2MPa pressure, pressurization charing, eight hours time.
Five, broken, screening: broken 150 mesh sieves of also crossing after the charing.
Six, sheet is pinched, rolled to secondary mixing: the coke powder that sieves and modifying asphalt are mixed in the ratio of 73:27 pinch, roll sheet, and broken then and cross 100 mesh sieves, make press-powder.
Seven, premolding: press-powder is packed in the steel die, and add the oleic acid of 2wt%, premolding under the pressure of 100 ~ 200kg/cm2.
Eight, isostatic pressing, roasting, dipping, greying; Wherein, coldmoulding under 160Mpa pressure during isostatic pressing, pressurize demoulding after 10 minutes; Base substrate behind isostatic pressing temperature rise rate with 10 ℃/h under nitrogen protection is warming up to 1000 ℃, and this is a bakes to burn the article.
Nine, cooling is come out of the stove the back under 260 ℃, 3.0MPa pressure, adopts the mid-temperature pitch dipping; Then, carry out re-baking, maturing temperature is 900 ℃.Behind the base substrate naturally cooling behind the re-baking, under 320 ℃, 3.5MPa pressure, adopt hard pitch dipping 4h once more, this is a double-steeping.
Ten, then, carry out three roastings, 900 ℃ of temperature.
Base substrate after 11, three roastings places the graphitizing furnace of Frequency Induction Heating, and the temperature rise rate with 150 ℃/h under argon shield is warming up to 2500 ℃, and constant temperature 1h makes finished product.
The extraordinary same sex graphite that adopts the method for present embodiment to make detects through test of many times, and to the performance of final graphitized material divide into groups test and analytical results, test result as follows:
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; The present invention is not restricted to the described embodiments; That describes in the foregoing description and the specification sheets just explains principle of the present invention; Under the prerequisite that does not break away from spirit and scope of the invention, the present invention also has various changes and modifications, and these variations and improvement all fall in the scope of the invention that requires protection.The scope of the present invention is required by the appended claims and their equivalents define
.
Claims (1)
1. the production technique of the extraordinary same sex graphite material of big specification is characterized in that, mainly comprises following operation steps:
Comminution by gas stream: calcined petroleum coke or pitch coke use micronizer mill that it is pulverized after coarse crushing, process the coke powder that median size is 6-20um;
Once mix and pinch, roll sheet: with the coke powder of 60:40 ~ 73:27 ratio and modifying asphalt under normal pressure the use kneading machine with its mixed pinching; Mix and pinch 0.35-2.6 hours time; 150 ~ 180 ℃ of temperature make it to become thickener, this thickener is mixed to pinch roll sheet while hot after finishing; Roll 130 ~ 170 ℃ of sheet temperature, roll the sheet number of times 1 ~ 10 time;
Extrusion molding: be crushed to below the 2mm after will rolling the thickener cooling behind the sheet, be squeezed into the elongated rods of 5 ~ 10mm with screw extrusion press;
Fast charring: elongated rods is inserted in the autoclave, under 550 ~ 650 ℃, 0.5 ~ 2.5MPa pressure, the pressurization charing, be 2 ~ 10 hours its pressure dwell, and the elongated rods after the charing is broken, screening, its broken fine and closely woven degree is being as the criterion through 80 ~ 200 mesh sieves;
Sheet is pinched, rolled to secondary mixing: the coke powder that sieves and modifying asphalt mixed in the carrying out with 60:40 ~ 73:27 ratio pinches, rolls sheet, and broken and cross 50 ~ 150 mesh sieves simultaneously, make press-powder;
Premolding: press-powder is packed in the steel die, and in press-powder, add 0.5 ~ 2wt% oleic acid, then at 100 ~ 200kg/cm
2Pressure condition under premolding; Perhaps adopt rubber coating vibration vacuum to decorate and carry out premolding;
Just processed isostatic pressing formed graphite behind the subsequent techniques such as the idiosome process isostatic pressing that premolding is good, dipping, roasting, greying; After treating hydrostatic profile, must coldmoulding under 100 ~ 200Mpa pressure, pressurize demoulding after 10 minutes, the temperature rise rate with 10 ℃/hour under nitrogen protection of the idiosome behind the isostatic pressing is warming up to 850 ~ 1000 ℃, and this is a bakes to burn the article; Cooling is come out of the stove the back under 265 ℃, 3.0Mpa pressure, adopts the mid-temperature pitch dipping 2.8 hours, and this is a single-steeping; Then, carry out re-baking, 800 ~ 900 ℃ of temperature: behind the idiosome naturally cooling behind the re-baking, going out time in temperature is that 320 ℃, pressure are under the condition of 33.5Mpa again, adopts the hard pitch dipping 4 hours, and this is a double-steeping; Then, carry out three roastings, 800 ~ 900 ℃ of temperature; Idiosome after three roastings places the graphitizing furnace of Frequency Induction Heating, and the temperature rise rate with 150 ℃/hour under the condition of argon shield is warming up to 2500 ℃, and constant temperature 1 hour makes finished product.。
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Cited By (16)
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| CN103121671A (en) * | 2013-03-15 | 2013-05-29 | 四川广汉士达炭素股份有限公司 | Preparation method of isostatic pressing formed graphite |
| CN103771404A (en) * | 2014-01-15 | 2014-05-07 | 湖南省长宇新型炭材料有限公司 | Preparation method of graphite rod of oilless bearing |
| CN103811758A (en) * | 2014-02-19 | 2014-05-21 | 新乡市赛日新能源科技有限公司 | Preparation method for synthesizing graphite particle negative electrode material |
| CN104828809A (en) * | 2015-04-23 | 2015-08-12 | 成都蓉光炭素股份有限公司 | Processing method for extrusion molded medium size structure graphite material |
| CN105236984A (en) * | 2015-10-20 | 2016-01-13 | 大同新成新材料股份有限公司 | Method for preparing graphite for compression molding casting |
| CN107522196A (en) * | 2017-08-28 | 2017-12-29 | 成都炭素有限责任公司 | A kind of superhard isostatic pressing formed graphite and preparation method thereof |
| CN107840328A (en) * | 2017-11-22 | 2018-03-27 | 大同新成新材料股份有限公司 | A kind of isostatic pressing formed graphite and its production method |
| CN107986786A (en) * | 2017-11-24 | 2018-05-04 | 大同新成新材料股份有限公司 | A kind of graphite product and production method |
| CN108911750A (en) * | 2018-07-24 | 2018-11-30 | 哈尔滨电碳厂 | A kind of preparation method of resistance to ablation carbon graphite material |
| CN109078690A (en) * | 2018-08-07 | 2018-12-25 | 东营鲁知信息科技有限公司 | A kind of isostatic pressing formed graphite production green coke pitch mixed grinding device |
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| CN110723971A (en) * | 2019-10-28 | 2020-01-24 | 焦作市中州炭素有限责任公司 | Special base material for annealing furnace for silicon steel production and preparation method |
| CN114349510A (en) * | 2022-01-14 | 2022-04-15 | 永安市鼎丰碳素科技有限公司 | Production process of isostatic pressing special graphite |
| CN114702316A (en) * | 2022-03-23 | 2022-07-05 | 湖南大学 | Preparation method and application of low-cost high-purity graphite material |
| CN115353391A (en) * | 2022-09-06 | 2022-11-18 | 湖南大学 | Method for preparing special graphite material by isostatic pressing graphite waste in short process |
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| CN103121671A (en) * | 2013-03-15 | 2013-05-29 | 四川广汉士达炭素股份有限公司 | Preparation method of isostatic pressing formed graphite |
| CN103771404A (en) * | 2014-01-15 | 2014-05-07 | 湖南省长宇新型炭材料有限公司 | Preparation method of graphite rod of oilless bearing |
| CN103811758A (en) * | 2014-02-19 | 2014-05-21 | 新乡市赛日新能源科技有限公司 | Preparation method for synthesizing graphite particle negative electrode material |
| CN103811758B (en) * | 2014-02-19 | 2016-04-20 | 新乡市赛日新能源科技有限公司 | A kind of preparation method of synthetic graphite particle negative material |
| CN104828809A (en) * | 2015-04-23 | 2015-08-12 | 成都蓉光炭素股份有限公司 | Processing method for extrusion molded medium size structure graphite material |
| CN105236984A (en) * | 2015-10-20 | 2016-01-13 | 大同新成新材料股份有限公司 | Method for preparing graphite for compression molding casting |
| CN105236984B (en) * | 2015-10-20 | 2018-05-01 | 大同新成新材料股份有限公司 | A kind of preparation method of compression molding casting graphite |
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| CN108911750A (en) * | 2018-07-24 | 2018-11-30 | 哈尔滨电碳厂 | A kind of preparation method of resistance to ablation carbon graphite material |
| CN109078690A (en) * | 2018-08-07 | 2018-12-25 | 东营鲁知信息科技有限公司 | A kind of isostatic pressing formed graphite production green coke pitch mixed grinding device |
| CN109192946A (en) * | 2018-08-28 | 2019-01-11 | 大同新成新材料股份有限公司 | A kind of preparation method of titanium-based ion cathode material lithium |
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Application publication date: 20121017 |