CN107522196A - A kind of superhard isostatic pressing formed graphite and preparation method thereof - Google Patents
A kind of superhard isostatic pressing formed graphite and preparation method thereof Download PDFInfo
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- CN107522196A CN107522196A CN201710750921.3A CN201710750921A CN107522196A CN 107522196 A CN107522196 A CN 107522196A CN 201710750921 A CN201710750921 A CN 201710750921A CN 107522196 A CN107522196 A CN 107522196A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The present invention relates to graphite preparing technical field, and in particular to a kind of superhard isostatic pressing formed graphite and preparation method thereof.Preparation method of the present invention includes：A, by after-smithing petroleum coke, forge rear pitch coke, graphite particle respectively through crushing, obtain aggregate after being mixed with carbon powder；B, by aggregate preheating, adding additives, 1~3h is strongly mixed at 150~180 DEG C, through extruding, shearing, disperseing, being kneaded, being granulated, is cooled to normal temperature, crushed, obtain the press-powder of average grain diameter≤20 μm；C, press-powder is loaded into rubber mass mould, sealing vacuumizes, and the isostatic pressing under 130~180MPa, obtains green compact；D, green compact are warming up to 950~1150 DEG C with 1~5 DEG C/h, obtain charcoal base substrate；E, charcoal base substrate is subjected to graphitization processing, produced.Superhard isostatic pressing formed graphite material prepared by the inventive method, have the characteristics that hardness superelevation, compact structure, uniformity are good, isotropism degree is high, production cost is low, with short production cycle.
Description
Technical field
The present invention relates to graphite preparing technical field, and in particular to a kind of superhard isostatic pressing formed graphite and preparation method thereof.
Background technology
Isostatic pressing formed graphite, a kind of New graphite material to grow up as the twentieth century middle and later periods, have a series of excellent
Different in nature energy, for example, highly dense, high-strength, isotropism, chemical resistance are strong, thermal conductivity is good, inoxidizability is strong, machinery adds
Work is good.Under an inert atmosphere, with the rise of temperature, its mechanical strength goes up not down isostatic pressing formed graphite, at 2500 DEG C or so
Reach peak.
For hyperfine structure isostatic pressing formed graphite because preparation technology is complicated, technical difficulty is big, relate generally to raw material, technique, equipment,
Process processing, surface treatment etc..With the development of science and technology, the application field of isostatic pressing formed graphite is constantly further widened,
Market demand increasing trend is gradually especially presented in fields such as space flight, military project, nuclear energy, electronic industries.Traditional preparation technology life
The isostatic pressing formed graphite of production, even across the hyperfine structure isostatic pressing formed graphite obtained after impregnation-calcination repeatedly again graphitization, its machinery
Intensity can be lifted necessarily, but the Shore hardness of material is general all below 80, and requiring wearability higher in part answers
With field, the low isostatic pressing formed graphite material of hardness typically shows that the life-span is low, the shortcomings that being easily lost.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of production cost is low, with short production cycle, product
The good superhard isostatic pressing formed graphite preparation method of homogenieity.
A kind of preparation method of superhard isostatic pressing formed graphite of the present invention, comprises the following steps：
A, by after-smithing petroleum coke, forge rear pitch coke, graphite particle by crushing, respectively obtain after particle diameter is 3~5 μm forge
Petroleum coke powder, rear pitch coke powder and graphite powder powder are forged, aggregate is obtained after being mixed with nanoscale carbon powder；
B, by the aggregate preheating that a steps obtain to 100~130 DEG C, binding agent is added, is strongly mixed at 150~180 DEG C
1~3h, through extruding, shearing, disperseing, being kneaded, being granulated, normal temperature is cooled to, crushes, obtain the press-powder of average grain diameter≤20 μm；
C, the press-powder obtained b step loads rubber mass mould, and sealing vacuumizes, under 130~180MPa isostatic pressed into
Type, obtain green compact；
D, the green compact for obtaining step c are warming up to 950~1150 DEG C with 1~5 DEG C/h, obtain charcoal base substrate；
E, the charcoal base substrate for obtaining Step d carries out graphitization processing, and graphitization temperature is 2300~2500 DEG C, and insulation 2~
6h, it is cooled to less than 120 DEG C and comes out of the stove, produce.
Crushed described in a steps first to obtain particle diameter≤1mm coarse powder material using hammer mill is slightly broken, then by air-flow
It is milled broken, obtains the powder that particle diameter is 3~5 μm.
Carbon powder described in a steps in aggregate is the reinforcement nano carbon black of natural gas half.
After-smithing petroleum coke powder in the aggregate, forge the percentage by weight of rear pitch coke powder, graphite powder and carbon powder for 0~
100:0~100:0~100:0~100, and four addition sum ＞ 0.
Binding agent described in b step is coal tar pitch, the softening point of the coal tar pitch 85~120 DEG C, coking value 48~
65%.
The percentage by weight of aggregate described in b step and binding agent is 55~60:45~40.
Crush described in b step and carried out using two steps ,≤3mm powder is first broken into using hammer mill, then use machine
The press-powder of particle mean size≤20 μm is made in tool pulverizer.
Bulk density >=1.81g/cm of the superhard isostatic pressing formed graphite3, rupture strength >=55MPa, compression strength >=
112MPa, Shore hardness >=78.
The bulk density of the superhard isostatic pressing formed graphite is 1.84g/cm3, rupture strength 74MPa, compression strength is
140MPa, Shore hardness 96.
The beneficial effects of the invention are as follows：
1st, to be said from raw material selected angle, aggregate is burnt to select after-smithing petroleum coke or pitch coke more universal on domestic market,
A certain proportion of the reinforcement nano carbon black of natural gas half and graphite powder are added, binding agent is existed from the softening point of common coke-oven plant production
85-120 DEG C, coking value in 48-65% coal tar pitch, therefore cost of material is relatively low；
2nd, for process equipment, domestic airslide disintegrating mill and mechanical crusher, kneading are selected according to feed particles characteristic
The strong kneader system transformed using autonomous Design, have mixing, extruding, shearing, scattered, mixing, granulation function concurrently, ensure bone
Material mixed powder is evenly distributed, and is combined with the abundant infiltration of binder pitch and cladding, makes the uniformity and plasticity of compound
It is improved, reduces being mingled with for powder and pitch, and eliminate traditional roller sheet equipment, avoids the drip that roller sheet process is brought
Blue or green flue gas environmental pollution；
3rd, for technological process, the technology that the present invention uses is direct graphitization after roasting, eliminates traditional handicraft
Impregnation-calcination repeatedly, the production cycle is shortened, reduce production cost.Than ever prepared by fine texture graphite material to need repeatedly leaching
Stain-firing cycles could realize that high-density high-strength technique is compared, and the present invention is closely knit using the heat-induced shrinkage raising material of material itself
Degree and intensity, substantially reduce the production cycle, reduce production cost；
4th, the superhard isostatic pressing formed graphite material being prepared by the method for the present invention, there is hardness superelevation, compact structure, uniformity
Well, the features such as isotropism degree is high, production cost is low, with short production cycle.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of the superhard isostatic pressing formed graphite of the present invention.
Embodiment
Technical scheme is described in further detail with reference to specific embodiment, but protection scope of the present invention is not
It is confined to as described below.
Embodiment 1
First by the petroleum coke through 1300 DEG C of calcination processings and graphite it is broken respectively with hammer mill be crushed to 1mm and with
Under, then with airslide disintegrating mill respectively be made 5 μm of particle mean size aggregate coke powder, by 5 μm obtained of petroleum coke powder and graphite
Powder presses 9:1 mass is than dispensing, then it is 95 DEG C that mixed powder homogenizing is preheating into 120 DEG C with softening point, coking value be 50% it is viscous
Tying agent coal tar pitch, (aggregate powder content is 59%, and binder pitch content is 41%), kneading is granulated in 160 DEG C of strength kneading 1.5h
Below 3mm is crushed to hammer mill after cooling, press-powder, 15 μm of press-powder particle mean size is made with mechanical crusher.By press-powder
Load the sealing of rubber die sleeve, the isostatic pressing under 140MPa pressure, molding blank is warming up to 950 with 5 DEG C/h heating rate
DEG C, obtain charcoal base substrate.Graphitization processing is carried out to charcoal base substrate, graphitization temperature is 2500 DEG C, and 2h is incubated under maximum temperature, natural
It is cooled to less than 120 DEG C to come out of the stove, completes the preparation of material.The Fundamental Physical Properties of final material are shown in Table 1.
Embodiment 2
The pitch coke through 1250 DEG C of calcination processings is crushed to 1mm and following with hammer mill first, then with air-flow powder
Broken mechanism obtains the aggregate coke powder of 5 μm of particle mean size, and the aggregate coke powder and carbon powder are pressed into 8:The mixing of 2 mass ratioes is preheating to 130 DEG C,
It it is 115 DEG C with softening point, in 180 DEG C of strength kneading 2.5h, (pitch coke aggregate powder contains the coal pitch of agglomerant that coking value is 62%
Measure as 57%, binder pitch content is 43%), compound is granulated after cooling and is crushed to below 3mm with hammer mill, uses machine
Press-powder, 15 μm of press-powder particle mean size is made in tool pulverizer.Press-powder is loaded into the sealing of rubber die sleeve, the isostatic pressed under 160MPa pressure
Shaping, molding blank are warming up to 1000 DEG C with 1.5 DEG C/h heating rate, charcoal base substrate are obtained after cooling.Stone is carried out to charcoal base substrate
Blackization processing, graphitization temperature are 2500 DEG C, are incubated 5h under maximum temperature, naturally cool to less than 120 DEG C and come out of the stove, complete material
Preparation.The Fundamental Physical Properties of final material are shown in Table 1.
Embodiment 3
1mm and following is crushed to hammer mill by the pitch coke through 1250 DEG C of calcination processings and graphite are broken respectively, then
The aggregate coke powder of 5 μm of particle mean size is made respectively with airslide disintegrating mill, 5 μm obtained of pitch coke powder and graphite powder are pressed 9:
1 mass is than dispensing, then it is 105 DEG C that mixed powder homogenizing is preheating into 120 DEG C with softening point, and coking value is 60% binding agent coal
In 170 DEG C of strength kneading 2.5h, (aggregate powder content is 57% to pitch, and binder pitch content is 43%), compound is granulated cooling
Below 3mm is crushed to hammer mill afterwards, press-powder, 15 μm of press-powder particle mean size is made with mechanical crusher.Press-powder is loaded
Rubber die sleeve seals, and the isostatic pressing under 150MPa pressure, molding blank is warming up to 1050 with 2.5 DEG C/h heating rate
DEG C, obtain charcoal base substrate.Graphitization processing is carried out to charcoal base substrate, graphitization temperature is 2500 DEG C, and 6h is incubated under maximum temperature, natural
It is cooled to less than 120 DEG C to come out of the stove, completes the preparation of material.The Fundamental Physical Properties of final material are shown in Table 1.
Embodiment 4
First by the petroleum coke through 1300 DEG C of calcination processings, the pitch coke through 1250 DEG C of calcination processings and graphite is broken uses respectively
Hammer mill is crushed to 1mm and following, then the aggregate coke powder of 5 μm of particle mean size is made with airslide disintegrating mill respectively, will be made
5 μm of petroleum coke powder, pitch coke powder and graphite powder press 45:45:10 mass are preheating to than dispensing, then by mixed powder homogenizing
130 DEG C are 115 DEG C with softening point, and in 175 DEG C of strength kneading 3h, (aggregate powder content is the coal pitch of agglomerant that coking value is 62%
58%, binder pitch content is 42%), compound is granulated after cooling and is crushed to below 3mm with hammer mill, with mechanical powder
Broken mechanism obtains press-powder, 15 μm of press-powder particle mean size.Press-powder is loaded into the sealing of rubber die sleeve, under 150MPa pressure isostatic pressed into
Type, molding blank are warming up to 1150 DEG C with 3 DEG C/h heating rate, obtain charcoal base substrate.Graphitization processing, stone are carried out to charcoal base substrate
Inkization temperature is 2500 DEG C, is incubated 5h under maximum temperature, naturally cools to less than 120 DEG C and come out of the stove, complete the preparation of material.Finally
The Fundamental Physical Properties of material are shown in Table 1.
Comparative example 1
The petroleum coke through 1300 DEG C of calcination processings is crushed to 1mm and following with hammer mill first, then with air-flow powder
Broken mechanism obtains the aggregate coke powder of 5 μm of particle mean size, and it is 95 DEG C that the coke powder is preheating into 110 DEG C with softening point, coking value 50%
Coal pitch of agglomerant in 160 DEG C of strength kneading 1.5h, (petroleum coke aggregate powder content is 60%, and binder pitch content is
40%), compound is granulated after cooling and is crushed to below 3mm with hammer mill, press-powder is made with mechanical crusher, press-powder is average
15 μm of granularity.Press-powder is loaded into the sealing of rubber die sleeve, the isostatic pressing under 140MPa pressure, molding blank is with 5 DEG C/h liter
Warm speed is warming up to 950 DEG C, obtains charcoal base substrate.Graphitization processing is carried out to charcoal base substrate, graphitization temperature is 2500 DEG C, the highest temperature
The lower insulation 2h of degree, naturally cooling to less than 120 DEG C comes out of the stove, and completes the preparation of material.The Fundamental Physical Properties of final material are shown in Table
1。
The Fundamental Physical Properties of the material of table 1
Described above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form, the exclusion to other embodiment is not to be taken as, and can be used for various other combinations, modification and environment, and can be at this
In the text contemplated scope, it is modified by the technology or knowledge of above-mentioned teaching or association area.And those skilled in the art are entered
Capable change and change does not depart from the spirit and scope of the present invention, then all should be in the protection domain of appended claims of the present invention
It is interior.
Claims (9)
1. a kind of preparation method of superhard isostatic pressing formed graphite, it is characterised in that comprise the following steps：
A, by after-smithing petroleum coke, forge rear pitch coke, graphite particle by crushing, respectively obtain particle diameter and be 3~5 μm and forge rear oil
Coke powder, rear pitch coke powder and graphite powder powder are forged, aggregate is obtained after being mixed with nanoscale carbon powder；
B, by the aggregate preheating that a steps obtain to 100~130 DEG C, binding agent is added, strongly mix 1 at 150~180 DEG C~
3h, through extruding, shearing, disperseing, being kneaded, being granulated, normal temperature is cooled to, crushes, obtain the press-powder of average grain diameter≤20 μm；
C, the press-powder for obtaining b step loads rubber mass mould, and sealing is vacuumized, the isostatic pressing under 130~180MPa, obtained
To green compact；
D, the green compact for obtaining step c are warming up to 950~1150 DEG C with 1~5 DEG C/h, obtain charcoal base substrate；
E, the charcoal base substrate for obtaining Step d carries out graphitization processing, and graphitization temperature is 2300~2500 DEG C, is incubated 2~6h, cold
But come out of the stove, produce to less than 120 DEG C.
2. the preparation method of a kind of superhard isostatic pressing formed graphite according to claim 1, it is characterised in that described in a steps
Crush first to use hammer mill is slightly broken to obtain particle diameter≤1mm coarse powder material, then crushed by airflow milling, obtain particle diameter as 3
~5 μm of powder.
3. the preparation method of a kind of superhard isostatic pressing formed graphite according to claim 1, it is characterised in that described in a steps
Carbon powder in aggregate is the reinforcement nano carbon black of natural gas half.
4. the preparation method of a kind of superhard isostatic pressing formed graphite according to claim 3, it is characterised in that forged in the aggregate
Afterwards petroleum coke powder, forge rear pitch coke powder, graphite powder and carbon powder percentage by weight be 0~100:0~100:0~100:0~
100, and four addition sum ＞ 0.
5. the preparation method of a kind of superhard isostatic pressing formed graphite according to claim 1, it is characterised in that described in b step
Binding agent is coal tar pitch, and the softening point of the coal tar pitch is in 85~120 DEG C, coking value 48~65%.
A kind of 6. preparation method of superhard isostatic pressing formed graphite according to claim 1 or 5, it is characterised in that institute in b step
The percentage by weight for stating aggregate and binding agent is 55~60:45~40.
7. the preparation method of a kind of superhard isostatic pressing formed graphite according to claim 1, it is characterised in that described in b step
It is broken to be carried out using two steps ,≤3mm powder is first broken into using hammer mill, then particle mean size is made with mechanical crusher
≤ 20 μm of press-powder.
8. the superhard isostatic pressing formed graphite that the preparation method described in any one of claim 1~7 is prepared, it is characterised in that institute
State bulk density >=1.81g/cm of superhard isostatic pressing formed graphite3, rupture strength >=55MPa, compression strength >=112MPa, Shore is hard
Degree >=78.
9. superhard isostatic pressing formed graphite according to claim 8, it is characterised in that the volume of the superhard isostatic pressing formed graphite is close
Spend for 1.84g/cm3, rupture strength 74MPa, compression strength 140MPa, Shore hardness 96.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503363A (en) * | 2018-03-26 | 2018-09-07 | 大同新成新材料股份有限公司 | A kind of pantograph carbon slide of carbon-carbon composite and preparation method thereof |
| CN108727063A (en) * | 2018-06-01 | 2018-11-02 | 中钢集团新型材料（浙江）有限公司 | A kind of dipping method for the big specification isostatic pressing formed graphite of fine texture high density |
| CN108751992A (en) * | 2018-07-19 | 2018-11-06 | 大同新成新材料股份有限公司 | A kind of preparation method of the copper-based isostatic pressing formed graphite composite material of isotropism |
| CN109319775A (en) * | 2018-11-19 | 2019-02-12 | 成都炭素有限责任公司 | A kind of preparation method of short route high-density high-strength isotropic graphite |
| CN109336604A (en) * | 2018-10-26 | 2019-02-15 | 上海东洋炭素有限公司 | A kind of preparation method of electric vacuum pump graphite rotator |
| CN109503169A (en) * | 2018-12-24 | 2019-03-22 | 成都阿泰克特种石墨有限公司 | A kind of special graphite and preparation method thereof |
| CN111875379A (en) * | 2020-06-15 | 2020-11-03 | 深圳市赛普戴蒙德科技有限公司 | Preparation method and application of carbon-based chip special carbon material |
| CN113896534A (en) * | 2021-09-29 | 2022-01-07 | 大同新成新材料股份有限公司 | Isostatic pressing graphite product with high compression strength and high breaking strength and forming method thereof |
| CN114604866A (en) * | 2022-04-26 | 2022-06-10 | 四川士达特种炭材有限公司 | Method for preparing high-performance isostatic pressing graphite in short process |
| CN115353390A (en) * | 2022-08-09 | 2022-11-18 | 自贡东新电碳有限责任公司 | Preparation method of high-density carbon graphite composite material |
| CN115403383A (en) * | 2021-05-28 | 2022-11-29 | 成都炭素有限责任公司 | Manufacturing method of graphite mold material for hot bending of curved-surface glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108503363A (en) * | 2018-03-26 | 2018-09-07 | 大同新成新材料股份有限公司 | A kind of pantograph carbon slide of carbon-carbon composite and preparation method thereof |
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| CN109336604A (en) * | 2018-10-26 | 2019-02-15 | 上海东洋炭素有限公司 | A kind of preparation method of electric vacuum pump graphite rotator |
| CN109319775A (en) * | 2018-11-19 | 2019-02-12 | 成都炭素有限责任公司 | A kind of preparation method of short route high-density high-strength isotropic graphite |
| CN109503169A (en) * | 2018-12-24 | 2019-03-22 | 成都阿泰克特种石墨有限公司 | A kind of special graphite and preparation method thereof |
| CN111875379A (en) * | 2020-06-15 | 2020-11-03 | 深圳市赛普戴蒙德科技有限公司 | Preparation method and application of carbon-based chip special carbon material |
| CN111875379B (en) * | 2020-06-15 | 2022-11-15 | 深圳市赛普戴蒙德科技有限公司 | Preparation method and application of carbon-based chip special carbon material |
| CN115403383A (en) * | 2021-05-28 | 2022-11-29 | 成都炭素有限责任公司 | Manufacturing method of graphite mold material for hot bending of curved-surface glass |
| CN113896534A (en) * | 2021-09-29 | 2022-01-07 | 大同新成新材料股份有限公司 | Isostatic pressing graphite product with high compression strength and high breaking strength and forming method thereof |
| CN114604866A (en) * | 2022-04-26 | 2022-06-10 | 四川士达特种炭材有限公司 | Method for preparing high-performance isostatic pressing graphite in short process |
| CN115353390A (en) * | 2022-08-09 | 2022-11-18 | 自贡东新电碳有限责任公司 | Preparation method of high-density carbon graphite composite material |
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