CN104649263B - The preparation method of carbon graphite composite material - Google Patents

The preparation method of carbon graphite composite material Download PDF

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CN104649263B
CN104649263B CN201510099268.XA CN201510099268A CN104649263B CN 104649263 B CN104649263 B CN 104649263B CN 201510099268 A CN201510099268 A CN 201510099268A CN 104649263 B CN104649263 B CN 104649263B
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petroleum coke
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CN104649263A (en
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张红亮
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Shanxi Liang Yutansu Co Ltd
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Abstract

The present invention relates to the preparation method of a kind of carbon graphite composite material, the raw material following granularity of employing and percentage by weight dispensing: white carbon black 1.5 2.5%, ≤ 1mm graphite 5 8%, ≤ 0.075mm calcined petroleum coke powder 25 30%, 1~4mm calcined petroleum coke 15 20%, 4~l0mm electric calcined anthracite 10 15%, 10 16mm electric calcined anthracite 5 ~ 10%, 10 16mm calcine pitch coke 5 ~ 15%, coal tar pitch 18 20%;Chopped carbon fiber is the 1 ~ 3% of above raw material total amount.Through dispensing, kneading, molding, roasting, graphitization, preparing carbon graphite composite material, function admirable, High anti bending strength, heat resistanceheat resistant performance of shaking is more excellent, and the coefficient of expansion is less, does not the most split continuous good stability.

Description

The preparation method of carbon graphite composite material
Technical field
The present invention relates to a kind of carbon graphite composite material preparation method, belong to specialty inorganic nonmetallic materials technical field.
Background technology
Carbon graphite material has that density is little, intensity is big, high temperature resistant, resist chemical, radioprotective, resisting fatigue, high connductivity, height Heat conduction, resistance to ablation, the characteristic of a series of excellences such as thermal expansion is little, physiological compatibility is good, obtain more and more in all trades and professions Many application.
Inorganic Non-metallic Materials is substantially fragile material, such as: brick, stone material, pottery, glass, cement concrete, carbon Material.Another feature of fragile material, comprcssive strength is higher, but anti-folding and shock resistance mechanical property are the lowest.Most inorganic non- Metal material (including carbon graphite material) has this feature.
Carbon graphite material 90% is mainly used in converter and aluminium cell and all kinds of mineral hot furnace, and its use occasion is usually It is the harsh conditions such as the corrosion of high temperature height electric current height and thermal vibration thermal shock.Owing to carbon graphite material rupture strength is low, poor toughness, Use under these harsh conditions and crackle often occurs, ftracture, rupture, fall block, peel off and fall slag and fall the phenomenons such as grain, improve charcoal graphite material The rupture strength of material and shaking property of heat resistanceheat resistant and toughness are difficult point and the focuses of current charcoal graphite technological progress in enterprises.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of carbon graphite composite material, and the method is prepared into To material there is good rupture strength, shaking property of heat resistanceheat resistant and toughness.
For solving above technical problem, the technical solution used in the present invention is:
A kind of preparation method of carbon graphite composite material, the raw material following granularity of employing and percentage by weight dispensing: white carbon black 1.5-2.5% ,≤1mm graphite 5-8% ,≤0.075mm calcined petroleum coke powder 25-30%, 1~4mm calcined petroleum coke 15 20%, 4~l0mm electric calcined anthracite 10-15%, 10-16mm electric calcined anthracite 5 ~ 10%, 10-16mm calcines pitch coke 5 ~ 15%, Coal tar pitch 18-20%;Chopped carbon fiber is the 1 ~ 3% of above raw material total amount.
Calcined petroleum coke powder and calcined petroleum coke are that electric calcined anthracite is through about 1100-through forming through about 1300 DEG C of calcinings 2000 DEG C of temperatures above calcinings form, and calcining pitch coke is to form through about 1300 DEG C of calcinings.White carbon black is conductive black, acetylene charcoal Black, semi-reinforcing hydrocarbon black and relevant white carbon black, performance indications are with to produce common carbon brush carbon black feed stock close.Native graphite, Ke Yishi Crystalline flake graphite can also be the amorphous graphite of low ash, and performance indications electromechanics carbon and graphite products native graphite common with production is former Expect close.Coal tar pitch can be medium temperature coal pitch can also be modified coal asphalt.Carbon graphite material and other inorganic non-metallic material As material, belonging to fragile material, rupture strength is low, and impact resistance is poor.And metal material feature is good toughness, High anti bending strength, anti- Impact is good.Add chopped carbon fiber sample rupture strength is significantly improved, add the toughness of carbon graphite material sample, carry High the shaking property of heat resistanceheat resistant of actual application.
Step includes:
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite and short Cut carbon fiber and be combined dispensing, kneading of heating with coal-tar bond after being dry mixed, form composite plastic gonosome;
(2) molding, is prepared as charcoal element compound green compact body by composite plastic gonosome by moulding process;
(3) roasting, loads roaster by green, through roasting, makes carbon material;
(4) graphitization, loads graphitizing furnace by carbon material, through 2200-3000 DEG C of high-temperature process, prepares charcoal graphite and is combined Material.
As preferred technical scheme, described kneading, it is first by white carbon black, native graphite, calcined petroleum coke powder, calcining stone Oil coke, electric calcined anthracite and calcining pitch coke add in kneading machine, add chopped carbon fiber and do after being spaced 5-6 minute Mixed, the time of being dry mixed is 35-40 minutes, and it is 120-150 DEG C that temperature is dry mixed;Time and temperature that temperature reach set is being dry mixed Time, the coal tar pitch adding 175 DEG C-185 DEG C carries out wet mixing, and the wet mixing time, kneading temperature was 160-165 DEG C at 30-50 minute, Thickener after kneading is carried out cool material, when thickener temperature is down to 125-145 DEG C, adds and mould is formed composite plastic gonosome.
As preferred technical scheme, described molding, refer to that vibration moulding, extruded, compression molding, isostatic pressed become One in type.
As preferred technical scheme, using hydraulic standing vibration moulding, main technologic parameters is: hydraulic pressure 4- 7Mpa, time of vibration is 3-7 minute;After vibration completes, pressure is kept to stand 2-5 minute;After standing completes, open mould, draw Green body water-spraying control 2-5 hour, coolant water temperature is 30-50 DEG C;After having cooled down, i.e. it is prepared as activated carbon composite element green.
As preferred technical scheme, described roasting completes according to following system,
1. shove charge system: green compact and green compact distance 100-120mm, green compact and kiln wall distance 150 1 250mm, raw The metallurgical coke particulate of base lower end paving 150mm thickness, green compact upper end covers the metallurgical coke particulate of 300-500mm thickness;
2. temperature increasing schedule: be 3-5 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C extremely 500 DEG C of temperature range average heating speeds are 1.0-1.5 DEG C per hour;At 500 DEG C to 600 DEG C of temperature range average heating speeds For 2.5-3.5 DEG C per hour;It it is 4-6 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;At 800 DEG C extremely 900 DEG C of temperature range average heating speeds are 5-15 DEG C per hour;At 900 DEG C to 1200 DEG C of temperature range average heating speeds it is 15-30 DEG C per hour;It is incubated 30-60 hour maximum temperature 1200 DEG C-1300 DEG C;
3. lower the temperature system: use natural cooling mode, per hour cooling 10-20 DEG C.
4. can come out of the stove when product is cooled to 300-400 DEG C.
As preferred technical scheme, described carbon fiber is PAN base chopped carbon fiber or asphaltic base chopped carbon fiber.Institute The chopped carbon fiber length stated can be 10-200mm, and average diameter is 5 microns-30 microns.Carbon fiber is being added kneading machine Use organic solvent the most in advance, as ethanol, acetone etc. carry out dispersion process.
The raw material of the present invention mainly uses oil refining side-product petroleum coke and stone coal, white carbon black, native graphite, drip Blue or green Jiao, metallurgical coke, carbon fiber are siccative raw material, and these raw material constituent element major parts are broken into the granularity of 0-20mm;Carbon graphite material Function admirable, High anti bending strength, heat resistanceheat resistant performance of shaking is more excellent, and the coefficient of expansion is less, does not the most split continuous good stability.
Detailed description of the invention
Embodiment 1
This embodiment as a comparison case, is not added with chopped carbon fiber.
Dispensing is :≤1mm micro crystal graphite 5% ,≤0.075mm calcined petroleum coke 28%, 1~4mm calcined petroleum coke 15%, 4 ~l0mm electric calcined anthracite 10%, 10-16mm electric calcined anthracite 5%, 10-16mm calcines pitch coke 15%, acetylene carbon black 2%, Coal tar pitch 20%.Additional 1% T300PAN chopped carbon fiber (diameter 12 m, length 10mm).
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite with forge Burning pitch coke to add in kneading machine, the time of being dry mixed is 35 minutes, and it is 120 DEG C that temperature is dry mixed;Be dry mixed temperature reach set time Between and during temperature, the coal tar pitch adding 175 DEG C carries out wet mixing, and the wet mixing time, kneading temperature was 160 DEG C at 30 minutes, is formed and answers Close plastic body;
(2) molding, uses compression molding, briquetting pressure 60Mpa, sample size Ф 80 × 80mm, system by composite plastic gonosome Standby one-tenth charcoal element compound green compact body;
(3) roasting, loads roaster by green, through roasting, makes carbon material;Roasting is complete according to following system Become:
1. shove charge system: green compact and green compact distance 100 mm, green compact and kiln wall distance 150mm, green compact lower end spreads The metallurgical coke particulate of 150mm thickness, green compact upper end covers the metallurgical coke particulate of 300 mm thickness;
2. temperature increasing schedule: be 3 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C to 500 DEG C temperature range average heating speed is 1.0 DEG C per hour;It is the least at 500 DEG C to 600 DEG C of temperature range average heating speeds Time 2.5 DEG C;It it is 4 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;800 DEG C to 900 DEG C temperature ranges Average heating speed is 5 DEG C per hour;It it is 15 DEG C per hour at 900 DEG C to 1200 DEG C of temperature range average heating speeds;? High-temperature 1200 DEG C is incubated 30-60 hour;
3. lower the temperature system: use natural cooling mode, per hour cooling 10-20 DEG C.
4. can come out of the stove when product is cooled to 300 DEG C.
(4) graphitization, loads graphitizing furnace by carbon material, through 2500 DEG C of high-temperature process, prepares carbon graphite composite material.
Carry out machining again, can be prepared by carbon material and the graphite composite material of function admirable.
Table 1 embodiment 1 prepared carbon material and graphite composite material quality index
Embodiment 2
Dispensing is :≤1mm micro crystal graphite 5% ,≤0.075mm calcined petroleum coke 28%, 1~4mm calcined petroleum coke 15%, 4 ~l0mm electric calcined anthracite 10%, 10-16mm electric calcined anthracite 5%, 10-16mm calcines pitch coke 15%, acetylene carbon black 2%, Coal tar pitch 20%.Additional 1% T300PAN chopped carbon fiber (diameter 12 m, length 10mm).
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite with forge Burning pitch coke to add in kneading machine, add chopped carbon fiber and be dry mixed after being spaced 5-6 minute, the time of being dry mixed is 35 minutes, It is 120 DEG C that temperature is dry mixed;When temperature being dry mixed and reaching the time and the temperature that set, the coal tar pitch adding 175 DEG C carries out wet mixing, wet Doing time at 30 minutes, kneading temperature is 160 DEG C, forms composite plastic gonosome;
(2) molding, uses compression molding, briquetting pressure 60Mpa, sample size Ф 80 × 80mm, system by composite plastic gonosome Standby one-tenth charcoal element compound green compact body;
(3) roasting, loads roaster by green, through roasting, makes carbon material;Roasting is complete according to following system Become:
1. shove charge system: green compact and green compact distance 100 mm, green compact and kiln wall distance 150mm, green compact lower end spreads The metallurgical coke particulate of 150mm thickness, green compact upper end covers the metallurgical coke particulate of 300mm thickness;
2. temperature increasing schedule: be 3 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C to 500 DEG C temperature range average heating speed is 1.0 DEG C per hour;It is the least at 500 DEG C to 600 DEG C of temperature range average heating speeds Time 2.5 DEG C;It it is 4 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;800 DEG C to 900 DEG C temperature ranges Average heating speed is 5 DEG C per hour;It it is 15 DEG C per hour at 900 DEG C to 1200 DEG C of temperature range average heating speeds;? High-temperature 1200 DEG C is incubated 30 hours;
3. lower the temperature system: use natural cooling mode, per hour cooling 10 DEG C.
4. can come out of the stove when product is cooled to 300 DEG C.
(4) graphitization, loads graphitizing furnace by carbon material, through 2500 DEG C of high-temperature process, prepares carbon graphite composite material.
Carry out machining again, can be prepared by carbon material and the graphite composite material of function admirable.
Table 2 embodiment 2 prepared carbon material and graphite composite material quality index
Embodiment 3
Use embodiment 2 dispensing constant, additional 2% T300PAN chopped carbon fiber (diameter 12 m, length 10mm), work Skill such as embodiment 1, records properties of sample index and is shown in Table 3.
Table 3 embodiment 3 prepared carbon material and graphite composite material quality index
Embodiment 4
Use embodiment 2 dispensing constant, additional 3% T300PAN chopped carbon fiber (diameter 12 m, length 10mm), work Skill such as embodiment 2, records properties of sample index and is shown in Table 4.
Table 4 embodiment 4 prepared carbon material and graphite composite material quality index
Embodiment 5
Use embodiment 2 dispensing constant, respectively additional 3% asphaltic base chopped carbon fiber (diameter 20 m, length 10mm), work Skill such as embodiment 2, records properties of sample index and is shown in Table 5.
Table 5 embodiment 5 prepared carbon material and graphite composite material quality index
Can be seen that from embodiment 1-5, under conditions of the dispensing of example 1 and technological requirement are constant, add T300PAN short Cutting carbon fiber (diameter 12 m, length 10mm), be improved comprehensive quality index, particularly rupture strength is worth to substantially carry Height, and with the increase of PAN chopped carbon fiber addition, rupture strength value improves the most obvious.Add 3% asphaltic base chopped carbon Fiber (diameter 20 m, length 10mm) does not add PAN to the improvement of sample rupture strength value and other quality indicator value Chopped carbon fiber is effective.Carbon graphite material, as other Inorganic Non-metallic Materials, belongs to fragile material, and rupture strength is low, anti- Impact is poor.And metal material feature is good toughness, High anti bending strength, good impact resistance.Add PAN chopped carbon fiber pair Sample rupture strength is significantly improved, and adds the toughness of carbon graphite material sample, improves the shaking property of heat resistanceheat resistant of actual application.
Embodiment 6
Dispensing is: 0.1mm micro crystal graphite 8%, 0.01mm calcined petroleum coke 25%, 1mm calcined petroleum coke 20%, 4mm electricity Forging anthracite 11%, 10mm electric calcined anthracite 6.5%, 10mm calcines pitch coke 10%, acetylene carbon black 1.5%, coal tar pitch 18%.Additional 2% T300PAN chopped carbon fiber (diameter 5 m, length 200mm).Use in advance before chopped carbon fiber is added kneading machine Organic solvent-acetone carries out dispersion process.
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite with forge Burning pitch coke to add in kneading machine, add chopped carbon fiber and be dry mixed after being spaced 6 minutes, the time of being dry mixed is 40 minutes, dry Mixed temperature is 150 DEG C;When temperature being dry mixed and reaching the time and the temperature that set, the coal tar pitch adding 185 DEG C carries out wet mixing, wet mixing Time, kneading temperature was 165 DEG C, and the thickener after kneading is carried out cool material at 50 minutes, when thickener temperature is down to 125 DEG C, added Enter formation composite plastic gonosome in mould;
(2) molding;Using hydraulic standing vibration moulding, main technologic parameters is: hydraulic pressure 4Mpa, and time of vibration is 3 Minute;After vibration completes, pressure is kept to stand 2 minutes;After standing completes, opening mould, pull-out green water-spraying control 2 is little Time, coolant water temperature is 30 DEG C;After having cooled down, i.e. it is prepared as activated carbon composite element green.
(3) roasting, loads roaster by green, through roasting, makes carbon material;Roasting is complete according to following system Become:
1. shove charge system: green compact and green compact distance 120 mm, green compact and kiln wall distance 250mm, green compact lower end spreads The metallurgical coke particulate of 150mm thickness, green compact upper end covers the metallurgical coke particulate of 500mm thickness;
2. temperature increasing schedule: be 5 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C to 500 DEG C temperature range average heating speed is 1.5 DEG C per hour;It is the least at 500 DEG C to 600 DEG C of temperature range average heating speeds Time 3.5 DEG C;It it is 6 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;800 DEG C to 900 DEG C temperature ranges Average heating speed is 15 DEG C per hour;It it is 30 DEG C per hour at 900 DEG C to 1200 DEG C of temperature range average heating speeds;Delay again Slowly it is warming up to 1300 DEG C, is incubated 60 hours;
3. lower the temperature system: use natural cooling mode, per hour cooling 20 DEG C.
4. can come out of the stove when product is cooled to 400 DEG C.
(4) graphitization, loads graphitizing furnace by carbon material, through 2200 DEG C of high-temperature process, prepares carbon graphite composite material.
Carry out machining again, can be prepared by carbon material and the graphite composite material of function admirable.
Embodiment 7
Dispensing is: 1mm native graphite 7%, 0.075mm calcined petroleum coke 28%, 4mm calcined petroleum coke 16%, 10mm electricity Forging anthracite 13%, 16mm electric calcined anthracite 10%, 16mm calcines pitch coke 5%, conductive black 2.5%, coal tar pitch 18.5%.Additional 1% T300PAN chopped carbon fiber (diameter 15 m, length 100mm).Adopt in advance before chopped carbon fiber is added kneading machine Dispersion process is carried out with organic solvent ethanol.
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite with forge Burning pitch coke to add in kneading machine, add chopped carbon fiber and be dry mixed after being spaced 6 minutes, the time of being dry mixed is 36 minutes, dry Mixed temperature is 130 DEG C;When temperature being dry mixed and reaching the time and the temperature that set, the coal tar pitch adding 180 DEG C carries out wet mixing, wet mixing Time, kneading temperature was 162 DEG C, and the thickener after kneading is carried out cool material at 40 minutes, when thickener temperature is down to 130 DEG C, added Enter formation composite plastic gonosome in mould;
(2) molding;Using hydraulic standing vibration moulding, main technologic parameters is: hydraulic pressure 7Mpa, and time of vibration is 7 Minute;After vibration completes, pressure is kept to stand 5 minutes;After standing completes, opening mould, pull-out green water-spraying control 5 is little Time, coolant water temperature is 50 DEG C;After having cooled down, i.e. it is prepared as activated carbon composite element green.
(3) roasting, loads roaster by green, through roasting, makes carbon material;Roasting is complete according to following system Become:
1. shove charge system: green compact and green compact distance 110 mm, green compact and kiln wall distance 200mm, green compact lower end spreads The metallurgical coke particulate of 150mm thickness, green compact upper end covers the metallurgical coke particulate of 400mm thickness;
2. temperature increasing schedule: be 4 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C to 500 DEG C temperature range average heating speed is 1.5 DEG C per hour;It is the least at 500 DEG C to 600 DEG C of temperature range average heating speeds Time 2.5 DEG C;It it is 5 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;800 DEG C to 900 DEG C temperature ranges Average heating speed is 10 DEG C per hour;It it is 20 DEG C per hour at 900 DEG C to 1200 DEG C of temperature range average heating speeds;? 1200 DEG C are incubated 50 hours;
3. lower the temperature system: use natural cooling mode, per hour cooling 15 DEG C.
4. can come out of the stove when product is cooled to 300 DEG C.
(4) graphitization, loads graphitizing furnace by carbon material, through 3000 DEG C of high-temperature process, prepares carbon graphite composite material.
Carry out machining again, can be prepared by carbon material and the graphite composite material of function admirable.
Embodiment 8
Dispensing is: 1mm native graphite 6%, 0.075mm calcined petroleum coke 26%, 4mm calcined petroleum coke 17%, 10mm electricity Forging anthracite 15%, 16mm electric calcined anthracite 6%, 16mm calcines pitch coke 9%, conductive black 2%, coal tar pitch 19%.Additional 3% T300PAN chopped carbon fiber (diameter 30 m, length 150mm).
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite with forge Burning pitch coke to add in kneading machine, add chopped carbon fiber and be dry mixed after being spaced 6 minutes, the time of being dry mixed is 38 minutes, dry Mixed temperature is 140 DEG C;When temperature being dry mixed and reaching the time and the temperature that set, the coal tar pitch adding 180 DEG C carries out wet mixing, wet mixing Time, kneading temperature was 160 DEG C, and the thickener after kneading is carried out cool material at 50 minutes, when thickener temperature is down to 145 DEG C, added Enter formation composite plastic gonosome in mould;
(2) molding;Using hydraulic standing vibration moulding, main technologic parameters is: hydraulic pressure 6Mpa, and time of vibration is 6 Minute;After vibration completes, pressure is kept to stand 4 minutes;After standing completes, opening mould, pull-out green water-spraying control 4 is little Time, coolant water temperature is 40 DEG C;After having cooled down, i.e. it is prepared as activated carbon composite element green.
(3) roasting, loads roaster by green, through roasting, makes carbon material;Roasting is complete according to following system Become:
1. shove charge system: green compact and green compact distance 110 mm, green compact and kiln wall distance 240mm, green compact lower end spreads The metallurgical coke particulate of 150mm thickness, green compact upper end covers the metallurgical coke particulate of 350mm thickness;
2. temperature increasing schedule: be 4 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C to 500 DEG C temperature range average heating speed is 1.5 DEG C per hour;It is the least at 500 DEG C to 600 DEG C of temperature range average heating speeds Time 2.5 DEG C;It it is 5 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;800 DEG C to 900 DEG C temperature ranges Average heating speed is 18 DEG C per hour;It it is 25 DEG C per hour at 900 DEG C to 1200 DEG C of temperature range average heating speeds;? 1200 DEG C are incubated 40 hours;
3. lower the temperature system: use natural cooling mode, per hour cooling 10 DEG C.
4. can come out of the stove when product is cooled to 350 DEG C.
(4) graphitization, loads graphitizing furnace by carbon material, through 3000 DEG C of high-temperature process, prepares carbon graphite composite material.
Carry out machining again, can be prepared by carbon material and the graphite composite material of function admirable.

Claims (8)

1. the preparation method of a carbon graphite composite material, it is characterised in that: raw material uses following granularity and percentage by weight to join Material: white carbon black 1.5-2.5% ,≤1mm graphite 5-8% ,≤0.075mm calcined petroleum coke powder 25-30%, 1~4mm calcined petroleum coke 15 20%, 4~l0mm electric calcined anthracite 10-15%, 10-16mm electric calcined anthracites 5 ~ 10%, 10-16mm calcines pitch coke 5 ~ 15%, coal tar pitch 18-20%;Chopped carbon fiber is the 1 ~ 3% of above raw material total amount, and step includes:
(1) dispensing, kneading, first by white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite, calcining drip Blue or green burnt and chopped carbon fiber is combined dispensing, and kneading of heating with coal-tar bond after being dry mixed forms composite plastic gonosome;
(2) molding, is prepared as charcoal element compound green compact body by composite plastic gonosome by moulding process;
(3) roasting, loads roaster by green, through roasting, makes carbon material;
(4) graphitization, loads graphitizing furnace by carbon material, through 2200-3000 DEG C of high-temperature process, prepares charcoal graphite composite wood Material.
Method the most according to claim 1, it is characterised in that:
Described kneading, is first white carbon black, native graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite and calcining to be dripped In blue or green burnt addition kneading machine, adding chopped carbon fiber and be dry mixed after being spaced 5-6 minute, the time of being dry mixed is 35-40 minutes, It is 120-150 DEG C that temperature is dry mixed;When temperature being dry mixed and reaching the time and the temperature that set, add the coal tar pitch of 175 DEG C-185 DEG C Carrying out wet mixing, the wet mixing time, kneading temperature was 160-165 DEG C, and the thickener after kneading is carried out cool material at 30-50 minute, when When thickener temperature is down to 125-145 DEG C, adds and mould is formed composite plastic gonosome.
Method the most according to claim 1, it is characterised in that: described molding, refer to vibration moulding, extruded, mould One in molded, isostatic pressing.
4. according to the method described in claim 1 or 3, it is characterised in that: use hydraulic standing vibration moulding, main technologic parameters For: hydraulic pressure 4-7MPa, time of vibration is 3-7 minute;After vibration completes, pressure is kept to stand 2-5 minute;Standing completes After, open mould, pull-out green water-spraying control 2-5 hour, coolant water temperature is 30-50 DEG C;After having cooled down, i.e. it is prepared as multiple Close charcoal element green.
Method the most according to claim 1, it is characterised in that:
Described roasting completes according to following system,
1. shove charge system: green compact and green compact distance 100-120mm, green compact and kiln wall distance 150 1 250mm, under green compact The metallurgical coke particulate of end paving 150mm thickness, green compact upper end covers the metallurgical coke particulate of 300-500mm thickness;
2. temperature increasing schedule: be 3-5 DEG C per hour from room temperature to 230 DEG C temperature range average heating speed;At 230 DEG C to 500 DEG C Temperature range average heating speed is 1.0-1.5 DEG C per hour;It is every at 500 DEG C to 600 DEG C of temperature range average heating speeds Hour 2.5-3.5 DEG C;It it is 4-6 DEG C per hour at 600 DEG C to 800 DEG C of temperature range average heating speeds;At 800 DEG C to 900 DEG C Temperature range average heating speed is 5-15 DEG C per hour;It is the least at 900 DEG C to 1200 DEG C of temperature range average heating speeds Time 15-30 DEG C;It is incubated 30-60 hour maximum temperature 1200 DEG C-1300 DEG C;
3. lower the temperature system: use natural cooling mode, per hour cooling 10-20 DEG C;
4. can come out of the stove when product is cooled to 300-400 DEG C.
Method the most according to claim 1, it is characterised in that: described chopped carbon fiber is PAN base carbon fibre or Colophonium Base carbon fibre.
7. according to the method described in claim 1 or 6, it is characterised in that: described chopped carbon fiber length is 10-200mm, flat All diameters are 5 microns-30 microns.
Method the most according to claim 1 and 2, it is characterised in that: before chopped carbon fiber is added kneading machine in advance Organic solvent is used to carry out dispersion process.
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CN106240039B (en) * 2016-07-28 2018-02-09 芜湖迈特电子科技有限公司 The technique that thermal diffusivity conductive graphite piece is prepared based on anthracite
CN106273820B (en) * 2016-07-28 2018-02-09 芜湖迈特电子科技有限公司 Insulated heat conductive graphite piece notacoria fine-processing technique
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CN107268034A (en) * 2017-06-15 2017-10-20 山西亮宇炭素有限公司 A kind of cathode carbon pieces of suitable phosphorus pig iron casting and preparation method thereof
CN108218429A (en) * 2017-10-10 2018-06-29 中国矿业大学 A kind of method that high purity graphite material is prepared using coal tar pitch as raw material
CN109456079B (en) * 2018-12-29 2021-08-17 宁夏宁平炭素有限责任公司 Preparation method of heat-preservation type microporous electric furnace carbon block for submerged arc furnace
CN110194666A (en) * 2019-04-30 2019-09-03 醴陵南方材料科技有限公司 The production method of big specification high-graphite carbon electrode for smelting industrial silicon
CN110054448A (en) * 2019-05-24 2019-07-26 重庆交通职业学院 A kind of environmental-friendly conductive concrete with and its preparation method and application
CN110380050B (en) * 2019-06-06 2021-05-18 湖南中科星城石墨有限公司 Mixing process for preparing high-tap microcrystalline graphite negative electrode material
CN110524905A (en) * 2019-08-21 2019-12-03 大同新成新材料股份有限公司 A kind of carbon carbon composite mould pressing method
CN113501515A (en) * 2021-07-29 2021-10-15 濮方正 Innovative process for manufacturing anthracite into conductor material
CN114478042A (en) * 2022-02-23 2022-05-13 永安市鼎丰碳素科技有限公司 Preparation method of fiber-reinforced special isostatic pressing graphite
CN115849907A (en) * 2022-12-05 2023-03-28 重庆东星炭素材料有限公司 Semi-carbon black lattice furnace process
CN116082041B (en) * 2023-02-20 2024-06-25 平顶山东方碳素股份有限公司 Graphite material with low thermal expansion coefficient and production method thereof
CN116283333B (en) * 2023-05-18 2023-08-04 西南交通大学 Sulfonated graphene reinforced carbon-based composite material and preparation method and application thereof
CN117263706B (en) * 2023-10-07 2024-05-14 湖北东南佳新材料有限公司 Wear-resistant low-resistance carbon material and preparation method thereof
CN117447204B (en) * 2023-12-22 2024-03-15 成都中超碳素科技有限公司 Preparation method of mechanical carbon material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102530923A (en) * 2010-12-08 2012-07-04 沈阳铝镁设计研究院有限公司 High-temperature electric calcining system and method of carbon raw material
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102530923A (en) * 2010-12-08 2012-07-04 沈阳铝镁设计研究院有限公司 High-temperature electric calcining system and method of carbon raw material
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

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