CN108675292A - The method that combination method prepares isotropic graphite material - Google Patents

The method that combination method prepares isotropic graphite material Download PDF

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Publication number
CN108675292A
CN108675292A CN201810802474.6A CN201810802474A CN108675292A CN 108675292 A CN108675292 A CN 108675292A CN 201810802474 A CN201810802474 A CN 201810802474A CN 108675292 A CN108675292 A CN 108675292A
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graphite material
prepares
oxygen
isotropic graphite
agent
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张海霞
闫桂林
李红岩
王方丽
胡春燕
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Jining Kenon New Carbon Materials Technology Co Ltd
JINING CARBON GROUP CO Ltd
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Jining Kenon New Carbon Materials Technology Co Ltd
JINING CARBON GROUP CO Ltd
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Priority to CN201810802474.6A priority Critical patent/CN108675292A/en
Publication of CN108675292A publication Critical patent/CN108675292A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/20Graphite
    • C01B32/205Preparation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The present invention relates to the methods that the preparation method of graphite material, especially combination method prepare isotropic graphite material, include the following steps:Using the pitch under the high softening-point state after Oxygen in Liquid agent and air oxygen agent joint cure treatment as raw material, by obtaining graphite material from sintering process.High softening point bitumen selected by this method, no matter macroscopically or it is microcosmic on be all it is isotropic, graphite material obtained have High anti bending strength, the characteristic that compression strength is good, bulk density and isotropism are good;Combined using the gentle phase oxidation agent of Oxygen in Liquid agent, Promethean two kinds of mode of oxidizing of liquid and gas can be effectively combined by unique processing method, so that short the time required to oxidation when preparing, controlled range is larger when time control, appearance that will not be because of the hyperoxidation caused by time control is careless slightly the problem of, oxidation is complete, small investment;Has the advantages that the shortcomings that existing method overcomes existing method again simultaneously.

Description

The method that combination method prepares isotropic graphite material
Technical field
The present invention relates to the methods that the preparation method of graphite material, especially combination method prepare isotropic graphite material.
Background technology
Graphite has the higher capacity of heat transmission, low coefficient of thermal expansion, good flexural strength, compression strength and chemistry steady It is qualitative, it is the indispensable conductive material of national economy and the structural materials such as development metallurgy, chemical industry, electronics and nuclear industry.Commonly Graphite is all " anisotropy " mostly.But many special occasions need the graphite of " isotropism ", such as military project, aerospace, surpass The leading-edge fields such as high power electrodes, nuclear industry graphite, metal mold just need High anti bending strength, compression strength height, thermally expand The low isotropic graphite material of coefficient.Therefore, the preparation of isotropic graphite becomes an important research of high performance graphite Direction.
Conventional prepares there are mainly two types of isotropic graphite materials:One is:Coke aggregate is with pitch binder through mixed Pinch molding, charing, graphitization, the performance of graphite material obtained is not very high under this kind of method, and isotropism degree is poor;It is another Planting is:By with self sintering green coke or mesophase pitch bead green-ball be molded directly into type, then carbonize, be graphitized, should Due to pitch middle-molecular-weihydroxyethyl wider distribution under kind of method, the component of small-molecular-weight is more, and when volatilization is easy to generate gap, is formed and is lacked It falls into, to reduce the performance of graphite, and the effusion of light component makes product be easy cracking.If carrying out appropriateness to pitch not melt Change, it is possible to reduce the component of small-molecular-weight improves the yield rate of product, and it is made to retain enough caking property, such viscous Knot property can play the role of binder during charing, achieve the purpose that, from being sintered, to obtain so-called " single-phase " graphite material Material.
There are mainly two types of the realization methods of cure treatment in existing processing method:
First, air curing:Oxidant is made using the oxygen in air.The method advantage be it is non-fusible the reaction was complete, non-fusible effect Fruit is good, the disadvantage is that time-consuming, investment is big;Especially to the pitch of low softening point, non-fusible temperature and heating rate are difficult control System, non-fusible time are up to tens hours, and non-fusible effect is poor.
Second is that liquid phase is non-fusible:Using liquid oxidizer, can be reduced to dozens of minutes, but this side the non-fusible time Method is very high to oxidant concentration requirement, and time control is stringent, is easy hyperoxidation.
In conclusion using current preparation method when carrying out the preparation of isotropic graphite material, prepared stone The performance of ink material cannot well simultaneously meet macroscopically with it is microcosmic on be all isotropic performance requirement or prepare when Between longer and effect is poor or to prepare short but time control very strict the time, be easy hyperoxidation;Pass through existing method in a word The isotropism degree of the isotropic graphite material of gained is relatively low, and product quality and performances are poor.
Invention content
The present invention is technical solution used by least solving one of above-mentioned technical problem:Combination method prepares isotropism The method of graphite material, includes the following steps:It is soft with the height after Oxygen in Liquid agent and air oxygen agent joint cure treatment It is raw material to change the pitch under dotted state;In the case of binder free, using the caking property that itself retains, by from sintering process Obtain graphite material.
Preferably, the temperature of the high softening-point state is 200-330 DEG C.
Preferably, the preparation method of the raw material includes the following steps:
A1:It is broken:It is 5-30 μm that high softening point bitumen of the softening point between 200-330 DEG C, which is crushed to grain size, obtains asphalt powder Material;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer, reacts 5-20 minutes;The pitch powder and the mass ratio of Oxygen in Liquid agent are 0.05-0.2;It pulls out Afterwards, in air, 200-400 DEG C is risen to 2 DEG C/min, and aoxidizes 1-8h at a temperature of 200-400 DEG C, to reach appropriateness not Fusing degree obtains powdery primary raw materials.
Preferably, described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 800-1000 DEG C under normal pressure, nonoxidizing atmosphere, obtains carbonaceous product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2200-2800 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropism Graphite material.
Preferably, the Oxygen in Liquid agent be mass concentration be 70-90% sulfuric acid, 10-30% nitric acid in one kind or Person is the mixed liquor that the nitric acid of the sulfuric acid that mass concentration is 70-90% and 10-30% are the proportioning composition of 0.5-3 in mass ratio.
Preferably, the temperature of the high softening-point state is 330 DEG C.
Preferably, the grain size of the pitch powder is 25 μm.
Preferably, pitch powder and 10% nitric acid mass ratio be 0.05.
Preferably, in the A2 steps:After pulling out, in air, 400 DEG C are risen to 2 DEG C/min, and in 400 DEG C of temperature Lower oxidation 1h obtains the powdery primary raw materials.
Preferably, in the B2:It is carbonized at 800 DEG C under normal pressure, inert atmosphere protection, constant temperature 1 hour obtains carbonaceous Product;In the B3:It is graphitized at 2600 DEG C under normal pressure, inert atmosphere protection, obtains target product.
Advantageous effect possessed by the present invention is:
1, the present invention selected by high softening point bitumen, no matter macroscopically or it is microcosmic on be all it is isotropic, it is obtained Graphite material has High anti bending strength, the characteristic that compression strength is good, bulk density and isotropism are good.
2, the present invention is combined using the gentle phase oxidation agent of Oxygen in Liquid agent, can be Promethean by unique processing method Two kinds of mode of oxidizing of liquid and gas be effectively combined so that it is short the time required to oxidation when preparation, when time control Controlled range is larger, appearance that will not be because of the hyperoxidation caused by time control is careless slightly the problem of, and oxidation is complete, investment It is few;Has the advantages that the shortcomings that existing method overcomes existing method again simultaneously.
3, the graphite material prepared from sintering using powder, preparation process is simple, binder free, and product quality is stablized, property It can be excellent.
4, resulting product improves preparation efficiency again while disclosure satisfy that production and application, reduces the unqualified of product Rate, whole operation process more easily control.
Specific implementation mode
In order to clarify the technical characteristics of the invention, below by specific implementation mode, the present invention is explained in detail It states.
Embodiment 1:
The method that combination method prepares isotropic graphite material, includes the following steps:With through Oxygen in Liquid agent and air oxygen agent The pitch under high softening-point state after joint cure treatment is raw material;In the case of binder free, retained using itself Caking property, by obtaining graphite material from sintering process;Appropriate cure treatment is exactly to use Oxygen in Liquid agent and air oxygen The method of agent co-oxidation keeps pitch not yet fully crosslinked, also has certain softening properties after heating, not yet fully crosslinked Assurance with the state with certain softening properties can be checked and controlled, judged by the operating personnel of this field, this A little fugitive constituents play the role of binder in carbonization process.
The temperature of the high softening-point state is 200 DEG C, the pitch under the state no matter from macroscopically or it is microcosmic on all It is isotropic, interphase content < 0.1%wt.
The preparation method of the raw material includes the following steps:
A1:It is broken:The high softening point bitumen that softening point is 200 DEG C is crushed to 30 μm of average grain diameter, obtains pitch powder;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer(Use mass concentration for 30% nitric acid)In, it reacts 20 minutes;The pitch powder and Oxygen in Liquid agent Mass ratio be 0.2;After pulling out, in air, 200 DEG C are risen to 2 DEG C/min, and 8h is aoxidized at a temperature of 200 DEG C, to reach To the non-fusible degree of appropriateness, powdery primary raw materials is obtained.
It is described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 800 DEG C under normal pressure, nonoxidizing atmosphere, constant temperature 1 hour obtains carbonaceous Product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2800 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropic graphite Material;Its nonoxidizing atmosphere refers to:In inert gas(Such as nitrogen, argon gas)Equal nonoxidizing atmospheres protection is lower or coke powder buries method isolation Air.
Embodiment 2:
The method that combination method prepares isotropic graphite material, includes the following steps:With through Oxygen in Liquid agent and air oxygen agent The pitch under high softening-point state after joint cure treatment is raw material;In the case of binder free, retained using itself Caking property, by obtaining graphite material from sintering process;Appropriate cure treatment is exactly to use Oxygen in Liquid agent and air oxygen The method of agent co-oxidation keeps pitch not yet fully crosslinked, also has certain softening properties after heating, not yet fully crosslinked Assurance with the state with certain softening properties can be checked and controlled, judged by the operating personnel of this field, this A little fugitive constituents play the role of binder in carbonization process.
The temperature of the high softening-point state is 220 DEG C.
The preparation method of the raw material includes the following steps:
A1:It is broken:The high softening point bitumen that softening point is 220 DEG C is crushed to 20 μm of average grain diameter, obtains pitch powder;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer(The sulfuric acid of mass concentration 90%)In, it reacts 15 minutes;The quality of the pitch powder and Oxygen in Liquid agent Than being 1:8;After pulling out, in air, 250 DEG C are risen to 2 DEG C/min, and 6h is aoxidized at a temperature of 250 DEG C, to reach appropriateness Non-fusible degree obtains powdery primary raw materials.
It is described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 950 DEG C under normal pressure, nonoxidizing atmosphere, constant temperature 1 hour obtains carbonaceous Product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2600 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropic graphite Material;Its nonoxidizing atmosphere refers to:In inert gas(Such as nitrogen, argon gas)Equal nonoxidizing atmospheres protection is lower or coke powder buries method isolation Air.
Embodiment 3:
The method that combination method prepares isotropic graphite material, includes the following steps:With through Oxygen in Liquid agent and air oxygen agent The pitch under high softening-point state after joint cure treatment is raw material;In the case of binder free, retained using itself Caking property, by obtaining graphite material from sintering process;Appropriate cure treatment is exactly to use Oxygen in Liquid agent and air oxygen The method of agent co-oxidation keeps pitch not yet fully crosslinked, also has certain softening properties after heating, not yet fully crosslinked Assurance with the state with certain softening properties can be checked and controlled, judged by the operating personnel of this field, this A little fugitive constituents play the role of binder in carbonization process.
The temperature of the high softening-point state is 250 DEG C.
The preparation method of the raw material includes the following steps:
A1:It is broken:The high softening point bitumen that softening point is 250 DEG C is crushed to 15 μm of average grain diameter, obtains pitch powder;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer(It is 1 in mass ratio by 30% nitric acid and 70% sulfuric acid:3 compositions)In, it reacts 15 minutes;The pitch Powder and the mass ratio of Oxygen in Liquid agent are 1:10;After pulling out, in air, 300 DEG C are risen to 2 DEG C/min, and in 300 DEG C At a temperature of aoxidize 5h, to reach the non-fusible degree of appropriateness, obtain powdery primary raw materials.
It is described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 900 DEG C under normal pressure, nonoxidizing atmosphere, constant temperature 1 hour obtains carbonaceous Product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2400 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropic graphite Material;Its nonoxidizing atmosphere refers to:In inert gas(Such as nitrogen, argon gas)Equal nonoxidizing atmospheres protection is lower or coke powder buries method isolation Air.
Embodiment 4:
The method that combination method prepares isotropic graphite material, includes the following steps:With through Oxygen in Liquid agent and air oxygen agent The pitch under high softening-point state after joint cure treatment is raw material;In the case of binder free, retained using itself Caking property, by obtaining graphite material from sintering process;Appropriate cure treatment is exactly to use Oxygen in Liquid agent and air oxygen The method of agent co-oxidation keeps pitch not yet fully crosslinked, also has certain softening properties after heating, not yet fully crosslinked Assurance with the state with certain softening properties can be checked and controlled, judged by the operating personnel of this field, this A little fugitive constituents play the role of binder in carbonization process.
The temperature of the high softening-point state is 280 DEG C.
The preparation method of the raw material includes the following steps:
A1:It is broken:The high softening point bitumen that softening point is 250 DEG C is crushed to 10 μm of average grain diameter, obtains pitch powder;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer(The nitric acid of mass concentration 20%)In, it reacts 10 minutes;The quality of the pitch powder and Oxygen in Liquid agent Than being 1:13;After pulling out, in air, 350 DEG C are risen to 2 DEG C/min, and 4h is aoxidized at a temperature of 350 DEG C, to reach appropriateness Non-fusible degree obtains powdery primary raw materials.
It is described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 1000 DEG C under normal pressure, nonoxidizing atmosphere, constant temperature 1 hour obtains charcoal Matter product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2800 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropic graphite Material;Its nonoxidizing atmosphere refers to:In inert gas(Such as nitrogen, argon gas)Equal nonoxidizing atmospheres protection is lower or coke powder buries method isolation Air.
Embodiment 5:
The method that combination method prepares isotropic graphite material, includes the following steps:With through Oxygen in Liquid agent and air oxygen agent The pitch under high softening-point state after joint cure treatment is raw material;In the case of binder free, retained using itself Caking property, by obtaining graphite material from sintering process;Appropriate cure treatment is exactly to use Oxygen in Liquid agent and air oxygen The method of agent co-oxidation keeps pitch not yet fully crosslinked, also has certain softening properties after heating, not yet fully crosslinked Assurance with the state with certain softening properties can be checked and controlled, judged by the operating personnel of this field, this A little fugitive constituents play the role of binder in carbonization process.
The temperature of the high softening-point state is 300 DEG C.
The preparation method of the raw material includes the following steps:
A1:It is broken:The high softening point bitumen that softening point is 300 DEG C is crushed to 5 μm of average grain diameter, obtains pitch powder;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer(The sulfuric acid of mass concentration 70%)In, it reacts 10 minutes;The quality of the pitch powder and Oxygen in Liquid agent Than being 1:15;After pulling out, in air, 380 DEG C are risen to 2 DEG C/min, and 3h is aoxidized at a temperature of 380 DEG C, to reach appropriateness Non-fusible degree obtains powdery primary raw materials.
It is described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 1000 DEG C under normal pressure, nonoxidizing atmosphere, constant temperature 1 hour obtains charcoal Matter product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2200 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropic graphite Material;Its nonoxidizing atmosphere refers to:In inert gas(Such as nitrogen, argon gas)Equal nonoxidizing atmospheres protection is lower or coke powder buries method isolation Air.
Embodiment 6:
The method that combination method prepares isotropic graphite material, includes the following steps:With through Oxygen in Liquid agent and air oxygen agent The pitch under high softening-point state after joint cure treatment is raw material;In the case of binder free, retained using itself Caking property, by obtaining graphite material from sintering process;Appropriate cure treatment is exactly to use Oxygen in Liquid agent and air oxygen The method of agent co-oxidation keeps pitch not yet fully crosslinked, also has certain softening properties after heating, not yet fully crosslinked Assurance with the state with certain softening properties can be checked and controlled, judged by the operating personnel of this field, this A little fugitive constituents play the role of binder in carbonization process.
The temperature of the high softening-point state is 330 DEG C.
The preparation method of the raw material includes the following steps:
A1:It is broken:The high softening point bitumen that softening point is 330 DEG C is crushed to 25 μm of average grain diameter, obtains pitch powder;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer(The nitric acid of mass concentration 10%)In, it reacts 10 minutes;The quality of the pitch powder and Oxygen in Liquid agent Than being 1:20;After pulling out, in air, 400 DEG C are risen to 2 DEG C/min, and 1h is aoxidized at a temperature of 400 DEG C, to reach appropriateness Non-fusible degree obtains powdery primary raw materials.
It is described to include the following steps from sintering process:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;Forming method have compression molding, Vibration moulding and isostatic pressing;
B2;Charing:Moulding material in B1 is heated to 800 DEG C under normal pressure, nonoxidizing atmosphere, constant temperature 1 hour obtains carbonaceous Product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2600 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropic graphite Material;Its nonoxidizing atmosphere refers to:In inert gas(Such as nitrogen, argon gas)Equal nonoxidizing atmospheres protection is lower or coke powder buries method isolation Air.
Test example summarizes:
After Shandong carbon materials company carries out many experiments according to above-described embodiment, and carried out for corresponding test example The statistics of the isotropic graphite material property obtained:
Test example particular product performance parameters:
According to the operating method and design parameter of embodiment 1-6, Shandong carbon materials company respectively to according to embodiment 1-6 into 600 kilograms of the graphite material product that row test operation is obtained(Each double centner of each embodiment products obtained therefrom)Carry out property It can detect, the product of acquisition is fully able to meet the requirement produced and used in various performance parameters.
Its concrete outcome is as shown in table 1 below:
Above-mentioned specific implementation mode cannot function as limiting the scope of the invention, and those skilled in the art are come It says, any alternate modification or transformation made to embodiment of the present invention are all fallen in protection scope of the present invention.
Place is not described in detail by the present invention, is the known technology of those skilled in the art of the present technique.

Claims (10)

1. the method that combination method prepares isotropic graphite material, it is characterised in that:Include the following steps:With through Oxygen in Liquid agent The pitch combined with air oxygen agent under the high softening-point state after cure treatment is raw material, by obtaining stone from sintering process Ink material.
2. the method that combination method according to claim 1 prepares isotropic graphite material, it is characterised in that:The height is soft The temperature for changing dotted state is 200-330 DEG C.
3. the method that combination method according to claim 1 prepares isotropic graphite material, it is characterised in that:The raw material Preparation method include the following steps:
A1:It is broken:It is 5-30 μm that high softening point bitumen of the softening point between 200-330 DEG C, which is crushed to grain size, obtains asphalt powder Material;
A2:Powdery primary raw materials is made in Oxygen in Liquid agent and air oxygen agent joint cure treatment:By the pitch powder in A1 It is put into liquid oxidizer, reacts 5-20 minutes;The pitch powder and the mass ratio of Oxygen in Liquid agent are 0.05-0.2;It pulls out Afterwards, in air, 200-400 DEG C is risen to 2 DEG C/min, and aoxidizes 1-8h at a temperature of 200-400 DEG C, it is primary former to obtain powdery Material.
4. the method that combination method according to claim 1 prepares isotropic graphite material, it is characterised in that:It is described to burn certainly Knot technique includes the following steps:
B1;Molding:It is moulding material by the powdery primary raw materials machine-shaping of the gained in A2;
B2;Charing:Moulding material in B1 is heated to 800-1000 DEG C under normal pressure, nonoxidizing atmosphere, obtains carbonaceous product;
B3;Graphitization:Carbonaceous product in B2 is heated to 2200-2800 DEG C under normal pressure, nonoxidizing atmosphere, obtains isotropism Graphite material.
5. the method that combination method according to claim 1 prepares isotropic graphite material, it is characterised in that:The liquid phase Oxidant be mass concentration be 70-90% sulfuric acid, 10-30% nitric acid in a kind of or mass concentration be 70-90% sulphur The nitric acid of acid and 10-30% are the mixed liquor of the proportioning composition of 0.5-3 in mass ratio.
6. the method that combination method according to claim 1 prepares isotropic graphite material, it is characterised in that:The height is soft The temperature for changing dotted state is 330 DEG C.
7. the method that combination method according to claim 3 prepares isotropic graphite material, it is characterised in that:The pitch The grain size of powder is 25 μm.
8. the method that combination method according to claim 3 prepares isotropic graphite material, it is characterised in that:Pitch powder Mass ratio with 10% nitric acid is 0.05.
9. the method that combination method according to claim 3 prepares isotropic graphite material, it is characterised in that:The A2 steps In rapid:After pulling out, in air, 400 DEG C are risen to 2 DEG C/min, and 1h is aoxidized at a temperature of 400 DEG C, it is primary to obtain the powdery Raw material.
10. the method that combination method according to claim 4 prepares isotropic graphite material, it is characterised in that:The B2 In:It is carbonized at 800 DEG C under normal pressure, inert atmosphere protection, constant temperature 1 hour obtains carbonaceous product;In the B3:Normal pressure, It is graphitized at 2600 DEG C under inert atmosphere protection, obtains target product.
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Publication number Priority date Publication date Assignee Title
CN110655413A (en) * 2019-09-18 2020-01-07 济宁碳素集团有限公司 Preparation method of isotropic graphite material

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CN105645960A (en) * 2015-12-11 2016-06-08 天津工业大学 Method for preparing isotropic graphite from isotropic asphalt with high softening point through self-sintering
CN106083049A (en) * 2016-06-16 2016-11-09 山东晨阳新型碳材料股份有限公司 A kind of method preparing isotropic graphite material from sintering

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Publication number Priority date Publication date Assignee Title
CN1349234A (en) * 2000-10-16 2002-05-15 日清纺织株式会社 Carbon material, dual layer capacitor polarizable electrode
CN103046165A (en) * 2013-01-09 2013-04-17 四川创越炭材料有限公司 Preparation method of continuous filament of asphalt-based carbon fiber
CN105645960A (en) * 2015-12-11 2016-06-08 天津工业大学 Method for preparing isotropic graphite from isotropic asphalt with high softening point through self-sintering
CN106083049A (en) * 2016-06-16 2016-11-09 山东晨阳新型碳材料股份有限公司 A kind of method preparing isotropic graphite material from sintering

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110655413A (en) * 2019-09-18 2020-01-07 济宁碳素集团有限公司 Preparation method of isotropic graphite material
CN110655413B (en) * 2019-09-18 2022-03-04 济宁碳素集团有限公司 Preparation method of isotropic graphite material

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Application publication date: 20181019