CN106698414A - Raw material composition and method for preparing special graphite material - Google Patents
Raw material composition and method for preparing special graphite material Download PDFInfo
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- CN106698414A CN106698414A CN201510776771.4A CN201510776771A CN106698414A CN 106698414 A CN106698414 A CN 106698414A CN 201510776771 A CN201510776771 A CN 201510776771A CN 106698414 A CN106698414 A CN 106698414A
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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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
- C01P2006/32—Thermal properties
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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
- C01P2006/40—Electric properties
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Abstract
The invention belongs to the field of graphite materials, and particularly relates to a raw material composition and method for preparing a special graphite material. The raw material composition is prepared from, by weight, 70-75% of isotropic coke and 5-30% of medium temperature coal-tar pitch, and preferably 70-72% of isotropic coke and 28-30% of medium temperature coal-tar pitch. The method comprises the following steps that the isotropic coke is crushed, screened and blended, medium temperature coal-tar pitch is added for mixing kneading, vibration molding, primary roasting, primary impregnation, secondary roasting and graphitization, and the special graphite material is obtained. The physical and chemical indexes of the prepared special graphite material can compare favourably with other mid-to-high end graphite materials and also can replace the mid-to-high end graphite materials; due to the fact that the raw material sources are wide, the price is low, the preparation process is easier, the technical difficulty is low, the production cost is low, the product performance is high, the quality is good, and the price is lower than other similar or mid-to-high end graphite materials, the raw material composition is very successful in business.
Description
Technical field
The invention belongs to graphite material field, specifically, it is related to a kind of feedstock composition for preparing special graphite material and side
Method.
Background technology
Middle-end graphite material, i.e., existing anisotropic graphite product is using after-smithing petroleum coke, medium temperature coal pitch as aggregate
And binding agent, being formed through technique productions such as overmolding, roasting, dipping, graphitization, machinings, the market price is popular,
But its physics and chemistry belongs to anisotropy, quality stability is poor.
High-end graphite material, this refers to isostatic pressing formed graphite product, it has an isotropism, high density, high intensity and non-
Normal uniform characteristic, but the ingredient requirement of isostatic pressed is high, is typically imported raw material, and its existing price is also high, generally 6-10
Ten thousand yuan/ton, and the advanced technologies of isostatic pressed also grasp industrially developed country's hand abroad, China produce big specification,
High density, the Tan Su enterprises of high intensity can be counted on one's fingers.
As application field is constantly widened, special graphite industry welcomes comprehensively quickly development.Special graphite is used as possessing body high
Close, resistivity is low, anti-oxidant, corrosion-resistant, high temperature resistant, conduct electricity very well charcoal element new material, be widely used in partly leading
The various fields such as the processing of body, photovoltaic solar, solar energy thermal-power-generating, electric spark and mould, nuclear energy, metallurgy, space flight.Not
Come in one period, as the quickening of the industries such as the processing of China's semiconductor, photovoltaic solar, electric spark and mould, nuclear power is sent out
Exhibition, the market demand of special graphite will be presented rapid growth situation, especially big specification, fine granularity special graphite will be with good
Good market prospects.Along with the high speed development of science and technology, every field proposes higher to the performance of special graphite material
Requirement.
Special graphite refers to the graphite product (also known as three graphite high, isostatic pressing formed graphite) of high intensity, high density, high-purity, extensively
It is general to be applied to the industrial circles such as metallurgy, chemical industry, space flight, electronics, machinery, nuclear energy.Especially big specification is high-quality high-purity
Graphite, alternatively material, has the application space of broadness, before having a wide range of applications in high-tech, new technical field
Scape, is described as one of 21 century most promising material.
CN102583346A discloses a kind of preparation method of special graphite, is the coal by the carbonaceous material of high-purity and high-purity
Pitch carries out roller sheet, air-flow crushing after being sufficiently mixed in kneading machine, obtains the mixing coke powder of high pure and ultra-fine；Ultra-fine mixing is burnt
Powder first uses cold isostatic compaction, then using high temperature insostatic pressing (HIP) and graphitization processing, just can obtain high performance physicochemical property excellent
More, isotropic requirement is met, technological process is short, energy consumption is low, low production cost, " three wastes " that system is produced are through place
Qualified discharge after reason, reaches national requirements for environmental protection.But use the resistivity of special graphite obtained in the method big, linear heat
The coefficient of expansion is high.
In view of this, it is special to propose the present invention.
The content of the invention
For the various physical and chemical indexs such as bulk density, resistivity, ash, the machinery that solve special graphite material in the prior art are strong
The problems such as spending not good enough, the present invention provides a kind of feedstock composition and method for preparing special graphite material, using the raw material and side
Special graphite material obtained in method has that bulk density is big, purity is high, high temperature resistant, corrosion resistance is strong, inoxidizability is strong, gas
Porosity is low, the low feature of thermal coefficient of expansion, close to isostatic pressed product the characteristics of make its isotropism.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of feedstock composition for preparing special graphite material, wherein, by weight percentage, it is constituted described feedstock composition
For:
Deng side burnt 70~75%
Medium temperature coal pitch 25~30%；
It is preferred that, described feedstock composition by weight percentage, consisting of:
Deng side burnt 70~72%
Medium temperature coal pitch 28~30%.
Special graphite material is a kind of middle and high end graphite products, with extraordinary physical and chemical index, and for middle coarse granule is each
To isotropic material, although the manufacturing technique requirent needed for isostatic pressing formed graphite product properties can fully meet each field, its price
Very expensive, and the domestic high performance isostatic pressing formed graphite product of large scale is in the growth stage, it is quiet that common graphite is unable to reach etc.
Press the physical and chemical index of graphite material.The present inventor researchs and analyses and is produced as a trial with product by many experiments, in terms of raw material selection,
It is final to determine with grade side Jiao for aggregate, medium temperature coal pitch are binding agent, be conducive to obtaining bulk density roasting product higher, favorably
In product percent of pass, and medium temperature coal pitch is improved in the easy graphitization of graphitization process, the physical and chemical index of its final products can be fully
It is met, and infinite approach isostatic pressing formed graphite product.
Further, the burnt particle size range in the grade side is 0 ＜ particle diameters≤0.5mm.
In the preparation technology of graphite product, performance parameter influence of the formula on graphite product is larger, particularly to bulk density, gas
The influence of porosity and thermal coefficient of expansion.The bulk density that in general, obtains product using relatively fine particle formula vibration moulding is big,
The porosity is smaller, bending and compressive strength is high.The present invention chooses highly isotropic, high density, high intensity, low hole in sorting
Rate, fine pore etc. side it is burnt, and in dispensing, using super fine powder, little particle formula, the most aniseed footpath of aggregate is less than or equal to
0.5mm。
It is preferred that, weight percentage, the burnt particle size range in the grade side is with content:
And in the range of 0 ＜ particle diameters≤0.5mm, the distribution of grain diameter directly affects the accumulation mode of particle, particle packing again
Tightr, the bulk density of graphite product is bigger, the porosity is smaller, in addition, in this particle size range, such as keep granularity constant,
Particle mean size is doubled, and coefficient of thermal expansion declines about 7%.The present invention is finally formulated through studying and testing using following aggregate, etc.
Side Jiao accounts for 15~20wt% of total amount by the weight of 0.335mm ＜ particle diameters≤0.5mm；The weight of 0.15mm ＜ particle diameters≤0.330mm
Account for 15~20wt% of total amount；The weight of 0.010mm ＜ particle diameters≤0.075mm accounts for 15~20wt% of total amount；0 ＜ particle diameters ＜
45~50wt% that the weight of 0.075mm accounts for total amount carries out dispensing, and at this moment, the particles of aggregates of different-grain diameter is piled up more closely, stone
The bulk density of Mo Pin, the porosity, mechanical strength and thermal coefficient of expansion can reach an extraordinary balance, prepared graphite system
The bulk density of product is big, the porosity is small, thermal coefficient of expansion is small.
As a kind of most preferably scheme of feedstock composition, weight percentage, the grade side burnt particle size range and content
For:
In the present invention, the grade side is burnt also known as isotropic coke, its real density >=2.12g/cm3, powder resistivity≤150 μ Ω m,
Ash content≤0.25%, hole is 25-55nm.
In the present invention, the softening point of binding agent medium temperature coal pitch is 83-86 DEG C, and coking value is >=48%, during ash content≤0.3%；And
The softening point of impregnating agent impregnating pitch is 83-86 DEG C, and coking value is >=48%, quinoline insolubles≤0.25%.
The present invention also provides a kind of method for preparing special graphite material, and the method is comprised the following steps:Deng the burnt broken, screening in side,
Dispensing, add mid temperature pitch carries out kneading, vibration moulding, once roasting, single-steeping, after baking and graphitization are obtained
Special graphite material；
Wherein, the dispensing is:The mass percent with medium temperature coal pitch burnt Deng side is 70~75%:25~30%；It is preferred that 70~
72%:28~30%.
The present invention uses vibration moulding mode, therefore consumption to binding agent medium temperature coal pitch has strict ratio requirement, glues
The surface area of the consumption and aggregate of tying agent has direct relation, and the particle diameter of aggregate is smaller, and surface area is bigger, and consumption of binder is then more,
But consumption of binder is excessive, and jolt ramming is difficult during shaping, thus the bulk density of product is smaller, and the easy deformation of product after the demoulding.
Binding agent of the present invention is 70 with aggregate proportioning:75-30:25%, after kneading, the thickener for obtaining substantially is not in for aggregate and binding agent
Agglomerate, be poured on it is most of in shot shape, or a little less small agglomerate on the material platform that dries in the air, obtained after shaping bulk density it is higher into
Type product.
The bulk density of the green compact after vibration moulding of the present invention reaches 1.75-1.79g/cm3。
The burnt particle size range in the grade side is 0 ＜ particle diameters≤0.5mm.
It is preferred that, weight percentage, the burnt particle size range in the grade side is with content:
It is further preferred that weight percentage, the burnt particle size range in the grade side is with content:
In the above method, wherein, the kneading is divided into dry blend wet mixing, and the dry-mixed time is 50~55 minutes, dry-mixed
Temperature is 140~160 DEG C；The wet mixing be medium temperature coal pitch is added at twice it is dry-mixed after aggregate in carry out kneading, first
The weight of the medium temperature coal pitch of secondary addition is the 75~85% of total medium temperature coal pitch, and the time of first time kneading is 20~25 minutes；
The weight of the medium temperature coal pitch for adding for second is the 15~25% of total mid temperature pitch, and second time of kneading is 20~25 points
Clock, twice the temperature of kneading be 150~170 DEG C.
The particle of aggregate is smaller, and surface area is bigger, is more difficult to be well mixed when wet mixing, and the time of wet mixing is more long, power consumption
Also increase therewith.The present invention during wet mixing, binding agent is added at twice it is dry-mixed after aggregate in carry out kneading, the
The binding agent and aggregate for once adding the 75-85% for accounting for total binding agent quality are bonded, because the amount for adding is few, the stickiness ratio of mixture
It is relatively low, under the mixing power effect of equal conditions, kneading uniformly, after first time wet mixing, feed particles grain can be made in a short time
Footpath becomes big than more uniform, its specific surface area is diminished, then remaining binding agent is added, and by aggregate and can glue in a short time
Knot agent uniformly mixes.Binding agent mid temperature pitch is added at twice, the time of wet mixing can be both reduced, and reducing energy consumption can make again
Thickener kneading is uniform, obtains the good thickener of plasticity, the yield rate and physical property of green compact after being conducive to raising to be molded.
It is described to be once roasted to：At 150-350 DEG C, heating rate is 1.2-1.6 DEG C/h；At 350-550 DEG C, heating rate
It is 0.8-1 DEG C/h；At 550-850 DEG C, heating rate is 1.2-1.4 DEG C/h；At 850-1150 DEG C, heating rate is 2.2-2.9 DEG C
/h。
The purpose of roasting is to carbonize binder pitch, and coke grid is formed between particles of aggregates, and varigrained aggregate is firm
Be bonded to an entirety., when carbon material is prepared, the probability for occurring crackle in follow-up heat treatment process can be big for little particle formula,
Yield rate may be relatively low, the factor such as heating curve, duration of heat when the present invention is by optimization and improvement roasting, improves
There is the low problem of crackle, yield rate in the coking rate of binding agent, overcome that little particle brings, to ensure product overall target
Yield rate.
A roasting process of the invention is carried out under conditions of air is completely cut off, and maximum temperature reaches 850-1150 DEG C, is being risen
1.2-1.6 DEG C of intensification per hour during 150-350 DEG C of warm area, lightweight fugitive constituent in roasting product is volatilized discharge, roasting with slower speed
Pressure suffered by burning product inside is smaller, more balance, it is to avoid crackle is produced in temperature-rise period, and light components have fully
Time discharge product；The polycondensation reaction enhancing in roasting product at 350-550 DEG C, coke is initially formed, per hour 0.8-1 DEG C of intensification,
Be conducive to improving the coking rate of binding agent, carbonization at low temperature is changed into coking；At 550-850 DEG C, polycondensation reaction continues generation, product
Further coking, per hour 1.2-1.4 DEG C of intensification；Heated up with slower heating rate, be conducive to improving the volume of roasting product
Density and intensity, and avoid roasting product during polycondensation reaction from being cracked when shrinking；At 850-1150 DEG C, per hour
2.2-2.9 DEG C of intensification, is heated up with very fast heating rate, and the institutional framework of roasting product is further densified.
The dipping is using medium temperature coal pitch as impregnating pitch, and dipping process is excellent for impregnating pitch first is heated into 220-320 DEG C
Choosing is heated to 220-260 DEG C, is incubated 1-2.5 hours, then impregnating pitch is risen again to 180-200 DEG C, and impregnating autoclave is carried out to take out true
It is empty, be forced into 1.5Mpa, pressurize 50-60 minute under 1.35Mpa, impregnate；The preheating temperature of pickled product is during dipping
360-380℃。
The softening point of the impregnating agent impregnating pitch is 83-86 DEG C, and coking value is >=48%, quinoline insolubles≤0.25%.
The characteristic of impregnating pitch has important influence to dipping effect, is mainly manifested in asphalt viscosity, quinoline insolubles content and knot
On coke number.Coking value is higher, and the bulk density and mechanical strength of product are bigger after roasting, and coking value rises and increases with softening point
Plus, therefore be conducive to improving the bulk density and mechanical strength of product material as binding agent using softening point coal tar pitch higher,
But impregnating pitch softening point is higher, and relative viscosity is bigger, it is difficult to penetrate into the hole of pickled product, asphalt viscosity is both by this
Body property influences, and is inversely proportional with heating-up temperature height.Be improve dipping effect, the present invention one be from softening point be 83-86 DEG C,
Coking value is >=48% pitch, two is that impregnating pitch is heated, to reduce the viscosity of impregnating pitch.In general, super
After crossing 200 DEG C, the light components in pitch start volatilization, 200-400 DEG C be the light components in impregnating pitch volatilization period,
And with the rising of temperature, the molecular weight of the light components volatilized in impregnating pitch gradually increases, the gas of volatilization enters dipping
In the stomata of product, the infiltration of pitch is hampered, so in the prior art, leaching is started after impregnating pitch is heated into 160-180 DEG C
Stain, impregnating pitch heating temperature not over 200 DEG C, but, because the preheating temperature of the carbonaceous product that need to be impregnated typically all exists
Between 300-400 DEG C, so during dipping, still thering are light components to be volatilized from the impregnating pitch in the carbonaceous product of dipping
Out, the infiltration of impregnating pitch is not only hampered, the aperture of many gases is also formd in pickled product, the present invention is in dipping
Before, impregnating pitch is first heated to 220-320 DEG C, it is preferably heated to 220-260 DEG C so that the part lightweight group in impregnating pitch
Divide volatilization to go out, the volatile small molecule in part is volatilized away, impregnating pitch is cooled to 180-200 DEG C again afterwards
Impregnated again, at this moment, impregnating pitch still has than relatively low viscosity, in being easier to penetrate into pickled product, present invention dipping
When pickled product 360-380 DEG C of preheating temperature, dipping when, because part light components volatilize away in impregnating pitch,
The coking value of impregnating pitch is not only increased, the infiltration of impregnating pitch has been also speeded up, and reduces the porosity in immersion oil product,
The effect of dipping is good, is conducive to improving the physical and chemical index of product.In dipping, first the carbonaceous product to be impregnated are vacuumized, take out true
Empty purpose is the gas of the carbonaceous product pore interior that discharge need to impregnate, and is beneficial to the infiltration of impregnating pitch, after adding impregnating pitch,
Under the effect of the pressure, soak clear pitch to be easier in the hole for penetrate into the carbonaceous product that need to be impregnated, so as to ensure rate of body weight gain；
Quinoline insolubles in coal tar pitch is a kind of small particle, and quinoline insolubles forms thin film in porous material surface during dipping,
Infiltration of the impregnating agent to porous material is hindered, therefore, impregnating pitch of the present invention from quinoline insolubles≤0.2%.
The time of two roasting is 300-330 hours, and the maximum temperature of after baking is up to 800 DEG C.
The graphited time is 450-500 hours, and graphited maximum temperature is 2850-3100 DEG C.
Compared with prior art, the invention has the advantages that：
The present invention is with real density >=2.12g/cm3, powder resistivity≤150 μ Ω m, ash content≤0.25%, hole is 25-55nm
Grade side it is burnt for aggregate and softening point are 83-86 DEG C, coking value is >=48%, the medium temperature coal pitch of ash content≤0.3% is binding agent；
Using super fine powder, little particle formula by optimizing and improving preparation technology, liter during especially by optimization and improvement roasting
Warm curve, the duration of heat, and heating, warming up treatment to impregnating pitch, the physics and chemistry of the special graphite material of preparation
Performance indications can match in excellence or beauty other middle and high end graphite materials, also alternative other middle and high end graphite materials, with its raw material sources it is wide,
Price is low, preparation technology is relatively easy, and technical difficulty is low, and low production cost, properties of product are high, quality upper strata, its price
Than other similar or middle and high end graphite materials, great success has been commercially available.
Specific embodiment
It is below specific embodiment of the invention, described embodiment is in order to further describe the present invention, rather than limitation
The present invention.
Embodiment 1
Will etc. side is burnt broken, screening, and carry out dispensing in the following manner：
By above-mentioned material put into kneading pot in carry out it is dry-mixed, dry-mixed temperature be 150 DEG C, the dry-mixed time be 52 minutes, done
Siccative after mixed.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 71%：
29%.Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the middle temperature coal drip for adding for the first time
Blue or green weight is the 80% of total medium temperature coal pitch, and the time of first time kneading is 22 minutes；The middle temperature coal drip for adding for second
Blue or green weight is the 20% of total mid temperature pitch, and second time of kneading is 22 minutes, and the temperature of kneading is 160 DEG C twice.
Twice thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.78g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.4 DEG C/h；At 350-550 DEG C, heating rate is 0.9 DEG C/h；At 550-850 DEG C, heating rate is 1.3 DEG C/h；
At 850-1150 DEG C, heating rate is 2.5 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming
The temperature range of instrument is in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 370 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 280 DEG C, 240 DEG C are preferably heated to, 2 hours are incubated, then by medium temperature coal pitch
Rise again to 190 DEG C, be added in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, the pressurize under 1.35Mpa
55 minutes, a roasting product is impregnated, obtain pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 320 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 480 hours, graphitization highest
Temperature is 3000 DEG C.Special graphite material is obtained after coming out of the stove.
Embodiment 2
Will etc. side is burnt broken, screening, and carry out dispensing in the following manner：
By above-mentioned material put into kneading pot in carry out it is dry-mixed, dry-mixed temperature be 140 DEG C, the dry-mixed time be 55 minutes, done
Siccative after mixed.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 70：30%.
Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the weight of the medium temperature coal pitch for adding for the first time
It is the 75% of total medium temperature coal pitch to measure, and the time of first time kneading is 20 minutes；The weight of the medium temperature coal pitch for adding for second
It is the 25% of total mid temperature pitch to measure, and second time of kneading is 20 minutes, and the temperature of kneading is 170 DEG C twice.Twice
Thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.75g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.2 DEG C/h；At 350-550 DEG C, heating rate is 0.8 DEG C/h；At 550-850 DEG C, heating rate is 1.2 DEG C/h；
At 850-1150 DEG C, heating rate is 2.2 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming
The temperature range of instrument is in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 360 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 220 DEG C, 1 hour is incubated, then medium temperature coal pitch is risen again to 180 DEG C, added
To in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, pressurize 50 minutes under 1.35Mpa, to once roasting
Burning product are impregnated, and obtain pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 300 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 450 hours, graphitization highest
Temperature is 2850 DEG C.Special graphite material is obtained after coming out of the stove.
Embodiment 3
Will etc. side is burnt broken, screening, and carry out dispensing in the following manner：
By above-mentioned material put into kneading pot in carry out it is dry-mixed, dry-mixed temperature be 160 DEG C, the dry-mixed time be 50 minutes, done
Siccative after mixed.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 72%：
28%.Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the middle temperature coal drip for adding for the first time
Blue or green weight is the 85% of total medium temperature coal pitch, and the time of first time kneading is 25 minutes；The middle temperature coal drip for adding for second
Blue or green weight is the 15% of total mid temperature pitch, and second time of kneading is 25 minutes, and the temperature of kneading is 150 DEG C twice.
Twice thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.79g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.6 DEG C/h；At 350-550 DEG C, heating rate is 1 DEG C/h；At 550-850 DEG C, heating rate is 1.4 DEG C/h；
At 850-1150 DEG C, heating rate is 2.9 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming instrument
Temperature range in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 380 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 320 DEG C, 2.5 hours are incubated, then medium temperature coal pitch is risen again to 200 DEG C, plus
Enter in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, pressurize 60 minutes under 1.35Mpa, to once
Roasting product is impregnated, and obtains pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 330 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 500 hours, graphitization highest
Temperature is 3100 DEG C.Special graphite material is obtained after coming out of the stove.
Embodiment 4
Will etc. side is burnt broken, screening, and carry out dispensing in the following manner：
By above-mentioned material put into kneading pot in carry out it is dry-mixed, dry-mixed temperature be 145 DEG C, the dry-mixed time be 52 minutes, done
Siccative after mixed.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 75%：
25%.Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the middle temperature coal drip for adding for the first time
Blue or green weight is the 82% of total medium temperature coal pitch, and the time of first time kneading is 23 minutes；The middle temperature coal drip for adding for second
Blue or green weight is the 18% of total mid temperature pitch, and second time of kneading is 23 minutes, and the temperature of kneading is 155 DEG C twice.
Twice thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.77g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.5 DEG C/h；At 350-550 DEG C, heating rate is 0.85 DEG C/h；At 550-850 DEG C, heating rate is 1.25 DEG C/h；
At 850-1150 DEG C, heating rate is 2.7 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming
The temperature range of instrument is in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 365 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 270 DEG C, 1.8 hours are incubated, then medium temperature coal pitch is risen again to 195 DEG C, plus
Enter in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, pressurize 58 minutes under 1.35Mpa, to once
Roasting product is impregnated, and obtains pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 325 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 485 hours, graphitization highest
Temperature is 2980 DEG C.Special graphite material is obtained after coming out of the stove.
Embodiment 5
Will etc. side is burnt broken, screening, and carry out dispensing in the following manner：
By above-mentioned material put into kneading pot in carry out it is dry-mixed, dry-mixed temperature be 156 DEG C, the dry-mixed time be 51 minutes, done
Siccative after mixed.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 74%：
26%.Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the middle temperature coal drip for adding for the first time
Blue or green weight is the 79% of total medium temperature coal pitch, and the time of first time kneading is 21 minutes；The middle temperature coal drip for adding for second
Blue or green weight is the 21% of total mid temperature pitch, and second time of kneading is 21 minutes, and the temperature of kneading is 157 DEG C twice.
Twice thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.76g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.3 DEG C/h；At 350-550 DEG C, heating rate is 0.95 DEG C/h；At 550-850 DEG C, heating rate is 1.35 DEG C/h；
At 850-1150 DEG C, heating rate is 2.7 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming
The temperature range of instrument is in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 376 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 258 DEG C, 2.3 hours are incubated, then medium temperature coal pitch is risen again to 194 DEG C, plus
Enter in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, pressurize 57 minutes under 1.35Mpa, to once
Roasting product is impregnated, and obtains pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 315 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 478 hours, graphitization highest
Temperature is 3050 DEG C.Special graphite material is obtained after coming out of the stove.
Embodiment 6
Will etc. side is burnt broken, screening；
Grade side Jiao of 0 ＜ particle diameters≤0.5mm is put into and carried out in kneading pot dry-mixed, dry-mixed temperature is 153 DEG C, and the dry-mixed time is
53 minutes, obtain it is dry-mixed after siccative.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 74%：
26%.Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the middle temperature coal drip for adding for the first time
Blue or green weight is the 83% of total medium temperature coal pitch, and the time of first time kneading is 21 minutes；The middle temperature coal drip for adding for second
Blue or green weight is the 17% of total mid temperature pitch, and second time of kneading is 21 minutes, and the temperature of kneading is 161 DEG C twice.
Twice thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.77g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.4 DEG C/h；At 350-550 DEG C, heating rate is 0.9 DEG C/h；At 550-850 DEG C, heating rate is 1.3 DEG C/h；
At 850-1150 DEG C, heating rate is 2.4 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming
The temperature range of instrument is in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 369 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 238 DEG C, 1.8 hours are incubated, then medium temperature coal pitch is risen again to 188 DEG C, plus
Enter in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, pressurize 53 minutes under 1.35Mpa, to once
Roasting product is impregnated, and obtains pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 308 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 468 hours, graphitization highest
Temperature is 2980 DEG C.Special graphite material is obtained after coming out of the stove.
Embodiment 7
By real density >=2.12g/cm3, powder resistivity≤150 μ Ω m, ash content≤0.25%, hole for 25-55nm etc.
Side is burnt broken, screening, puts into and carried out in kneading pot dry-mixed, and dry-mixed temperature is 150 DEG C, and the dry-mixed time is 52 minutes, is obtained
Siccative after dry-mixed.
After the completion of dry-mixed, to medium temperature coal pitch is added in kneading pot, the mass percent of siccative and medium temperature coal pitch is 71%：
29%.Wherein, medium temperature coal pitch be added at twice it is dry-mixed after siccative in carry out kneading, the middle temperature coal drip for adding for the first time
Blue or green weight is the 80% of total medium temperature coal pitch, and the time of first time kneading is 22 minutes；The middle temperature coal drip for adding for second
Blue or green weight is the 20% of total mid temperature pitch, and second time of kneading is 22 minutes, and the temperature of kneading is 160 DEG C twice.
Twice thickener is obtained after the completion of kneading.
Thickener is put into the material machine that dries in the air carries out material operation of drying in the air, and when thickener temperature is down to 120 DEG C, thickener is put into vibrating forming machine mould
Vibration moulding is carried out in tool, the bulk density of the green compact after shaping reaches 1.78g/cm3, and ensure the green compact flawless after shaping.
Green compact after shaping are put into roaster and are once calcined, one time Baking profile is：At 150-350 DEG C, heat up speed
Rate is 1.4 DEG C/h；At 350-550 DEG C, heating rate is 0.9 DEG C/h；At 550-850 DEG C, heating rate is 1.3 DEG C/h；
At 850-1150 DEG C, heating rate is 2.5 DEG C/h.Whole temperature-rise period temperature alarming instrument is controlled, it is ensured that temperature alarming
The temperature range of instrument is in 5 DEG C, it is ensured that product flawless.A roasting product is obtained after the completion of being once calcined.
Roasting product is put into preheating furnace and is preheated, preheating temperature is 370 DEG C, and roasting product is taken out from preheating furnace, is put
Enter in impregnating autoclave；Medium temperature coal pitch is heated to 280 DEG C, 240 DEG C are preferably heated to, 2 hours are incubated, then by medium temperature coal pitch
Rise again to 190 DEG C, be added in impregnating autoclave, impregnating autoclave is vacuumized, 1.5Mpa is forced into, the pressurize under 1.35Mpa
55 minutes, a roasting product is impregnated, obtain pickled product；
Pickled product is put into carries out after baking in roaster, the time of after baking is 320 hours, the highest temperature of after baking
Degree obtains after baking product up to 800 DEG C.
After baking product are put into acheson furnace carries out graphitization, and graphitization time is 480 hours, graphitization highest
Temperature is 3000 DEG C.Special graphite material is obtained after coming out of the stove.
Test example 1
Performance parameter to the special graphite material sample obtained by embodiment 1-7 is detected, as a result as shown in table 1 below：
Table 1
Comparative example 1
The comparative example compares influence of the assistant ingredients to special graphite material property parameter.
Sample 1：Special graphite material obtained in embodiment 1；
Sample 2：Using the preparation method of embodiment 1, difference be use calcined coke to replace etc. square Jiaozhuo is aggregate, forge
The particle size range burnt is with content：
Sample 3：Using the preparation method of embodiment 1, difference is that the particle size range and content of grade side Jiao are：
0.5mm ＜ particle diameters≤0.6mm 100wt%.
Sample 4：Using the preparation method of embodiment 1, difference is that the particle size range and content of grade side Jiao are：
Sample 5：Using the preparation method of embodiment 1, difference is that the particle size range and content of grade side Jiao are：
Performance parameter to sample 1-5 is detected, as a result as shown in table 2 below：
Table 2
Comparative example 2
The comparative example compares the influence to special graphite material property parameter using a different Baking profiles.
Trial target：Special graphite material obtained in embodiment 1；
Reference substance 1：With reference to the preparation method of embodiment 1, the difference with the preparation method of embodiment 1 is：Once it is calcined bent
Line is：At 150-550 DEG C, heating rate is 1.2 DEG C/h；At 550-700 DEG C, heating rate is 0.6 DEG C/h；In 700-1150
Heating rate is 2.1 DEG C/h.
Reference substance 2：Difference with the preparation method of embodiment 1 is：One time Baking profile is：At 150-350 DEG C, rise
Warm speed is 1.4 DEG C/h；At 350-550 DEG C, heating rate is 1.2 DEG C/h；At 550-850 DEG C, heating rate is 1.3 DEG C
/h；At 850-1150 DEG C, heating rate is 2.5 DEG C/h.
Trial target and reference substance 1, the performance parameter of reference substance 2 are detected, it is as a result as shown in table 3 below：
Table 3
Claims (10)
1. a kind of feedstock composition for preparing special graphite material, it is characterised in that described feedstock composition by weight percentage,
Consisting of:
Deng side burnt 70~75%
Medium temperature coal pitch 25~30%；
It is preferred that, described feedstock composition by weight percentage, consisting of:
Deng side burnt 70~72%
Medium temperature coal pitch 28~30%.
2. feedstock composition according to claim 1, it is characterised in that the burnt particle size range in described grade side is 0 ＜
Footpath≤0.5mm；
It is preferred that, weight percentage, the burnt particle size range in the grade side is with content:
It is further preferred that weight percentage, the burnt particle size range in the grade side is with content:
3. feedstock composition according to claim 1 and 2, it is characterised in that the burnt real density in described grade side >=
2.12g/cm3, powder resistivity≤150 μ Ω m, ash content≤0.25%, hole is 25-55nm.
4. a kind of method for preparing special graphite material, it is characterised in that described method is comprised the following steps:Deng the broken of side Jiao
Broken, screening, dispensing, add mid temperature pitch carry out kneading, vibration moulding, once roasting, single-steeping, after baking and
Graphitization obtains special graphite material；
Wherein, the dispensing is:The mass percent with medium temperature coal pitch burnt Deng side is 70~75%:25~30%；It is preferred that 70~
72%:28~30%.
5. method according to claim 4, it is characterised in that the burnt particle size range in the grade side is 0 ＜ particle diameters≤0.5mm；
It is preferred that, weight percentage, the burnt particle size range in the grade side is with content:
It is further preferred that weight percentage, the burnt particle size range in the grade side is with content:
6. the method according to claim 4 or 5, it is characterised in that the kneading is divided into dry blend wet mixing, described dry-mixed
Time be 50~55 minutes, dry-mixed temperature is 140~160 DEG C；The wet mixing is to be added to medium temperature coal pitch at twice
Kneading is carried out in aggregate after dry-mixed, the weight of the medium temperature coal pitch for adding for the first time is the 75~85% of total medium temperature coal pitch,
The time of first time kneading is 20~25 minutes；The weight of second medium temperature coal pitch for adding be total mid temperature pitch 15~
25%, second time of kneading is 20~25 minutes, and the temperature of kneading is 150~170 DEG C twice.
7. method according to claim 6, it is characterised in that described to be once roasted to：At 150-350 DEG C, heat up
Speed is 1.2-1.6 DEG C/h；At 350-550 DEG C, heating rate is 0.8-1 DEG C/h；At 550-850 DEG C, heating rate is
1.2-1.4℃/h；At 850-1150 DEG C, heating rate is 2.2-2.9 DEG C/h.
8. the method according to claim 6 or 7, it is characterised in that the dipping is dripped using medium temperature coal pitch as dipping
Green grass or young crops, dipping process is preferably heated to 220-260 DEG C for impregnating pitch first is heated into 220-320 DEG C, is incubated 1-2.5 hours,
Impregnating pitch is risen again to 180-200 DEG C again, impregnating autoclave is vacuumized, 1.5Mpa is forced into, the pressurize under 1.35Mpa
50-60 minutes, dipping；The preheating temperature of pickled product is 360-380 DEG C during dipping.
9. method according to claim 8, it is characterised in that the times of two roasting are 300-330 hours, secondary
The maximum temperature of roasting is up to 800 DEG C.
10. method according to claim 9, it is characterised in that the graphited time is 450-500 hours, stone
The maximum temperature of inkization is 2850-3100 DEG C.
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| CN108101045A (en) * | 2017-12-18 | 2018-06-01 | 大同新成新材料股份有限公司 | A kind of preparation method of carbon product |
| CN108341669A (en) * | 2018-03-29 | 2018-07-31 | 中钢集团新型材料（浙江）有限公司 | High temperature gas cooled reactor in-pile component big specification nuclear graphite materials and preparation method |
| CN108794011A (en) * | 2018-07-05 | 2018-11-13 | 自贡东新电碳有限责任公司 | A kind of preparation method from sintering carbon graphite sealing material |
| CN108862272A (en) * | 2018-08-21 | 2018-11-23 | 大同新成新材料股份有限公司 | A method of expanded graphite is prepared using graphene oxide, nano-carbon powder |
| CN109081695A (en) * | 2018-07-24 | 2018-12-25 | 中钢集团新型材料（浙江）有限公司 | The preparation method of the molten salt reactor ultra-fine aperture nuclear graphite materials of high density large scale |
| CN109852081A (en) * | 2018-12-20 | 2019-06-07 | 淄博大陆石墨科技有限公司 | The preparation method that vibration-compression molding special graphite is homogenized with thickener |
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| CN115108833A (en) * | 2022-08-03 | 2022-09-27 | 湖北东南佳特碳新材料有限公司 | Continuous casting graphite material and preparation method thereof |
| CN115215655A (en) * | 2022-08-09 | 2022-10-21 | 中钢集团南京新材料研究院有限公司 | Kneading method of isostatic pressing graphite product and product thereof |
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| CN108101045A (en) * | 2017-12-18 | 2018-06-01 | 大同新成新材料股份有限公司 | A kind of preparation method of carbon product |
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| CN108862272A (en) * | 2018-08-21 | 2018-11-23 | 大同新成新材料股份有限公司 | A method of expanded graphite is prepared using graphene oxide, nano-carbon powder |
| CN109852081B (en) * | 2018-12-20 | 2021-07-30 | 淄博大陆石墨科技有限公司 | Preparation method of paste homogenization for special graphite by vibration-compression molding |
| CN109852081A (en) * | 2018-12-20 | 2019-06-07 | 淄博大陆石墨科技有限公司 | The preparation method that vibration-compression molding special graphite is homogenized with thickener |
| CN110981483A (en) * | 2019-11-22 | 2020-04-10 | 大同新成新材料股份有限公司 | Method for preparing graphite electrode joint material by utilizing isotropic coke |
| CN115108833A (en) * | 2022-08-03 | 2022-09-27 | 湖北东南佳特碳新材料有限公司 | Continuous casting graphite material and preparation method thereof |
| CN115108833B (en) * | 2022-08-03 | 2023-08-18 | 湖北东南佳特碳新材料有限公司 | Continuous casting graphite material and preparation method thereof |
| CN115215655A (en) * | 2022-08-09 | 2022-10-21 | 中钢集团南京新材料研究院有限公司 | Kneading method of isostatic pressing graphite product and product thereof |
| CN117800743A (en) * | 2024-02-28 | 2024-04-02 | 淄博大陆石墨科技有限公司 | Roasting method of carbon impregnated product |
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