CN104477902B - Porous aggregate preparation method and the preparation technology of high strength graphite thereof - Google Patents
Porous aggregate preparation method and the preparation technology of high strength graphite thereof Download PDFInfo
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Abstract
The embodiment of the invention discloses a kind of porous aggregate preparation method and the preparation technology of high strength graphite thereof, wherein, described porous aggregate preparation method includes: pulverizes petroleum coke, sieve, and chooses 2 5mm petroleum coke particles of uniform size；Quickly through continuous graphite gasifying device, described petroleum coke particles is carried out the semi-graphited that temperature is 1,500 2000 DEG C process, and obtain described porous aggregate.The porous aggregate preparation method provided by the embodiment of the present invention such that it is able to obtain uniformity, and there is the porous aggregate material of high porosity, thus be effectively improved porous aggregate material and combine with other bonding agents the intensity of the isostatic pressing formed graphite prepared.
Description
Technical field
The present invention relates to machining graphite technical field, particularly relate to preparation method and the high strength graphite of a kind of porous aggregate
Preparation technology.
Background technology
Isostatic pressing formed graphite is formed by high purity graphite compacting.Isostatic pressing formed graphite is the new product that immediate and mid-term grows up in the world
Product, closely coupled with current high-tech；Not only fully develop talents on civilian, national defence highly sophisticated products also occupy importantly
Position, belongs to new material.Isostatic pressing formed graphite is not only manufacture single crystal growing furnace, metal continuous cast graphite crystallizer, spark machined
With irreplaceable materials such as graphite electrodes, and it is to manufacture rocket nozzle, the decelerating material of graphite reactor and reflecting material
The excellent material of material.
In recent years, along with the fast development of domestic photovoltaic industry, domestic isostatic pressing formed graphite demand expands year by year.Meanwhile,
Owing to domestic isostatic pressing formed graphite manufacturing enterprise technical foundation is weak, add the blockade on new techniques of overseas enterprise, the isostatic pressed of China
Yield and the quality of graphite are the most effectively promoted.Such as 2011, domestic isostatic pressing formed graphite demand reached 1.8
Ten thousand tons, and the isostatic pressing formed graphite yield same period is only 9500 tons, supply breach reaches 8500 tons.At present, domestic to isostatic pressed
The preparation method that graphite generally uses is by crushing after-smithing petroleum coke, pitch coke, and carries out pulverizing, qualified
Powder dispensing in proportion also mixes, and by mixed mixture carries out roll, and carries out the tablet after roll
Cooling, pulverizing, compressing, in roaster, then carry out roasting, and the tablet after roasting is carried out pitch pressurization leaching
Stain, finally purifies graphitization and forms.
For in domestic conventional machining graphite production technology, although the isostatic pressing formed graphite drawing certain specification can be produced,
But, owing to prior art being limited only to manufacturing process, such as hot pressing temperature, temperature increasing schedule, granular size, bonding agent
Isostatic pressing formed graphite is improved by the factors such as the proportioning with aggregate so that the pressure resistance of the isostatic pressing formed graphite that existing technique produces
Degree and bend resistance intensity are relatively low, cause domestic isostatic pressing formed graphite product quality and yield rate all ratios relatively low, thus can not meet
Home products demand.
Summary of the invention
The embodiment of the present invention provides a kind of porous aggregate preparation method and the preparation technology of high strength graphite thereof, to solve
Comprcssive strength and the bend resistance intensity of the isostatic pressing formed graphite that prior art produces are relatively low, cause domestic isostatic pressing formed graphite product matter
Amount and yield rate all ratios are relatively low, thus the problem that home products demand can not be met.
In order to solve above-mentioned technical problem, the embodiment of the invention discloses following technical scheme:
Embodiments provide a kind of porous aggregate preparation method, including:
Petroleum coke is pulverized, sieves, and choose 2-5mm petroleum coke particles of uniform size；
Described petroleum coke particles is carried out at the semi-graphited that temperature is 1500-2000 DEG C quickly through continuous graphite gasifying device
Reason, and obtain described porous aggregate.
Optionally, the described petroleum coke particles holdup time in described continuous graphite gasifying device is less than or equal to 0.5 hour.
Optionally, in described petroleum coke particles carries out semi-graphited processing procedure, described continuous graphite gasifying device is passed through
Appropriate oxidizing gas.
The embodiment of the present invention also provides for the preparation technology of a kind of high strength graphite, including:
(1) porous aggregate as claimed in claim 1 and coal tar pitch are chosen, and respectively by described porous aggregate
It is powder with described coal tar pitch comminution by gas stream；
(2) described coal tar pitch is melted into hard pitch solution, according to porous aggregate and the phase of hard pitch solution
Answer ratio to be slowly added in described hard pitch solution by porous aggregate powder, stir successively, be dried, kneading is formed mixed
Compound, and carry out described mixture rolling sheet for the first time；
(3) mixture after rolling sheet for the first time carries out crushing, sieving, and the mixture after sieving carries out second time and rolls
Sheet, and the mixture after rolling sheet for the second time is pulverized, sieved, strengthened powder body；
(4) described reinforcement powder body is carried out successively compression molding, roasting, dipping, and the product after dipping is carried out slightly
Powder after broken and comminution by gas stream, and comminution by gas stream sieves and obtains high-strength powder body；
(5) described high-strength powder body is carried out compression molding, roasting successively；
(6) product after roasting is impregnated, roasting；
(7) product after roasting is warming up to 2400 DEG C with the heating rate of 160 DEG C/h under ar gas environment, and insulation 1
Hour, thus complete graphitization and purification, obtain described high strength graphite.
Optionally, described step (2) farther includes:
By toluene, described coal tar pitch is melted into hard pitch solution；
Described porous aggregate powder and described hard pitch solution are with (63-75): the ratio of (37-25), by described porous
Aggregate powder is slowly added in hard pitch solution, and hard pitch solution described in uniform stirring and described porous aggregate powder
End；
Mixture after stirring is dried process, and in the environment of temperature is 75-100 DEG C, to dried described
Hard pitch solution and mixture kneading 0.5-3 hour of described porous aggregate powder；
In the environment of temperature is 130-170 DEG C, the mixture after kneading carries out rolling for the first time sheet, and rolls sheet for the first time
The sheet number of times that rolls be 1-10 time.
Optionally, described step (3) farther includes:
Mixture after rolling sheet for the first time in described step (2) cools down；
Mixture after cooling is crushed, and the compound particles obtaining size less than 0.5mm that sieves；
In the environment of temperature is 130-170 DEG C, described compound particles is carried out second time and rolls sheet, and second time rolls sheet
The sheet number of times that rolls be 1-10 time；
Mixture after second time is rolled sheet is pulverized, is crossed 100-200 mesh sieve, and strengthened powder body.
Optionally, described step (5) farther includes:
The oleic acid of incorporation 0.8-2.5wt% in the described high-strength powder body obtained in described step (4), first pre-molding,
Isostatic pressing obtains base substrate again；
By the base substrate of isostatic pressing in a nitrogen environment with the ramp of 5 DEG C/h to 850-1050 DEG C, complete roasting.
Optionally, the pressure when product after pre-molding carries out isostatic pressing is 80-200Mpa, and the dwell time is
15 minutes.
Optionally, described step (6) farther includes:
Product after roasting in described step (5) is heated；
Product after heating is put into the pressure vessel filling mid temperature pitch solution, and at 250 DEG C and the environment of 3.5Mpa
Under, the described product after heating is impregnated at least 5 hours in mid temperature pitch solution；
Product after dipping is carried out roasting at the highest sintering temperature is 850-950 DEG C.
Optionally, described step (6) also includes:
Product after roasting is heated；
Product after heating is put into the pressure vessel filling hard pitch solution, and at 325 DEG C and the environment of 4.5Mpa
Under, the described product after heating is impregnated at least 4 hours in hard pitch solution；
Product after dipping is carried out roasting at the highest sintering temperature is 850-900 DEG C.
From above technical scheme, the porous aggregate preparation method that the embodiment of the present invention provides includes choosing 2-5mm size
Uniform petroleum coke particles, and petroleum coke particles is carried out temperature quickly through continuous graphite gasifying device be 1500-2000 DEG C
Semi-graphited process, thus obtain porous aggregate；And, need to add oxidation in carrying out semi-graphited processing procedure
Property gas；Process by using semi-graphited technique that petroleum coke particles is carried out semi-graphited in continuous graphite gasifying device
To porous aggregate such that it is able to obtain uniformity, and there is the porous aggregate material of high porosity, improve bonding agent and
The interface cohesion effect of porous aggregate, thus be effectively improved porous aggregate material combine with other bonding agents preparation etc. quiet
The intensity of pressure graphite.
Further, the preparation method of the high strength graphite that the embodiment of the present invention provides, by choosing petroleum coke porous aggregate
And coal tar pitch, and be hard pitch solution by coal tar pitch melting, according to petroleum coke porous aggregate powder and high temperature
The ratio of Colophonium carries out mix and blend, by hard pitch, porous aggregate powder is carried out liquid phase coating, mixes after drying
Pinch, crush, preforming, second-time breakage, post forming, isostatic pressing, the most at high temperature under high pressure at cold primer-oil
Middle dipping and carry out roasting in roaster, finally by carrying out graphitization and purification under the high temperature of 2400 DEG C, thus
It is effectively improved the intensity of strength graphite material, makes the comprcssive strength of high strength graphite and rupture strength to significantly improve.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In technology description, the required accompanying drawing used is briefly described, it should be apparent that, for those of ordinary skill in the art
Speech, on the premise of not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
The schematic flow sheet of a kind of porous aggregate preparation method that Fig. 1 provides for the embodiment of the present invention；
The schematic flow sheet of the preparation technology of a kind of high strength graphite that Fig. 2 provides for the embodiment of the present invention；
The schematic flow sheet of the preparation technology of the another kind of high strength graphite that Fig. 3 provides for the embodiment of the present invention；
The schematic flow sheet of the preparation technology of another high strength graphite that Fig. 4 provides for the embodiment of the present invention；
The schematic flow sheet of the preparation technology of another high strength graphite that Fig. 5 provides for the embodiment of the present invention；
The schematic flow sheet of the preparation technology of the another kind of high strength graphite that Fig. 6 provides for the embodiment of the present invention.
Detailed description of the invention
For the technical scheme making those skilled in the art be more fully understood that in the present invention, implement below in conjunction with the present invention
Accompanying drawing in example, is clearly and completely described the technical scheme in the embodiment of the present invention, it is clear that described reality
Executing example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, ability
The every other embodiment that territory those of ordinary skill is obtained under not making creative work premise, all should belong to this
The scope of invention protection.
See Fig. 1, for the schematic flow sheet of a kind of porous aggregate preparation method that the embodiment of the present invention provides.
As it is shown in figure 1, the porous aggregate preparation method that the embodiment of the present application provides includes:
Step S10: petroleum coke is pulverized, sieves, and choose 2-5mm petroleum coke particles of uniform size；
Wherein, first select petroleum coke, by pulverizer or other disintegrating apparatus, volume or larger-size petroleum coke are entered
Row pulverize, and will pulverize after petroleum coke sieved by sieve device, the slot size of this sieve device can be
2-5mm, thus choose the size after screening uniformly and the petroleum coke particles of a size of 2-5mm size.
Step S20: petroleum coke particles is carried out, quickly through continuous graphite gasifying device, half stone that temperature is 1500-2000 DEG C
Inkization processes, and obtains porous aggregate；
Wherein, carry out in semi-graphited processing procedure at this petroleum coke particles by this continuous graphite gasifying device, this petroleum coke
The time that granule is detained in continuous graphite gasifying device not can exceed that 0.5 hour, and i.e. this petroleum coke particles is by this continuous stone
The time of ink gasifying device controls to carry out semi-graphited process within 0.5 hour；And, at continuous graphite gasifying device to stone
During oil coke carries out semi-graphited process, oxidizing gas such as oxygen, nitrogen can be passed through in this continuous graphite gasifying device
Gas and chlorine etc. have the gas of oxidation susceptibility, by adding oxidizing gas in continuous graphite gasifying device, thus protect
Demonstrate,prove this petroleum coke in carrying out semi-graphited processing procedure, make petroleum coke easily produce more hole such that it is able to ensure
The quality of porous aggregate.
The porous aggregate preparation method using the embodiment of the present invention to provide, obtains volume relatively by choosing, pulverize and sieving
Little petroleum coke particles, this petroleum coke particles is by quickly carrying out in the continuous graphite gasifying device being passed through oxidizing gases
Semi-graphited processes, so that this petroleum coke particles is in an oxidizing environment by semi-graphited PROCESS FOR TREATMENT petroleum coke, thus obtains
Obtain the porous aggregate material of the high porosity of uniformity.
See Fig. 2, for the schematic flow sheet of preparation technology of a kind of high strength graphite that the embodiment of the present invention provides.
As in figure 2 it is shown, the preparation technology of the high strength graphite of the present embodiment offer includes:
Step S100: choose porous aggregate and coal tar pitch, and respectively by porous aggregate and coal tar pitch comminution by gas stream
For powder；
Wherein, porous aggregate is petroleum coke porous aggregate, the preparation method of this porous aggregate for petroleum coke is pulverized,
Screening, chooses petroleum coke particles of uniform size, and by continuous graphite gasifying device, petroleum coke particles is carried out semi-graphited
Process obtains this petroleum coke porous aggregate；After having chosen this porous aggregate and coal tar pitch, airflow pulverization can be passed through
Porous aggregate and coal tar pitch are pulverized the porous aggregate powder for 1-20 μm and coal tar pitch powder, it is simple to high temperature
Coal tar pitch and the mixing of porous aggregate.
In implementation process, before step S100, include prepared by porous aggregate, and this concrete porous aggregate preparation method
Including step S10 and step S20, then choosing petroleum coke porous aggregate and coal tar pitch by step S100, should
The concrete steps of step S10 and step S20 the most no longer elaborate, can be referring to the embodiment of respective figure 1.
The porous aggregate chosen and coal tar pitch are by the process of step S200.
Step S200: coal tar pitch is melted into hard pitch solution, corresponding according to porous aggregate and coal tar pitch
Porous aggregate powder is slowly added in hard pitch solution by ratio, stirs successively, is dried, kneading forms mixture,
And carry out mixture rolling sheet for the first time；
It is illustrated in figure 3 the schematic flow sheet of the preparation technology of the another kind of high strength graphite that the embodiment of the present invention provides, tool
Body be high strength graphite preparation technology in the schematic flow sheet of step S200 embodiment, as it can be seen, this step S200
Farther include:
Step S201: coal tar pitch melted into hard pitch solution by toluene；
Wherein, in toluene is joined coal tar pitch and heat, thus this coal tar pitch is melted into high temperature drip
Blue or green solution, using this hard pitch solution as the bonding agent of this porous aggregate powder.
Step S202: porous aggregate powder and hard pitch solution are with (63-75): the ratio of (37-25), by porous bone
Material powder is slowly added in hard pitch solution, and uniform stirring hard pitch solution and porous aggregate powder；
Wherein, the ratio of this porous aggregate powder and hard pitch solution quality is (63-75) in the present embodiment:
(37-25), i.e. the ratio of this porous aggregate powder and hard pitch solution is between 63:37 to 75:25, as this is many
Hole aggregate powder and the gross mass of hard pitch and be 100 parts, every part of representation quality be A, this porous aggregate powder is 68,
Hard pitch is 32, then the quality of this porous aggregate powder is 68A, and the quality of hard pitch is 32A；Thus by setting
Ratio porous aggregate powder is slowly added in hard pitch solution, in hard pitch solution, be slowly added into porous
While aggregate powder, this hard pitch solution of uniform stirring and the porous aggregate powder of addition so that porous aggregate powder
Fully can mix with hard pitch solution, form hard pitch solution and the mixture of porous aggregate powder.
Step S203: the mixture after stirring is dried process, and in the environment of temperature is 75-100 DEG C, right
Dried hard pitch solution and mixture kneading 0.5-3 hour of porous aggregate powder；
Wherein, after step S202 completes the uniform stirring of hard pitch solution and porous aggregate powder, hard pitch is molten
Porous aggregate powder can fully be carried out bonding by liquid, enables hard pitch solution and porous aggregate powder to be sufficiently mixed shape
Resulting mixture thickener, is dried mixture the most successively and kneading processes；Treat hard pitch solution and porous aggregate powder
After the mixing of end, by desiccant or other operations, the mixture after uniform stirring can be dried process, remove mixture
In moisture；Then, for the ease of being thoroughly mixed of hard pitch and porous aggregate powder, by kneading pot or its
His kneading equipment carries out the kneading of 0.5-3 hour to the hard pitch solution after stirring and porous aggregate powder, in order to avoid
Mixture cools down, and mixture temperature should be kept at 75-100 DEG C；And carry out the operation of step S204.
Step S204: in the environment of temperature is 130-170 DEG C, carries out the mixture after kneading rolling sheet for the first time, and
The sheet number of times that rolls rolling sheet for the first time is 1-10 time；
Wherein, for the hard pitch solution after kneading and the mixture of porous aggregate powder, need to roll while hot sheet, therefore,
The temperature of hard pitch solution and porous aggregate powder can be increased to 130-170 DEG C, thus after step S203 is processed
Hard pitch solution and porous aggregate powder carry out rolling sheet；The mixture of hard pitch solution and porous aggregate powder is being entered
During row rolls sheet, can repeatedly roll sheet (can repeatedly roll sheet in the scope of 1-10 time), so that mixture
Fully carry out rolling sheet, obtain the product after rolling sheet for the first time；And the product after rolling sheet for the first time is carried out by step S300
Reason.
Step S300: the mixture after rolling sheet for the first time carries out crushing, sieving, and the mixture after sieving is carried out second
The secondary sheet that rolls, and the mixture after rolling sheet for the second time is pulverized, sieved, strengthened powder body；
According to mixture is carried out by step S200 first roll sheet after product crush successively, sieving obtains 0.5mm
Following mixture, and it is carried out second roll sheet, then the product after rolling sheet to second successively is pulverized, sieving obtains
Strengthen powder body；Wherein, the flow process of the preparation technology of a kind of high strength graphite that the embodiment of the present invention provides it is illustrated in figure 4
The schematic flow sheet of step S300 embodiment in the preparation technology of schematic diagram, specially high strength graphite, as it can be seen,
This step S300 specifically includes:
Step S301: the mixture after rolling sheet for the first time in step S204 cools down；The mixture after rolling sheet is made to drop
To room temperature state, thus ensure shattering process to make it the most broken；
Step S302: the mixture after cooling is crushed, and the compound particles obtaining size less than 0.5mm that sieves；
Wherein, for the first time sheet is rolled owing to the mixture of hard pitch solution and porous aggregate powder being carried out by step S204
After, owing to rolling the mixture after sheet the most in the form of sheets, therefore, can be by disintegrating machine or other breakers by step S301
Mixture after cooling carries out crushing and sieves the granular mixture after broken, thus choose sieve after size
Compound particles less than 0.5mm；Concrete, the sieve aperture of this sieve device can be set to the hole of 0.5mm size,
Thus the size of the compound particles after being sieved by sieve device is less than 0.5mm.
Step S303: in the environment of temperature is 130-170 DEG C, carries out second time and rolls sheet, and second compound particles
The secondary sheet number of times that rolls rolling sheet is 1-10 time；
Wherein, the size of the compound particles after processing in step s 302 is below 0.5mm, in order to ensure
Second time rolls sheet, needs the compound particles being crushed to below 0.5mm is carried out heat temperature raising, and ensures that mixture is in
Temperature carries out second time to the mixture of hard pitch solution and porous aggregate powder in the environment of being 130-170 DEG C and rolls sheet,
Second time roll sheet time mixture can be rolled repeatedly sheet (can to its carry out 1-10 time roll sheet).
Step S304: the mixture after rolling sheet to second is pulverized, crossed 100-200 mesh sieve, and strengthened powder body；
Wherein, after mixture being carried out by step S303 roll sheet for the second time, this porous aggregate powder and hard pitch solution
Mixture between gap less, and porous aggregate powder can fully bond by this hard pitch solution, thus right
Second time roll sheet after mixture pulverize, specifically can pulverize by disintegrating machine, and will pulverizing after powder pass through
The sieve device of 100-200 mesh sieves, thus removes the powder that particle-removing is bigger, remaining is the reinforcement powder obtained
Body.Meanwhile, the reinforcement powder body that the process of step S300 obtains carries out the process of step S400.
Step S400: carry out compression molding, roasting, dipping successively to strengthening powder body, and the product after dipping is carried out slightly
Broken and comminution by gas stream, the powder after comminution by gas stream sieves and obtains high-strength powder body；
Wherein, in order to improve the intensity of graphite, the porous aggregate needed for this graphite and bonding agent (i.e. hard pitch solution)
Hole after bonding is minimum, accordingly, it would be desirable to the reinforcement powder body obtaining step S300 carries out separating twice and obtains high-strength powder
Body, so that the reinforcement powder body that high-strength powder body and step S300 obtain is smaller, strengthens the intensity of high strength graphite；
Concrete, step S400 farther includes:
First, the reinforcement powder body obtaining step S300 carries out pre-molding by pre-pressing die, and to pre-molding
Graphite products carries out roasting for the first time, wherein, the graphite products of pre-molding can be carried out in roaster high-temperature roasting；
Secondly, carrying out in mid temperature pitch the graphite products after first time roasting impregnating for the first time, wherein, this mid temperature pitch can
Carry out melting obtain mid temperature pitch solution by the coal tar pitch chosen in the step s 100 adds toluene；Then, right
Graphite products after dipping carries out coarse crushing and comminution by gas stream by breaker and air flow crushing device respectively for the first time, will
The graphite products of pre-molding is ground into powder, and obtains high-strength powder body by the sieve device of 100-200 mesh.And it is high-strength
Powder body continues through the process of step S500.
Step S500: high-strength powder body is carried out successively compression molding, roasting；
Wherein, relatively big in order to ensure the graphite products intensity of preparation, need the high-strength powder body to obtaining in step S400 to enter
Row second time compression molding and roasting；It is illustrated in figure 5 the system of another high strength graphite that the embodiment of the present invention provides
The schematic flow sheet of standby technique, the specially flow process signal of step S500 embodiment in the preparation technology of high strength graphite
Figure, as it can be seen, this step S500 includes:
Step S501: mix the oleic acid of 0.8-2.5wt% in the high-strength powder body obtained in step S400, first pre-molding,
Isostatic pressing obtains base substrate again；
Wherein, obtaining high-strength powder body in step S400, oleic acid carries out the profit of compression molding graphite products as high-strength powder body
Lubrication prescription, can be according to the weight of this high-strength powder body toward adding oleic acid in this high-strength powder body, and wt% is weight percentage unit, i.e. oil
The 0.8-2.5% that weight is high-strength powder body weight of acid, thus the oleic acid of 0.8-2.5wt% is joined in high-strength powder body；First
Elder generation, can be carried out pre-molding by mould, then, be incited somebody to action by isostatic tooling the high-strength powder body being added with oleic acid
Graphite products after pre-molding carries out isostatic pressing process under 80-200Mpa pressure, forms the base of isostatic pressing formed graphite
Body；Meanwhile, in order to ensure the intensity of isostatic pressing formed graphite, in isostatic pressing processing procedure, the base of this isostatic pressing formed graphite
Body needs pressurize 15 minutes, it is ensured that the blank forming of isostatic pressing formed graphite.
Step S502: by the base substrate of isostatic pressing in a nitrogen environment with the ramp of 5 DEG C/h to 850-1050 DEG C,
Complete roasting；
Wherein, after isostatic pressing in step S501, form the base substrate of isostatic pressing formed graphite, this base substrate is carried out second time
Roasting；But, in base substrate second time roasting process, need in roaster, be passed through appropriate nitrogen, and roaster
Heating rate be 5 DEG C/h so that base substrate in roaster to rise the slow roasting of the speed of 5 DEG C per hour, until roasting
The temperature burnt in stove rises to 850 DEG C-1050 DEG C, then complete second time roasting；It is passed through nitrogen in slow roasting process
Purpose is to ensure that in step S501 that the base substrate of isostatic pressing can be fully oxidized, is effectively improved the strong of isostatic pressing formed graphite
Degree.After completing the second time roasting of base substrate, the product after roasting can be carried out the operation of step S600.
Step S600: the product after roasting is impregnated, roasting；
Wherein, can respectively the product after the second time roasting of step S500 be carried out successively in step S600 the dipping of twice
With the roasting of twice, thus impregnation-calcination is repeated, completes graphite purification；It is illustrated in figure 6 the embodiment of the present invention to carry
Step in the preparation technology of the schematic flow sheet of the preparation technology of another high strength graphite of confession, specially high strength graphite
The schematic flow sheet of S600 embodiment, as it can be seen, step S600 includes:
Step S601: (i.e. base substrate is under nitrogen protection with the speed liter of 5 DEG C/h to the product after roasting in step S502
Temperature is to the product after the second time roasting of 850-1050 DEG C) heat, to be heated after carry out the operation of step S602；
Step S602: the product after heating is put into pressure vessel, and in the environment of 250 DEG C and 3.5Mpa, will
Product after heating impregnates at least 5 hours in mid temperature pitch；
Wherein, the product after heating is put in pressure vessel, fills mid temperature pitch solution in this pressure vessel, and this middle temperature drips
Blue or green solution is interpolation toluene in coal tar pitch, and melts for mid temperature pitch solution；And ensure the temperature in this pressure vessel
Degree is 250 DEG C, and the pressure in pressure vessel is 3.5Mpa；Thus the product after heating is soaked in mid temperature pitch solution
Stain at least 5 hours, it is preferred that the product after heating impregnates 5 hours in mid temperature pitch solution.
Step S603: the product after dipping is carried out roasting at the highest sintering temperature is 850-950 DEG C；
Wherein, in step S602, the product after heating is after mid temperature pitch solution impregnation 5 hours, can be drawn off also
It is placed in roaster, by roaster, the product after dipping is carried out third time roasting, and the temperature of roaster promotion
Temperature is to 850 DEG C-950 DEG C.
It addition, after carrying out third time roasting, in order to ensure the intensity of the graphite finally prepared, need to carry out the 4th roasting
Burning, concrete steps include:
Step S604: the product after roasting is heated；Concrete, can be by heater in step S603 the
Product after three roastings heats, and makes the product temperature after third time roasting raise or keep constant；And then carry out
The operation of step S605；
Step S605: the product after heating is put into and fills the pressure vessel of hard pitch solution, and at 325 DEG C and
In the environment of 4.5Mpa, the product after heating is impregnated at least 4 hours in hard pitch solution；
Wherein, hard pitch solution is that coal tar pitch melts into hard pitch solution by toluene, by molten for this hard pitch
Liquid is placed in pressure vessel, and ensure pressure vessel be in temperature be 325 DEG C, in the environment of pressure is 4.5Mpa, will
Product after heating impregnates at least 4 hours in hard pitch solution；In implementation process, preferred dip time is 4
Hour, i.e. temperature be 325 DEG C, pressure be under 4.5Mpa, the product after third time roasting to be soaked in hard pitch solution
Stain can be drawn off for 4 hours.
Step S606: the product after dipping is carried out roasting at the highest sintering temperature is 850-950 DEG C；
Wherein, the product after impregnating in step s 605 is placed in roaster and carries out the 4th roasting, by this roasting
Stove gradually heats up and the product after dipping is carried out the temperature in roasting, and this roaster and is up between 850-950 DEG C,
When temperature in roaster is increased to 850-950 DEG C, i.e. complete the 4th roasting.
By porous aggregate and coal tar pitch are repeatedly impregnated by above step S400 to S600, roasting, thus
It is effectively increased the intensity of isostatic pressing formed graphite.
Step S700: the product after roasting is warming up to 2400 DEG C with the heating rate of 160 DEG C/h under ar gas environment, and
It is incubated 1 hour, thus completes graphitization and purification, obtain described high strength graphite；
Wherein, the product after step S606 carries out the 4th roasting, can by it under ar gas environment, with 160 DEG C/h
Heating rate be warming up to 2400 DEG C, and at 2400 DEG C be incubated 1 hour；Or 2500-2600 DEG C can be warming up to,
Product after 4th roasting is carried out graphitization and purification；And it is incubated 1 hour, it is finally completed graphitization and obtains this reality
Execute the high strength graphite that example proposes, i.e. isostatic pressing formed graphite.
By using the preparation technology of the high strength graphite of the present embodiment offer, by semi-graphited technique by petroleum coke particles
Carry out semi-graphited and process prepared petroleum coke porous aggregate, then by hard pitch solution, porous aggregate powder is carried out liquid
Be coated with mutually, carry out after drying kneading, broken, preforming, second-time breakage, post forming, isostatic pressing, dipping,
The series of processes such as roasting, then carry out high temperature graphitization and purification, thus prepare the high intensity stone that the present embodiment proposes
Ink；In the preparation technology of the high strength graphite of the embodiment of the present invention, obtained the height of uniformity by semi-graphited technique
The porous aggregate material of porosity, thus improve and improve the interface cohesion of bonding agent and porous aggregate, and to porous bone
Material and hard pitch carry out kneading, broken, molding and repeatedly form the isostatic pressing formed graphite of high intensity under dipping, roasting,
Thus it is effectively improved the intensity of graphite material.
Each embodiment in this specification all uses the mode gone forward one by one to describe, identical similar part between each embodiment
Seeing mutually, what each embodiment stressed is the difference with other embodiments.System described above
Preparation Method embodiment is only schematically, some or all of module therein can be selected according to the actual needs real
The purpose of existing the present embodiment scheme.Those of ordinary skill in the art, in the case of not paying creative work, i.e. can manage
Solve and implement.
It should be noted that in this article, such as the relational terms of " first " and " second " or the like be used merely to by
One entity or operation separate with another entity or operating space, and not necessarily require or imply these entities or behaviour
Relation or the order of any this reality is there is between work.And, term " includes ", " comprising " or it is any
Other variants are intended to comprising of nonexcludability so that include the process of a series of key element, method, article or
Equipment not only includes those key elements, but also includes other key elements being not expressly set out, or also includes for this mistake
The key element that journey, method, article or equipment are intrinsic.In the case of there is no more restriction, statement " include one
It is individual ... " key element that limits, it is not excluded that there is also in including the process of described key element, method, article or equipment
Other identical element.
The above is only the detailed description of the invention of the present invention, makes to skilled artisans appreciate that or realize the present invention.
Multiple amendment to these embodiments will be apparent to one skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, this
The bright the embodiments shown herein that is not intended to be limited to, and be to fit to and principles disclosed herein and features of novelty
The widest consistent scope.
Claims (9)
1. a porous aggregate preparation method, it is characterised in that including:
Petroleum coke is pulverized, sieves, and choose 2-5mm petroleum coke particles of uniform size；
Quickly through continuous graphite gasifying device, described petroleum coke particles is carried out the semi-graphited that temperature is 1500-2000 DEG C process, after described petroleum coke particles is detained less than or equal to 0.5 hour in described continuous graphite gasifying device, obtain described porous aggregate.
Porous aggregate preparation method the most according to claim 1, it is characterised in that in described petroleum coke particles carries out semi-graphited processing procedure, is passed through oxidizing gas in described continuous graphite gasifying device.
3. the preparation technology of a high strength graphite, it is characterised in that including:
(1) choose porous aggregate as claimed in claim 1 and coal tar pitch, and be powder by described porous aggregate and described coal tar pitch comminution by gas stream respectively；
(2) described coal tar pitch is melted into hard pitch solution, porous aggregate powder is slowly added in described hard pitch solution by the corresponding proportion according to porous aggregate and hard pitch solution, stir successively, be dried, kneading forms mixture, and carries out described mixture rolling sheet for the first time；
(3) mixture after rolling sheet for the first time carries out crushing, sieving, and the mixture after sieving carries out second time and rolls sheet, and the mixture after rolling sheet for the second time is pulverized, sieved, and strengthened powder body；
(4) described reinforcement powder body is carried out successively compression molding, roasting, dipping, and the powder after the product after dipping is carried out coarse crushing and comminution by gas stream, and comminution by gas stream sieves and obtains high-strength powder body；
(5) described high-strength powder body is carried out compression molding, roasting successively；
(6) product after roasting is impregnated, roasting；
(7) product after roasting is warming up to 2400 DEG C with the heating rate of 160 DEG C/h under ar gas environment, and is incubated 1 hour, thus completes graphitization and purification, obtains described high strength graphite.
4. according to claim 3
The preparation technology of described high strength graphite, it is characterised in that described step (2) farther includes:
By toluene, described coal tar pitch is melted into hard pitch solution；
Described porous aggregate powder and described hard pitch solution are with (63-75): the ratio of (37-25), described porous aggregate powder is slowly added in hard pitch solution, and hard pitch solution described in uniform stirring and described porous aggregate powder；
Mixture after stirring is dried process, and in the environment of temperature is 75-100 DEG C, to dried described hard pitch solution and mixture kneading 0.5-3 hour of described porous aggregate powder；
In the environment of temperature is 130-170 DEG C, the mixture after kneading carries out rolling for the first time sheet, and the sheet number of times that rolls rolling sheet for the first time is 1-10 time.
5. according to claim 3
The preparation technology of described high strength graphite, it is characterised in that described step (3) farther includes:
Mixture after rolling sheet for the first time in described step (2) cools down；
Mixture after cooling is crushed, and the compound particles obtaining size less than 0.5mm that sieves；
In the environment of temperature is 130-170 DEG C, described compound particles is carried out second time and rolls sheet, and the sheet number of times that rolls rolling sheet for the second time is 1-10 time；
Mixture after second time is rolled sheet is pulverized, is crossed 100-200 mesh sieve, and strengthened powder body.
6. according to claim 3
The preparation technology of described high strength graphite, it is characterised in that described step (5) farther includes:
Mix the oleic acid of 0.8-2.5wt%, first pre-molding, then isostatic pressing in the described high-strength powder body obtained in described step (4) and obtain base substrate；
By the base substrate of isostatic pressing in a nitrogen environment with the ramp of 5 DEG C/h to 850-1050 DEG C, complete roasting.
7. according to claim 6
The preparation technology of described high strength graphite, it is characterised in that the pressure when product after pre-molding carries out isostatic pressing is 80-200MPa, the dwell time is 15 minutes.
8. according to claim 3
The preparation technology of described high strength graphite, it is characterised in that described step (6) farther includes:
Product after roasting in described step (5) is heated；
Product after heating is put into the pressure vessel filling mid temperature pitch solution, and in the environment of 250 DEG C and 3.5MPa, the described product after heating is impregnated at least 5 hours in mid temperature pitch solution；
Product after dipping is carried out roasting at the highest sintering temperature is 850-950 DEG C.
The most according to Claim 8
The preparation technology of described high strength graphite, it is characterised in that described step (6) also includes:
Product after roasting is heated；
Product after heating is put into the pressure vessel filling hard pitch solution, and in the environment of 325 DEG C and 4.5MPa, the described product after heating is impregnated at least 4 hours in hard pitch solution；
Product after dipping is carried out roasting at the highest sintering temperature is 850-900 DEG C.
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| CN105177628B (en) * | 2015-10-29 | 2017-10-17 | 中南大学 | One kind modification carbon anode and preparation method thereof |
| CN107022690B (en) * | 2017-05-03 | 2019-03-08 | 合肥工业大学 | A method of aluminium/C-base composte material is prepared by Pressure Infiltration aluminium alloy |
| CN107337460B (en) * | 2017-07-13 | 2020-08-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Refractory aggregate, preparation method thereof and refractory heat-insulating material |
| CN108101017A (en) * | 2017-12-21 | 2018-06-01 | 吉林市松江炭素有限责任公司 | A kind of petroleum coke die mould technique |
| CN114739176B (en) | 2022-03-11 | 2024-01-23 | 中国铝业股份有限公司 | Graphitizing furnace |
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