CN108298985A - The preparation method of graphite jig - Google Patents
The preparation method of graphite jig Download PDFInfo
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- CN108298985A CN108298985A CN201810091599.2A CN201810091599A CN108298985A CN 108298985 A CN108298985 A CN 108298985A CN 201810091599 A CN201810091599 A CN 201810091599A CN 108298985 A CN108298985 A CN 108298985A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/06—Permanent moulds for shaped castings
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Abstract
The invention discloses a kind of preparation methods of graphite jig, its key points of the technical solution are that raw material is made of following components in parts by weight：20~30 parts by weight of petroleum coke powder that 10~15 parts by weight of petroleum coke powder that 10~15 parts by weight of petroleum coke powder that grain size is 1~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm, grain size is less than 20~35 parts by weight of 0.05mm petroleum coke powders, grain size is less than 20~25 parts by weight of pitch of 10mm, and preparation method includes the following steps：(1) it calcines；(2) it crushes, dispensing；(3) kneading；(4) isostatic pressing；(5) it roasts：It is handled being placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block, treatment temperature is 1100~1300 DEG C；(6) it impregnates；(7) after baking；(8) graphitization processing；(9) graphite jig is prepared.The present invention solves the problems, such as that graphite jig is being easy cracking after multiple high temp and fast cooling.
Description
Technical field
The present invention relates to graphite jig technical fields, more specifically, it is related to a kind of preparation method of graphite jig.
Background technology
Non-ferrous metal refers to the general name of all metals in addition to the ferrous metal that iron, manganese, chromium are constituted, with ferrous metal
Compare, with more corrosion resistance, wearability, electric conductivity, thermal conductivity, toughness, high intensity, radioactivity, easy ductility, plasticity, easily
The properties such as pressure property and easy rolling property.Non-ferrous metal metallurgy refers to that certain non-ferrous metals are heated to fusion temperature, is carried out certain
The casting manipulations of workpiece.And graphite is increasingly becoming mold manufacturing in non-ferrous metal metallurgy with its good physical and chemical properties
Preferred material.The graphite jig made of graphite block not only has excellent heat conduction, electric conductivity and resistance to chemical corrosion, also
With good lubrication and wear resistence.
But graphite jig is in use, needs the process by high temperature and fast cooling, is easy out after being used for multiple times
It splits.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of preparation method of graphite jig, energy
The intensity for enough increasing graphite jig, extends the service life of graphite jig.
To achieve the above object, the present invention provides following technical solutions：A kind of preparation method of graphite jig, raw material
It is made of following components in parts by weight：10~15 parts by weight of petroleum coke powder that grain size is 1~3mm, grain size are 0.5~1.5mm's
10~15 parts by weight of petroleum coke powder, grain size are 20~30 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size less than 0.05mm stones
20~35 parts by weight of oil coke powder, 20~25 parts by weight of pitch, preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1350~1400 DEG C vacuum calcining 20~30 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into pulverizer and is crushed, the petroleum coke powder completed will be crushed
It is put into screening machine and is screened, it is 0.5~1.5mm particles, grain to be sieved into particle, particle size range that particle size range is 1~3mm
Diameter ranging from 0.05~0.1mm particles and grain size are less than four kinds of specifications of fine powder of 0.05mm, are then 1~3mm's according to grain size
10~15 parts by weight of petroleum coke powder that 10~15 parts by weight of petroleum coke powder, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
20~30 parts by weight of petroleum coke powder, grain size be less than 20~35 parts by weight of 0.05mm petroleum coke powders ratio dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading are carried out at 110~150 DEG C
Time is 40~60min；Then the pitch of 20~25 parts by weight is added, then carries out 40~60min of kneading；
(4) isostatic pressing：Raw material obtained by above-mentioned steps (3) is put into rubber mold, is then placed in iso-static pressure shaping machine
It is shaped to graphite block, the pressure of isostatic pressing is 100~200 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1100~1300 DEG C；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
Middle dipping 8~9 hours；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1100~1300 DEG C；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 2800~3500 DEG C, and graphitization time is 84~96 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
By using above-mentioned technical proposal, the higher easily graphited high-quality needle coke of intensity is selected, is matched using small pellet
Side, and the methods roasted are soaked using high pressure more more, make in the full penetration to the hole of graphite block of dipping pitch, reduces in this way
The porosity of graphite block improves the compactness, bulk density and intensity of graphite block, by being passed through nitrogen and first in roasting process
The gaseous mixture of alkane, and calcination temperature is more than 1000 DEG C, so that methane gas is entered in the stomata on graphite block, methane resolves into carbon black
And hydrogen, carbon black are attached in stomata, increase the intensity of graphite block, extend the service life of graphite jig, using isostatic pressed
Molding manufacture graphite block, can make petroleum coke powder press closely knit, the air between powder is discharged, make graphite jig that stomata be not present,
Prolong the service life.
The present invention is further arranged to：The grain size of the pitch is less than 10mm.
By using above-mentioned technical proposal, the performance of isostatic pressing by raw material extreme influence, by the grain size of pitch
Control can improve the performance of isostatic pressing, when also asphalt volatile constituents may make to be discharged, on graphite block within 10mm
Hole diameter is smaller, when being impregnated, is without the use of more impregnating pitch, and saving resource can also make when producing mixed raw material
Pitch is uniformly mixed with the petroleum coke powder of different size.
The present invention is further arranged to：The rotating speed of pulverizer is 500~700 turns/min, grinding time in the step (2)
For 20~30min.
By using above-mentioned technical proposal, because needing strictly to control the size of raw material in isostatic pressing,
It is 500~700 turns/min by the control of pulverizer rotating speed, grinding time is 20~30min, and pitch and petroleum coke powder can be made to be ground into
Required specification.
The present invention is further arranged to：Step (5) roasting time is 25~40 days.
By using above-mentioned technical proposal, because during isostatic pressing, need strictly to control heating process, heating compared with
To be slow, in a longer range by time control, graphite block can be made to roast more uniform so that the methane being passed through in roaster
Gas decomposes completely, forms coating on graphite block surface, enhances the intensity of graphite block, extend the graphite jig that graphite block makes
Service life.
The present invention is further arranged to：Roasting time is 10~15 days in the step (7).
By using above-mentioned technical proposal, the graphite block by biscuit firing is because of the discharge of asphalt volatile constituents, graphite block
Middle formation micropore when being roasted again, can reduce the micropore on graphite block surface, roast again by the dipping of impregnating pitch
Burn, need to only roast the pitch of dipping, so controlling roasting time at 10~15 days, can make graphite block roasting uniformly and
So that the methane being passed through is decomposed complete, forms coating on graphite block surface again, increase the intensity of graphite block.
The present invention is further arranged to：In the step (5) and step (7) treatment temperature speed no more than 1 DEG C/it is small
When, temperature difference requirement is less than 20 DEG C in stove.
By using above-mentioned technical proposal, in roasting process, the graphite block of isostatic pressing is due to close structure, roasting
It is especially slow to cross range request, and in-furnace temperature wants highly uniform, the temperature stage being especially drastically discharged in asphalt volatile constituents,
So heating process is very slow, the temperature difference is less than 20 DEG C in stove.
The present invention is further arranged to：The pressure of step (6) the mesohigh impregnating autoclave is 0.2~0.25MPa, and temperature is
200~250 DEG C.
In roasting process, since asphalt volatile constituents are discharged, when gas discharge is with volume contraction, left in graphite block
Subtle stomata, and be nearly all open pore, the pressure of high-pressure impregnation tank is controlled in 0.2~0.25MPa, pressurization can be passed through
Dipping, improves the bulk density and mechanical strength of graphite block, i.e., impregnating pitch is impregnated into inside graphite block by open pore,
It needs to preheat graphite block before impregnation, so being 200~250 DEG C by the temperature of high-pressure impregnation tank.
In conclusion the invention has the advantages that：The present invention is used as guarantor by being passed through nitrogen in roasting process
Gas is protected, methane is passed through and controls temperature at 1000 DEG C or more, using methane at 1000 DEG C, carbon black can be resolved into, and
Due to the volatilization of pitch in roasting process, many stomatas can be formed in graphite block, carbon black can be convenient for enter in these stomatas,
The intensity for increasing graphite block, extends the service life of graphite jig；Using isostatic pressing manufacture graphite block, can be discharged powder it
Between air, so that petroleum coke powder is pressed closely knit, keep graphite bulk strength obtained higher, graphite jig exists made from the graphite block
It does not crack, prolongs the service life after multiple high temp and fast cooling；It is impregnated using high pressure, pitch can be made to enter roasting
In the stomata generated in the process, the bulk density and mechanical strength of graphite block can be improved, and then improve the intensity of graphite jig,
Extend the service life of graphite jig.
Specific implementation mode
With reference to specific embodiment, invention is further described in detail.
Embodiment one：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
10 parts by weight of petroleum coke powder that 10 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
20 parts by weight of petroleum coke powder, grain size be less than 35 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 25 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1350 DEG C vacuum calcining 30 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 500 turns/min and is crushed, is crushed
Time is 30min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 10 that then 10 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 35 parts by weight of 0.05mm petroleum coke powders for 20 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 110 DEG C
For 60min；Then the pitch of 25 parts by weight is added, then carries out kneading 60min；
(4) isostatic pressing：Raw material obtained by above-mentioned steps (3) is put into rubber mold, is then placed in iso-static pressure shaping machine
It is shaped to graphite block, the pressure of isostatic pressing is 100 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1100 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove,
Roasting time is 40 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8 hours, high-pressure impregnation tank is 0.2MPa, and temperature is 250 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1100 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, temperature difference requirement in stove
Less than 20 DEG C, roasting time is 15 days；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 2800 DEG C, and graphitization time is 96 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Embodiment two：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
11 parts by weight of petroleum coke powder that 11 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
22 parts by weight of petroleum coke powder, grain size be less than 32 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 24 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1360 DEG C vacuum calcining 28 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 540 turns/min and is crushed, is crushed
Time is 28min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 11 that then 11 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 32 parts by weight of 0.05mm petroleum coke powders for 22 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 120 DEG C
For 55min；Then the pitch of 24 parts by weight is added, then carries out kneading 55min；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 120 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1150 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove,
Roasting time is 37 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8.2 hours, high-pressure impregnation tank is 0.21MPa, and temperature is 240 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1150 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, temperature difference requirement in stove
Less than 20 DEG C, roasting time is 14 days；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3000 DEG C, and graphitization time is 94 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Embodiment three：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
12 parts by weight of petroleum coke powder that 12 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
24 parts by weight of petroleum coke powder, grain size be less than 29 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 23 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1370 DEG C vacuum calcining 26 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 600 turns/min and is crushed, is crushed
Time is 26min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 12 that then 12 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 29 parts by weight of 0.05mm petroleum coke powders for 24 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 130 DEG C
For 50min；Then the pitch of 23 parts by weight is added, then carries out kneading 50min；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 140 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1200 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove,
Roasting time is 34 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8.4 hours, high-pressure impregnation tank is 0.22MPa, and temperature is 230 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1200 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, temperature difference requirement in stove
Less than 20 DEG C, roasting time is 13 days；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3100 DEG C, and graphitization time is 90 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Example IV：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
13 parts by weight of petroleum coke powder that 13 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
26 parts by weight of petroleum coke powder, grain size be less than 28 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 22 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1380 DEG C vacuum calcining 24 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 640 turns/min and is crushed, is crushed
Time is 24min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 13 that then 13 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 28 parts by weight of 0.05mm petroleum coke powders for 26 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 135 DEG C
For 48min；Then the pitch of 22 parts by weight is added, then carries out kneading 48min；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 160 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1250 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove,
Roasting time is 31 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8.6 hours, high-pressure impregnation tank is 0.23MPa, and temperature is 220 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1250 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, temperature difference requirement in stove
Less than 20 DEG C, roasting time is 12 days；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3200 DEG C, and graphitization time is 88 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Embodiment five：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
14 parts by weight of petroleum coke powder that 14 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
27 parts by weight of petroleum coke powder, grain size be less than 24 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 21 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1390 DEG C vacuum calcining 22 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 680 turns/min and is crushed, is crushed
Time is 22min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 14 that then 14 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 24 parts by weight of 0.05mm petroleum coke powders for 27 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 140 DEG C
For 45min；Then the pitch of 21 parts by weight is added, then carries out kneading 45min；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 180 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1280 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove,
Roasting time is 28 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8.8 hours, high-pressure impregnation tank is 0.24MPa, and temperature is 210 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1280 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, temperature difference requirement in stove
Less than 20 DEG C, roasting time is 11 days；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3400 DEG C, and graphitization time is 86 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Embodiment six：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
15 parts by weight of petroleum coke powder that 15 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
28 parts by weight of petroleum coke powder, grain size be less than 22 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 20 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1400 DEG C vacuum calcining 20 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 700 turns/min and is crushed, is crushed
Time is 20min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 15 that then 15 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 22 parts by weight of 0.05mm petroleum coke powders for 28 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 150 DEG C
For 40min；Then the pitch that 20 parts by weight are added carries out kneading 40min again；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 200 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1300 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove,
Roasting time is 25 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 9 hours, high-pressure impregnation tank is 0.25MPa, and temperature is 200 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1300 DEG C, and the heating rate for the treatment of temperature is no more than 1 DEG C/h, temperature difference requirement in stove
Less than 20 DEG C, roasting time is 10 days；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3500 DEG C, and graphitization time is 84 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Comparative example one：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
10 parts by weight of petroleum coke powder that 10 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
20 parts by weight of petroleum coke powder, grain size be less than 35 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 25 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1350 DEG C vacuum calcining 30 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 500 turns/min and is crushed, is crushed
Time is 30min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 10 that then 10 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 35 parts by weight of 0.05mm petroleum coke powders for 20 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 110 DEG C
For 60min；Then the pitch of 25 parts by weight is added, then carries out kneading 60min；
(4) isostatic pressing：Raw material obtained by above-mentioned steps (3) is put into rubber mold, is then placed in iso-static pressure shaping machine
It is shaped to graphite block, the pressure of isostatic pressing is 100 DEG C；
(5) it roasts：It will be placed in roaster and handle through step (4) molding graphite block, treatment temperature is 1100 DEG C, treatment temperature
Heating rate no more than 1 DEG C/h, temperature difference requirement is less than 20 DEG C in stove, and roasting time is 40 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8 hours, high-pressure impregnation tank is 0.2MPa, and temperature is 250 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into roaster and is handled, treatment temperature is
1100 DEG C, the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove, roasting time 15
It；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 2800 DEG C, and graphitization time is 96 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Comparative example two：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
12 parts by weight of petroleum coke powder that 12 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
24 parts by weight of petroleum coke powder, grain size be less than 29 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 23 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1370 DEG C vacuum calcining 26 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 600 turns/min and is crushed, is crushed
Time is 26min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 12 that then 12 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 29 parts by weight of 0.05mm petroleum coke powders for 24 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 130 DEG C
For 50min；Then the pitch of 23 parts by weight is added, then carries out kneading 50min；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 140 DEG C；
(5) it roasts：It will be placed in roaster and handle through step (4) molding graphite block, treatment temperature is 1200 DEG C, treatment temperature
Heating rate no more than 1 DEG C/h, temperature difference requirement is less than 20 DEG C in stove, and roasting time is 34 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 8.4 hours, high-pressure impregnation tank is 0.22MPa, and temperature is 230 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into roaster and is handled, treatment temperature is
1200 DEG C, the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove, roasting time 13
It；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3100 DEG C, and graphitization time is 90 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Comparative example three：A kind of preparation method of graphite jig, raw material are made of following components in parts by weight：Grain size is 1
15 parts by weight of petroleum coke powder that 15 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
28 parts by weight of petroleum coke powder, grain size be less than 22 parts by weight of 0.05mm petroleum coke powders, grain size be less than 10mm 20 parts by weight of pitch,
Preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1400 DEG C vacuum calcining 20 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into the pulverizer that rotating speed is 700 turns/min and is crushed, is crushed
Time is 20min, and the petroleum coke powder that will crush completion, which is put into screening machine, to be screened, and it is 1~3mm's to be sieved into particle size range
Particle, particle size range are 0.5~1.5mm particles, particle size range is the fine powder of 0.05~0.1mm particles and grain size less than 0.05mm
The petroleum coke powder 15 that then 15 parts by weight of petroleum coke powder that four kinds of specifications are 1~3mm according to grain size, grain size are 0.5~1.5mm
Parts by weight, grain size are less than the ratio of 22 parts by weight of 0.05mm petroleum coke powders for 28 parts by weight of petroleum coke powder of 0.05~0.1mm, grain size
Example dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading time are carried out at 150 DEG C
For 40min；Then the pitch of 20 parts by weight is added, then carries out kneading 40min；
(4) isostatic pressing：Graphite block obtained by above-mentioned steps (3) is put into rubber mold, iso-static pressure shaping machine is then placed in
In be shaped to graphite block, the pressure of isostatic pressing is 200 DEG C；
(5) it roasts：It will be placed in roaster and handle through step (4) molding graphite block, treatment temperature is 1300 DEG C, treatment temperature
Heating rate no more than 1 DEG C/h, temperature difference requirement is less than 20 DEG C in stove, and roasting time is 25 days；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
The pressure of middle dipping 9 hours, high-pressure impregnation tank is 0.25MPa, and temperature is 200 DEG C；
(7) after baking：The graphite block completed through step (6) dipping is put into roaster and is handled, treatment temperature is
1300 DEG C, the heating rate for the treatment of temperature is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove, roasting time 10
It；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 3500 DEG C, and graphitization time is 84 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
Intensity detection, obtained data such as following table institute are carried out to graphite jig made from the various embodiments described above and comparative example
Show：
The strength test results of graphite jig made from 1 each embodiment and comparative example of table
Graphite jig made from the various embodiments described above and comparative example is carried out at the same time to the melting continuously of identical non-ferrous metal, testing stone
The access times of black mold, test result is as follows shown in table：
The service life test result of graphite jig made from 2 each embodiment and comparative example of table
The present invention by be passed through in roasting process nitrogen be used as protection gas, be passed through methane and by temperature control 1000 DEG C with
On, using methane at 1000 DEG C or more, carbon black can be resolved into, and can be caused due to the volatilization of pitch in roasting process
Many stomatas are formed in graphite block, can be convenient for coal is black to enter in these stomatas, be increased the intensity of graphite block, extend graphite mo(u)ld
The service life of tool；Graphite block is manufactured using isostatic pressing, the air between powder can be discharged, petroleum coke powder is made to press close
Real, graphite bulk strength obtained is higher, and graphite jig made from the graphite block is made not opened after high temperature and fast cooling
It splits, prolongs the service life；It is impregnated using high pressure, pitch can be made to enter in the stomata generated in roasting process, can be improved
The bulk density and mechanical strength of graphite block make graphite jig will not cracking after experience multiple high temp and fast cooling, extend
Service life.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of graphite jig, it is characterised in that：Its raw material is made of following components in parts by weight：Grain size is 1
10~15 parts by weight of petroleum coke powder that 10~15 parts by weight of petroleum coke powder of~3mm, grain size are 0.5~1.5mm, grain size 0.05
20~30 parts by weight of petroleum coke powder of~0.1mm, grain size are less than 20~35 parts by weight of 0.05mm petroleum coke powders, 20~25 weight of pitch
Part is measured, preparation method includes the following steps：
(1) it calcines：By petroleum coke powder at 1350~1400 DEG C vacuum calcining 20~30 minutes；
(2) it crushes, dispensing：Petroleum coke powder after calcining is put into pulverizer and is crushed, the petroleum coke powder completed will be crushed
It is put into screening machine and is screened, it is 0.5~1.5mm particles, grain to be sieved into particle, particle size range that particle size range is 1~3mm
Diameter ranging from 0.05~0.1mm particles and grain size are less than four kinds of specifications of fine powder of 0.05mm, are then 1~3mm's according to grain size
10~15 parts by weight of petroleum coke powder that 10~15 parts by weight of petroleum coke powder, grain size are 0.5~1.5mm, grain size are 0.05~0.1mm
20~30 parts by weight of petroleum coke powder, grain size be less than 20~35 parts by weight of 0.05mm petroleum coke powders ratio dispensing；
(3) kneading：The raw material that above-mentioned steps (2) are prepared is placed in kneading machine, kneading, kneading are carried out at 110~150 DEG C
Time is 40~60min；Then the pitch of 20~25 parts by weight is added, then carries out 40~60min of kneading；
(4) isostatic pressing：Raw material obtained by above-mentioned steps (3) is put into rubber mold, is then placed in iso-static pressure shaping machine
It is shaped to graphite block, the pressure of isostatic pressing is 100~200 DEG C；
(5) it roasts：It will be placed in the roaster for the mixed gas for being connected with nitrogen and methane through step (4) molding graphite block
Reason, treatment temperature are 1100~1300 DEG C；
(6) it impregnates：It will be put into the high-pressure impregnation tank equipped with impregnating pitch after the graphite block natural cooling after step (5) roasting
Middle dipping 8~9 hours；
(7) after baking：The graphite block completed through step (6) dipping is put into the roasting for the mixed gas for being connected with nitrogen and methane
It is handled in stove, treatment temperature is 1100~1300 DEG C；
(8) graphitization processing：The graphite block completed through step (6) after baking is put into graphitizing furnace and is graphitized, stone
The temperature of inkization stove is 2800~3500 DEG C, and graphitization time is 84~96 hours；
(9) graphite jig is prepared：Graphite block made from step (8) is prepared into the graphite of different model and specification by machining
Mold.
2. the preparation method of graphite jig according to claim 1, it is characterised in that：The grain size of the pitch is less than
10mm。
3. the preparation method of graphite jig according to claim 1, it is characterised in that：Pulverizer in the step (2)
Rotating speed is 500~700 turns/min, and grinding time is 20~30min.
4. the preparation method of graphite jig according to claim 1, it is characterised in that：Step (5) roasting time is equal
It is 25~40 days.
5. the preparation method of graphite jig according to claim 1, it is characterised in that：Roasting time in the step (7)
It is 10~15 days.
6. the preparation method of graphite jig according to claim 1, it is characterised in that：In the step (5) and step (7)
Treatment temperature speed is no more than 1 DEG C/h, and temperature difference requirement is less than 20 DEG C in stove.
7. the preparation method of graphite jig according to claim 1, it is characterised in that：Step (6) the mesohigh dipping
The pressure of tank is 0.2~0.25MPa, and temperature is 200~250 DEG C.
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| CN109694251A (en) * | 2019-03-07 | 2019-04-30 | 中国科学院山西煤炭化学研究所 | A kind of low-resistivity graphite material and preparation method thereof with anti-oxidation function |
| CN109865815A (en) * | 2019-03-12 | 2019-06-11 | 泗阳敏于行精密机械有限公司 | A kind of manufacturing method of the graphite spreader used in manufacture wheel hub process |
| CN115246737A (en) * | 2022-08-09 | 2022-10-28 | 中钢集团南京新材料研究院有限公司 | Roasting method for preparing isostatic pressing graphite product and product thereof |
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| CN109694251A (en) * | 2019-03-07 | 2019-04-30 | 中国科学院山西煤炭化学研究所 | A kind of low-resistivity graphite material and preparation method thereof with anti-oxidation function |
| CN109865815A (en) * | 2019-03-12 | 2019-06-11 | 泗阳敏于行精密机械有限公司 | A kind of manufacturing method of the graphite spreader used in manufacture wheel hub process |
| CN109865815B (en) * | 2019-03-12 | 2021-03-16 | 泗阳敏于行精密机械有限公司 | Manufacturing method of graphite shunt cone used in aluminum hub die-casting process |
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