CN108821770B - A kind of preparation method of high performance graphite sealing material - Google Patents
A kind of preparation method of high performance graphite sealing material Download PDFInfo
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- CN108821770B CN108821770B CN201810819092.4A CN201810819092A CN108821770B CN 108821770 B CN108821770 B CN 108821770B CN 201810819092 A CN201810819092 A CN 201810819092A CN 108821770 B CN108821770 B CN 108821770B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/0097—Press moulds; Press-mould and press-ram assemblies
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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
- C04B35/522—Graphite
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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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract
The invention discloses a kind of preparation methods of high performance graphite sealing material, belong to carbon material processing technique field.This method is to mix partial size in 50 μm of pitch coke powders below in 50 μm of graphite powders and partial size below in 10 μm of ultra-fine coke powders below, partial size, add the mid temperature pitch that softening point is 70 DEG C -100 DEG C, Residual carbon is 30wt%-50wt%, roller sheet after kneading, it is crushed milling after cooling, press-powder is made；By annular casted die mould compression moulding, the prefabricated green compact of annular are placed in closed crucible and are roasted, are impregnated after the completion, graphitizing furnace is packed into after the completion of dipping and is graphitized, graphite sealing material is obtained after the completion of graphitization.Graphite sealing material dense uniform of the present invention, wearability is good, and degree of graphitization is high, and high mechanical strength, the porosity is low, and ratio of briquetting and roasting yield rate are improved, and save raw material, reduce production cost.
Description
Technical field
The present invention relates to a kind of preparation methods of high performance graphite sealing material, belong to carbon material processing technique field.
Background technique
It is higher and higher with graphite sealing material technical requirements to aviation with the continuous development of China's Aviation Industry.Certain boat
Empty engine is completely dependent on import with graphite sealing material, and the country there is no such material to can satisfy requirement.System of the present invention
Standby graphite sealing material technical indicator reaches requirement, fills the domestic gaps.
Coke powder is one of raw material of graphite sealing material, is mostly used greatly in the preparation process of conventional graphite sealing material old-fashioned
Milling equipment prepares coke powder, and the coke fines size of acquisition prepares graphite grazing using the coke powder of the granularity about at 50 μm or so
Material haves the shortcomings that structure is not fine and close enough, the porosity is big.
It is to be prepared into solid core blank mostly in compacting process in the preparation process of conventional graphite sealing material, so
Afterwards be used for subsequent roasting technique, but it is subsequent graphite sealing material is prepared into product during need shaping, remove nothing
Place, wastage of material is than more serious.
Using the roasting technique of conventional graphite sealing material, big specification, fine grained endless shaper article are roasted, are also easy to produce
Contraction distortion phenomenon, leads to Mass Cracking.
Summary of the invention
For the leakproofness and wearability for improving graphite sealing material, the present invention provides a kind of high performance graphite sealing materials
Preparation method, the technical solution adopted is as follows:
The purpose of the present invention is to provide a kind of preparation methods of carbon material of resistance to ablation, and this method comprises the following steps:
1) partial size is below at 50 μm in 50 μm of graphite powders and partial size below in 10 μm of ultra-fine coke powders below, partial size
Pitch coke powder mixes, and obtains mixture；
2) to step 1) obtain mixture in be added softening point be 70 DEG C -100 DEG C, Residual carbon 30wt%-50wt%
Mid temperature pitch, kneading 2h-3h material temperature reaches 150-170 DEG C, then the roller sheet at 130 DEG C -150 DEG C, cooling after roller sheet, is crushed
Milling, is made press-powder；
3) press-powder that step 2) obtains is passed through annular casted die mould to carry out under conditions of room temperature and 50MPa-100Mpa
Compression moulding obtains the prefabricated green compact of annular；
4) step 3) is obtained the prefabricated green compact of annular to be placed in closed crucible, is roasted by predetermined heating curve,
Crucible is inside and outside to fill metallurgical coke, after the completion of roasting by product temperature be 150 DEG C -300 DEG C, pressure 1MPa-3MPa, time it is big
It is impregnated under conditions of 5h by impregnating agent of pitch, repeats above-mentioned roasting and Pitch-impregnation Process 2-3 times；
5) green body after step 4) roasts and impregnates is packed into graphitizing furnace, with 0.5~5mm and two kinds of 5~20mm
Coke is filler, and the ash content of coal is insulation material in 5% carbon black below, carries out graphitization processing, stone by predetermined graphitization curve
Graphite sealing material is obtained after the completion of inkization.
It preferably, is in terms of 100% by the total weight of mixture in step 1), three kinds of components are according to following weight in mixture
Percentage mixing: the content of ultra-fine coke powder is 65wt%-70wt%, and pitch coke powder is 20-25wt%, graphite powder 5wt%-
15wt%；Pitch is added by the 40wt%-50wt% of mixture summation in step 2).
It is highly preferred that by the total weight of mixture being in terms of 100% in step 1), three kinds of components are according to following weight in mixture
Measure percentage mixing: ultra-fine coke powder 70wt%, pitch coke powder 20wt%, graphite powder 10wt%；Pitch presses mixture in step 2)
The 45wt% of summation is added.
Preferably, the partial size is in 10 μm of ultra-fine coke powders below the preparation method comprises the following steps: coke is put into tricyclic micropowder grinding
It in powder machine, is milled, obtains under conditions of 92A, frequency conversion grader current control are in 108A in the current control of high-pressure suction fan
Partial size is in 10 μm of ultra-fine coke powders below.
Preferably, it is 93 DEG C that the step 2) mid temperature pitch, which selects asphalt softening point, the pitch that Residual carbon is 40wt%.
Preferably, in step 3) press-powder in 100MPa down-pressing type.
Preferably, bituminizing described in step 4) be temperature be 190 DEG C, pressure 1MPa, time 5h under conditions of with
Pitch is that impregnating agent is impregnated twice.
Preferably, the predetermined heating curve of the step 4) roasting are as follows:
Most preferably, the predetermined heating curve of the step 4) roasting are as follows:
Preferably, it is 2300 DEG C -2500 DEG C that graphitization temperature is controlled in the treatment process of the step 5) graphitization processing,
The predetermined graphitization curve are as follows:
Unit power consumption amount is 8.0 ± 0.5kWh/kg, and when power maximum has maintained blowing out after unit power consumption amount.
Optimally, step 5) the predetermined graphitization curve are as follows:
Unit power consumption amount is 8.0 ± 0.5kWh/kg, and when power maximum has maintained blowing out after unit power consumption amount.
Preferably, annular casted die mould described in step 3) includes binder component and charge component；
The binder component includes die shank 1, top connection 2 and upper male mould 3；Wherein: 1 bottom of die shank and top connection 2 are solid
Fixed connection；The top connection 2 is cylindrical and is internally provided with the first cylindrical cavity；The bottom wall body of the top connection 2
It is fixedly connected with upper male mould 3；The upper male mould 3 is in circular ring shape, the difference of the outer diameter and inner diameter of upper male mould 3 and the wall thickness of top connection 2
It is equal；
The charge component includes 9,4 mold core 4, former 5, lower punch 6, upper pad post 7, lower contact 8, Pressure Block lower pad columns
10, top plate 11, mandril 12 and 4 piece charging ram 13, in which: the mold core 4 is in cylindrical, and its bottom is equipped with protrusion；It is described
Former 5 is cylindrical, is internally provided with the second cylindrical cavity, and the bottom of 5 lateral wall of former is equipped with a circle along the circumferential direction
The outer convex edge of the circular ring shape of setting；The circular ring shape is fixedly connected with multiple evenly arranged upper pad posts 7 immediately below outer convex edge；Institute
The underface for stating multiple evenly arranged upper pad posts 7 is fixedly connected with Pressure Block 9；The bottom of the Pressure Block 9 and 4 lower pad columns
10 are fixedly connected；The Pressure Block 9 is equipped with I-shaped inner hole, the top ruler of I-shaped inner hole in cylindrical and its inside center
The very little bump sizes with 4 bottom of mold core match；The mold core 4 is inserted into the second cylindrical cavity center of former 5 and mold core 4
Top is concordant with the top of former 5, and 4 bottom of mold core is pierced by from 5 bottom of former and the protrusion of 4 bottom of mold core is inserted into I-shaped inner hole
Top, mold core 4 is fixedly connected with Pressure Block 9 by screw；It is empty that annular is formed between 4 outer wall of mold core and 5 inner wall of former
Chamber, having a circle in the underfill of toroidal cavity is in the lower punch 6 of circular ring shape, the size of the lower punch 6 and toroidal cavity
Size matches；The bottom of the lower punch 6 is fixedly connected with lower contact 8；The inside of the Pressure Block 9 toroidal cavity just
Lower section is additionally provided with 4 evenly arranged through-holes；The top of 4 charging rams 13 is each passed through 4 through-holes of Pressure Block 9 under
Connector 8 is fixedly connected；The bottom of 4 charging rams 13 be located at the bottom end of the outside of Pressure Block 9 and 4 charging rams 13 respectively with
Top plate 11 is fixedly connected；11 bottom centre of top plate is fixedly connected with mandril 12；
The difference of the outer diameter and inner diameter of the upper male mould 3, the wall thickness of top connection 2 match with the size of toroidal cavity respectively,
So that top connection 2 and upper male mould 3 are inserted into toroidal cavity；The size of the lower contact 8, the size of 4 charging rams 13 are divided
Do not match with the size of toroidal cavity, so that lower contact 8 and 4 piece charging ram 13 is inserted into toroidal cavity；
It is empty by the way that the annular that mold core 4 and former 5 are formed is inserted into top connection 2 and upper male mould 3 to the pressure of die shank 1 when binder
It is intracavitary, and mold core 4 is inserted into the first cylindrical cavity of top connection 2；When feeding, driving mandril 12 is moved up, mandril
12 promotion top plates 11 move up, and top plate 11 drives 4 charging rams 13 to push up lower contact 8, and lower contact 8 pushes lower punch 6
It moves up and completes feeding.
Lower pad column 10 is fixed on die mould machine by above-mentioned annular casted die mould when in use.
Annular casted die mould of the invention is placed in mold core outer wall and former inner hole wall in use, by compacting powder
Between be formed by toroidal cavity, by hydraulic press drive upper male mould movement by powder pressing cyclization shape sealing ring, pass through liquid
Cylinder pressure drives mandril to move upwards lower punch and ejects ring type seal.By using the structure annular casted die mould not only
The quality of suppressed ring type seal is improved, and the ring type seal after the completion of compacting can be made no longer to need to scratch
Hole is greatly saved the consumption of raw material, reduces manufacturing procedure, shortens the process-cycle, having saved the energy and improve production
Efficiency.The two cooperation precision that the upper male mould and female mould structure that the present invention designs are is high, ensure that the quality of product.
The invention has the advantages that:
The present invention using partial size in 10 μm of ultra-fine coke powders below as primary raw material, and cooperate partial size below at 50 μm
Graphite powder, partial size 50 μm of pitch coke powders and softening point below be 70 DEG C -100 DEG C, the drip that Residual carbon is 30wt%-50wt%
It is green.The structure that graphite material has dense uniform wherein can be improved using ultra-fine coke powder；Graphite powder has good self-lubricating
Property suitable graphite powder is added can make graphite material that there is better wearability；Since pitch can infiltrate and permeate well coke
Carbon surface and hole gradually decompose carbonization in roasting, coke granule can be firmly linked together, and it analyses burnt rate
Higher also easy graphitization can improve the comprehensive performance of graphite material and perfect so using pitch as binder
The purpose of its structure.The present invention is by solving the problems, such as above-mentioned raw materials rational proportion that graphite material structure is not fine and close enough, mentioning
While high mechanical strength, the porosity of graphite material is reduced.It obtains and meets requirement, there is good seal performance
With the graphite sealing material of wear-resisting property.
The preparation of micro mist be it is relatively difficult, be difficult by granularity control at 10 μm hereinafter, the present invention is for the first time by tricyclic differential
Flour mill is applied to the preparation process of graphite sealing material, prepares 10 μm of ultra-fine coke powders below by tricyclic differential flour mill,
Effectively the granularity of ultra-fine coke powder can be controlled at 10 μm hereinafter, being used then applied to the processing technology of graphite sealing material
10 μm of ultra-fine coke powders below are the structure that raw material can make graphite sealing material even compact.
Press-powder is suppressed into ring by using annular compression moulding technology, by the ring mould of design by the method for the present invention
The prefabricated green compact of shape can solve using the prefabricated green compact of annular and occur the problem of layer is split in forming process, and ratio of briquetting is improved, and
The prefabricated green compact of section annular can also save raw material, reduce production cost.
The present invention can solve by filling metallurgical coke inside and outside crucible and aoxidize problem on deformation in product roasting process, improve
Product serviceability rate.
Baking technology of the present invention can solve the problem of contraction distortion in product roasting process, improve roasting yield rate.
Graphitization technique of the invention formulates reasonable unit power consumption amount and strict control, guarantees product degree of graphitization, machine
Tool intensity is double high.
The method of the present invention utilizes product itself that is, by the way that product to be placed in closed crucible using hot pressure sintering
Elastic after effect forms pressure, to achieve the purpose that pressure sintering, what which solved that product cracks in roasting process is asked
Topic, so that without cracking phenomena in product roasting process, high yield rate is up to 100%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of annular compacting tool set；
(1, die shank；2, top connection；3, upper male mould；4, mold core；5, former；6, lower punch；7, upper pad post；8, lower contact；9,
Pressure Block；10, lower pad column；11, top plate；12, mandril；13, charging ram).
Specific embodiment
The present invention will be further described combined with specific embodiments below, but the present invention should not be limited by the examples.
Embodiment 1
A kind of preparation method of carbon material of resistance to ablation is present embodiments provided, this method comprises the following steps:
1) partial size is below at 50 μm in 50 μm of graphite powders and partial size below in 10 μm of ultra-fine coke powders below, partial size
Pitch coke powder mixes, and obtains mixture；Wherein: being in terms of 100% by the total weight of mixture, three kinds of components are according to such as in mixture
Lower weight percent mixing: the content of ultra-fine coke powder is 70wt%, and pitch coke powder is 20wt%, graphite powder 10wt%；
It 2) is 93 DEG C, Residual carbon according to the 45wt% addition softening point of mixture summation in the mixture obtained to step 1)
For the mid temperature pitch of 40wt%, kneading 3h material temperature reaches 160 DEG C, then the roller sheet at 130 DEG C, the thickness of roller sheet in 2mm hereinafter,
And will the piece that rolled into it is cooling after be crushed milling to partial size at 70 μm hereinafter, press-powder is made；
3) press-powder that step 2) obtains is passed through annular casted die mould to be pressed under conditions of room temperature and 100Mpa
Type obtains the prefabricated green compact of annular；
4) step 3) is obtained the prefabricated green compact of annular to be placed in closed crucible, is roasted by predetermined heating curve,
Crucible is inside and outside to fill metallurgical coke, after the completion of roasting by product under conditions of temperature is 190 DEG C, pressure 1MPa, time 5h with drip
Blueness is that impregnating agent is impregnated, and repeats above-mentioned roasting and dipping process 2-3 times；
5) green body after step 4) roasts and impregnates is packed into graphitizing furnace, with 0.5~5mm and two kinds of 5~20mm
Coke is filler, and the ash content of coal is insulation material in 5% carbon black below, carries out graphitization processing, stone by predetermined graphitization curve
Graphite sealing material is obtained after the completion of inkization.
" partial size is in 10 μm of ultra-fine coke powders below " described in the present embodiment step 1) the preparation method comprises the following steps: coke is put into three
In ring micro mist flour mill, ground under conditions of 92A, frequency conversion grader current control are in 108A in high-pressure suction fan current control
Powder obtains partial size in 10 μm of ultra-fine coke powders below.
The predetermined heating curve roasted in the present embodiment step 4) are as follows:
It is 2300 DEG C -2500 DEG C that graphitization temperature is controlled during graphitization processing described in the present embodiment step 5),
Predetermined graphitization curve are as follows:
Unit power consumption amount is 8.0 ± 0.5kWh/kg, and when power maximum has maintained blowing out after unit power consumption amount.
Annular casted die mould described in the present embodiment step 3) includes binder component and charge component；Binder component includes mould
Handle 1, top connection 2 and upper male mould 3；Wherein: 1 bottom of die shank is fixedly connected with top connection 2；The top connection 2 is cylindrical
And it is internally provided with the first cylindrical cavity；The bottom wall body of the top connection 2 is fixedly connected with upper male mould 3；It is described convex
Mould 3 is in circular ring shape, and the difference of the outer diameter and inner diameter of upper male mould 3 is equal with the wall thickness of top connection 2；Charge component includes mold core 4, former
5, lower punch 6, upper pad post 7, lower contact 8,9,4 lower pad columns 10 of Pressure Block, top plate 11, mandril 12 and 4 piece charging ram 13,
In: the mold core 4 is in cylindrical, and its bottom is equipped with protrusion；The former 5 is cylindrical, is internally provided with the second cylinder
Cone cavity, the bottom of 5 lateral wall of former are equipped with the outer convex edge of the peripherally disposed circular ring shape of a circle；The circular ring shape evagination
Multiple evenly arranged upper pad posts 7 are fixedly connected with immediately below edge；The underface of the multiple evenly arranged upper pad post 7 with
Pressure Block 9 is fixedly connected；The bottom of the Pressure Block 9 is fixedly connected with 4 lower pad columns 10；The Pressure Block 9 is in cylindrical
And its inside center is equipped with I-shaped inner hole, the top dimension of I-shaped inner hole and the bump sizes of 4 bottom of mold core match；Institute
State the second cylindrical cavity center and 4 top, mold core 4 bottom concordant with the top of former 5 of mold core that mold core 4 is inserted into former 5
Be pierced by from 5 bottom of former and the protrusion of 4 bottom of mold core to be inserted into the top of I-shaped inner hole, mold core 4 and Pressure Block 9 solid by screw
Fixed connection；Toroidal cavity is formed between 4 outer wall of mold core and 5 inner wall of former, has the circle to be in the underfill of toroidal cavity
The lower punch 6 of circular ring shape, the size of the lower punch 6 and the size of toroidal cavity match；The bottom of the lower punch 6 is under
Connector 8 is fixedly connected；The inside of the Pressure Block 9 is additionally provided with 4 evenly arranged through-holes immediately below toroidal cavity；It is described
4 through-holes that the top of 4 charging rams 13 is each passed through Pressure Block 9 are fixedly connected with lower contact 8；4 charging rams 13
Bottom is located at the outside of Pressure Block 9 and the bottom end of 4 charging rams 13 and is fixedly connected respectively with top plate 11；In 11 bottom of top plate
The heart is fixedly connected with mandril 12；The difference of the outer diameter and inner diameter of upper male mould 3, top connection 2 wall thickness respectively with the size of toroidal cavity
Match, so that top connection 2 and upper male mould 3 are inserted into toroidal cavity；The size of the lower contact 8,4 charging rams 13
Size matches with the size of toroidal cavity respectively, so that lower contact 8 and 4 piece charging ram 13 is inserted into toroidal cavity；
It is empty by the way that the annular that mold core 4 and former 5 are formed is inserted into top connection 2 and upper male mould 3 to the pressure of die shank 1 when binder
It is intracavitary, and mold core 4 is inserted into the first cylindrical cavity of top connection 2；When feeding, driving mandril 12 is moved up, mandril
12 promotion top plates 11 move up, and top plate 11 drives 4 charging rams 13 to push up lower contact 8, and lower contact 8 pushes lower punch 6
It moves up and completes feeding.Lower pad column 10 is fixed on die mould machine by above-mentioned annular casted die mould when in use.
The annular casted die mould is placed in institute between mold core outer wall and former inner hole wall in use, by compacting powder
In the toroidal cavity of formation, drives upper male mould movement by powder pressing cyclization shape sealing ring by hydraulic press, pass through hydraulic cylinder band
Dynamic mandril moves upwards lower punch to eject ring type seal.
The extrudate density that the present embodiment obtains is 1.90g/cm3, Shore hardness 55, degree of graphitization 90%.
Embodiment 2
The present embodiment the difference from embodiment 1 is that each composition of raw materials is different, specifically: with mixed in the present embodiment step 1)
The total weight for closing material is 100% meter, and three kinds of components are mixed according to following weight percent in mixture: the content of ultra-fine coke powder is
70wt%, graphite powder 5wt%, pitch coke powder 25wt%；Pitch is added by the 50wt% of mixture summation in step 2).
The extrudate density that the present embodiment obtains is 1.87g/cm3, Shore hardness 53, degree of graphitization 88%
Embodiment 3
The present embodiment the difference from embodiment 1 is that each composition of raw materials is different, specifically: with mixed in the present embodiment step 1)
The total weight for closing material is 100% meter, and three kinds of components are mixed according to following weight percent in mixture: the content of ultra-fine coke powder is
65wt%, graphite powder 15wt%, pitch coke powder 20wt%；Pitch is added by the 40wt% of mixture summation in step 2).
The extrudate density 1.83g/cm that the present embodiment obtains3, Shore hardness 51, degree of graphitization 87%.
Embodiment 4
The present embodiment the difference from embodiment 1 is that each composition of raw materials is different, specifically: with mixed in the present embodiment step 1)
The total weight for closing material is 100% meter, and three kinds of components are mixed according to following weight percent in mixture: the content of ultra-fine coke powder is
65wt%, graphite powder 10wt%, pitch coke powder 25wt%；Pitch is added by the 40wt% of mixture summation in step 2).
The extrudate density 1.84g/cm that the present embodiment obtains3, Shore hardness 51, degree of graphitization 88%.
Embodiment 5
The present embodiment the difference from embodiment 1 is that: the softening point of mid temperature pitch used in the present embodiment be 70 DEG C, Residual carbon
For 30wt%.
Embodiment 6
The present embodiment the difference from embodiment 1 is that: the softening point of mid temperature pitch used in the present embodiment be 100 DEG C, carbon residue
Rate is 50wt%.
Embodiment 7
The present embodiment the difference from embodiment 1 is that: the present embodiment step 2) is that kneading 2h material temperature reaches 160 DEG C, then
The roller sheet at 130 DEG C, it is cooling after roller sheet, it is crushed milling, press-powder is made；Step 3) is pressed under conditions of 50MPa
Type obtains the prefabricated green compact of annular；In step 4) after the completion of roasting by product temperature is 150 DEG C, pressure 1MPa, time are greater than
It is impregnated under conditions of 5h by impregnating agent of pitch, repeats above-mentioned roasting and Pitch-impregnation Process 2 times.
Embodiment 8
The present embodiment the difference from embodiment 1 is that: the present embodiment step 2) is that kneading 3h material temperature reaches 160 DEG C, then
The roller sheet at 150 DEG C, it is cooling after roller sheet, it is crushed milling, press-powder is made；Step 3) is pressed under conditions of 100MPa
Type obtains the prefabricated green compact of annular；In step 4) after the completion of roasting by product temperature is 300 DEG C, pressure 3MPa, time are greater than
It is impregnated under conditions of 5h by impregnating agent of pitch, repeats above-mentioned roasting and Pitch-impregnation Process 2 times.
The beneficial effect that method can obtain to illustrate the invention has carried out following experiment:
Control group 1: the 10 μm of ultra-fine coke powders below in coke powder alternative embodiment 1 for being 50 μm with partial size, other steps
It is carried out according to embodiment 1 with formula；
Control group 2: the annular press-moulding die in embodiment 1 is replaced with typical round compacting tool set in this experiment forming process
Tool, other steps and formula are carried out according to embodiment 1；
Control group 3: this experiment is commonly baked mode pressurization is replaced to bake mode using existing, i.e., obtains step 3)
Raw embryo is directly placed at roasting kiln roasting (raw embryo is not put into closed crucible), other steps and formula are according to embodiment
1 carries out；
The performance indicator of comparing embodiment 1-8 and control group 1-3 resulting product, experimental result are as shown in table 1.
The effect of 1 control group of table and experimental group compares
By comparing embodiment 1-8 with control group 1 it follows that the present invention is below ultra-fine at 10 μm by using partial size
Coke powder solves the problems, such as that graphite material structure is not fine and close enough as primary raw material, and graphite material can be made to have dense uniform
Structure reduce the porosity of graphite material, while graphite sealing material is had and while improving mechanical strength
There are good seal performance and wearability.
By comparing embodiment 1-8 and control group 2 it follows that the present invention prepares annular by using annular casted die mould
Prefabricated green compact, can solve and occur the problem of layer is split in raw embryo forming process, improve ratio of briquetting, and save the prefabricated green compact of annular
Raw material can also be saved, reduce production cost.
By comparing embodiment 1-8 and control group 3 it follows that the hot pressure sintering technology that the present invention uses, i.e., by raw embryo
It is put into closed crucible and roasts, can solve the problems, such as traditional baking modes product cracking, product roasting yield rate is effectively ensured.
Although the present invention has been disclosed in the preferred embodiment as above, it is not intended to limit the invention, any to be familiar with this
The people of technology can do various changes and modification, therefore protection of the invention without departing from the spirit and scope of the present invention
Range should subject to the definition of the claims.
Claims (10)
1. a kind of preparation method of high performance graphite sealing material, which is characterized in that described method includes following steps:
1) by partial size in 10 μm of ultra-fine coke powders below, partial size in 50 μm of graphite powders and partial size below in 50 μm of pitches below
Coke powder mixes, and obtains mixture；
2) addition softening point is 70 DEG C -100 DEG C in the mixture obtained to step 1), Residual carbon is in 30wt%-50wt%
Warm pitch, kneading 2h-3h material temperature reach 150 DEG C -170 DEG C, then the roller sheet at 130 DEG C -150 DEG C, cooling after roller sheet, are crushed mill
Press-powder is made in powder；
3) press-powder that step 2) obtains is passed through annular casted die mould to suppress under conditions of room temperature and 50MPa-100Mpa
Molding obtains the prefabricated green compact of annular；
4) step 3) is obtained the prefabricated green compact of annular to be placed in closed crucible, is roasted by predetermined heating curve, crucible
Inside and outside filling metallurgical coke, after the completion of roasting by product temperature be 150 DEG C -300 DEG C, pressure 1MPa-3MPa, time >=5h
Under the conditions of impregnated by impregnating agent of pitch, repeat above-mentioned roasting and Pitch-impregnation Process 2-3 times；
5) green body after step 4) roasts and impregnates is packed into graphitizing furnace, with two kinds of cokes of 0.5~5mm and 5~20mm
For filler, the ash content of coal is insulation material in 5% carbon black below, carries out graphitization processing, graphitization by predetermined graphitization curve
Graphite sealing material is obtained after the completion.
2. the method according to claim 1, wherein in step 1) by the total weight of mixture be 100% in terms of, mix
Close three kinds of components in material to mix according to following weight percent: the content of ultra-fine coke powder is 65wt%-70wt%, and pitch coke powder is
20-25wt%, graphite powder 5wt%-15wt%；Pitch is added by the 40wt%-50wt% of mixture summation in step 2).
3. the method according to claim 1, wherein in step 1) by the total weight of mixture be 100% in terms of, mix
It closes three kinds of components in material to mix according to following weight percent: ultra-fine coke powder 70wt%, pitch coke powder 20wt%, graphite powder
10wt%；Pitch is added by the 45wt% of mixture summation in step 2).
4. the method according to claim 1, wherein the step 1) partial size is in 10 μm of ultra-fine coke powders below
The preparation method comprises the following steps: coke is put into tricyclic micro mist flour mill, high-pressure suction fan current control in 92A, frequency conversion grader
Current control is milled under conditions of 108A, obtains partial size in 10 μm of ultra-fine coke powders below.
5. the method according to claim 1, wherein it is 93 that the step 2) mid temperature pitch, which selects asphalt softening point,
DEG C, Residual carbon be 40wt% pitch.
6. the method according to claim 1, wherein press-powder is in 100MPa down-pressing type in step 3).
7. the method according to claim 1, wherein bituminizing described in step 4) be temperature be 190 DEG C,
It is impregnated twice under conditions of pressure 1MPa, time 5h using pitch as impregnating agent.
8. the method according to claim 1, wherein the predetermined heating curve of the step 4) roasting are as follows:
9. the method according to claim 1, wherein being controlled in the treatment process of the step 5) graphitization processing
Graphitization temperature is 2300 DEG C -2500 DEG C, the predetermined graphitization curve are as follows:
Unit power consumption amount is 8.0 ± 0.5kWh/kg, and when power maximum has maintained blowing out after unit power consumption amount.
10. the method according to claim 1, wherein annular casted die mould described in step 3) includes binder group
Part and charge component；
The binder component includes die shank (1), top connection (2) and upper male mould (3)；Wherein: die shank (1) bottom and top connection
(2) it is fixedly connected；The top connection (2) is cylindrical and is internally provided with the first cylindrical cavity；The top connection (2)
Bottom wall body is fixedly connected with upper male mould (3)；The upper male mould (3) be in circular ring shape, the difference of the outer diameter and inner diameter of upper male mould (3) with
The wall thickness of top connection (2) is equal；
The charge component includes mold core (4), former (5), lower punch (6), upper pad post (7), lower contact (8), Pressure Block (9), 4
Root lower pad column (10), top plate (11), mandril (12) and 4 charging rams (13), in which: the mold core (4) is in cylindrical, and its
Bottom is equipped with protrusion；The former (5) is cylindrical, is internally provided with the second cylindrical cavity, the bottom of former (5) lateral wall
Portion is equipped with the outer convex edge of the peripherally disposed circular ring shape of a circle；It is fixedly connected with immediately below the outer convex edge of the circular ring shape multiple
Evenly arranged upper pad post (7)；The underface of the multiple evenly arranged upper pad post (7) is fixedly connected with Pressure Block (9)；Institute
The bottom for stating Pressure Block (9) is fixedly connected with 4 lower pad columns (10)；The Pressure Block (9) is in cylindrical and its inside center
Equipped with I-shaped inner hole, the top dimension of I-shaped inner hole and the bump sizes of mold core (4) bottom match；The mold core (4)
It is inserted into, mold core (4) bottom concordant with the top of former (5) at the top of the second cylindrical cavity center of former (5) and mold core (4)
It is pierced by from former (5) bottom and the protrusion of mold core (4) bottom is inserted into the top of I-shaped inner hole, mold core (4) and Pressure Block (9) are logical
Screw is crossed to be fixedly connected；Toroidal cavity is formed between mold core (4) outer wall and former (5) inner wall, in the bottom of toroidal cavity
It is in the lower punch (6) of circular ring shape filled with a circle, the size of the lower punch (6) and the size of toroidal cavity match；It is described
The bottom of lower punch (6) is fixedly connected with lower contact (8)；The inside of the Pressure Block (9) is also set in the underface of toroidal cavity
There are 4 evenly arranged through-holes；4 through-holes and the lower contact of Pressure Block (9) are each passed through at the top of 4 charging rams (13)
(8) it is fixedly connected；The bottom of 4 charging rams (13) is located at the bottom end point of the outside of Pressure Block (9) and 4 charging rams (13)
It is not fixedly connected with top plate (11)；Top plate (11) bottom centre is fixedly connected with mandril (12)；
The difference of the outer diameter and inner diameter of the upper male mould (3), the wall thickness of top connection (2) match with the size of toroidal cavity respectively,
So that top connection (2) and upper male mould (3) are inserted into toroidal cavity；The size of the lower contact (8), 4 charging rams (13)
Size match respectively with the size of toroidal cavity so that lower contact (8) and 4 charging rams (13) are inserted into toroidal cavity
It is interior；
When binder, pass through top connection (2) and upper male mould (3) insertion mold core (4) and former (5) is formed to die shank (1) pressure
In toroidal cavity, and will be in the first cylindrical cavity of mold core (4) insertion top connection (2)；When feeding, driving mandril (12) to
Upper movement, mandril (12) push top plate (11) to move up, and top plate (11) drives 4 charging rams (13) to push up lower contact
(8), lower contact (8) pushes lower punch (6) to move up and completes feeding.
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| CN114014658A (en) * | 2020-12-21 | 2022-02-08 | 哈尔滨电碳厂有限责任公司 | Preparation method of oxidation-resistant graphite material matrix |
| CN114014661A (en) * | 2020-12-21 | 2022-02-08 | 哈尔滨电碳厂有限责任公司 | Preparation method of wear-resistant graphite sealing material with high environmental adaptability |
| TWI785803B (en) * | 2021-09-15 | 2022-12-01 | 中國鋼鐵股份有限公司 | Isotropic graphite material composition and method of producing isotropic graphite material |
| CN115626826B (en) * | 2022-11-11 | 2023-09-05 | 湖南大学 | Low-density wear-resistant carbon graphite material with independent micropores and preparation method thereof |
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| CN202527254U (en) * | 2012-04-24 | 2012-11-14 | 上海建冶机器有限公司 | Three-ring-mill grinding system |
| CN103286850A (en) * | 2012-09-25 | 2013-09-11 | 江苏宏基炭素科技有限公司 | One-time forming method and special mold for graphite crucible |
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| CN108083806A (en) * | 2017-12-12 | 2018-05-29 | 中国平煤神马集团开封炭素有限公司 | A kind of hyperfine structure isotropic graphite and preparation method thereof |
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|---|---|---|---|---|
| US5590887A (en) * | 1992-12-22 | 1997-01-07 | Toyoda Gosei Co., Ltd. | Sealing apparatus |
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| CN202527254U (en) * | 2012-04-24 | 2012-11-14 | 上海建冶机器有限公司 | Three-ring-mill grinding system |
| CN103286850A (en) * | 2012-09-25 | 2013-09-11 | 江苏宏基炭素科技有限公司 | One-time forming method and special mold for graphite crucible |
| CN107265450A (en) * | 2017-06-20 | 2017-10-20 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of fine structure graphite |
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Address after: 150025 Diantan Road North and Wuxi Street East, Limin Development Zone, Harbin, Heilongjiang Patentee after: Harbin Electric Carbon Plant Co.,Ltd. Address before: 150025 Diantan Road North, Wuxi Street East, Limin Development Zone, Hulan District, Harbin City, Heilongjiang Province Patentee before: HARBIN ELECTRIC CARBON FACTORY |