CN115626826A - Low-density wear-resistant carbon graphite material with independent micropores and preparation method thereof - Google Patents
Low-density wear-resistant carbon graphite material with independent micropores and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-density wear-resistant carbon graphite material with independent micropores and a preparation method thereof, wherein the preparation method comprises the following steps: weighing 60 to 80 parts of graphite fine powder, 1 to 10 parts of superfine artificial graphite powder, 1 to 10 parts of superfine modified green coke powder, 1 to 10 parts of carbon black, 1 to 2 parts of dispersing agent, 40 to 50 parts of asphalt, 1 to 5 parts of coupling agent and 100 to 250 parts of ethanol-acetone mixed solution; adding a dispersing agent into the ethanol-acetone mixed solution, uniformly stirring, sequentially adding the superfine artificial graphite powder and the carbon powder, and performing ultrasonic dispersion to obtain mixed slurry; placing the graphite fine powder and the superfine raw coke powder into a Raymond mill, mixing and milling to obtain mixed fine powder; and putting the mixed fine powder and the mixed slurry into a kneading pot for kneading, when the temperature of the material rises to 180-200 ℃, putting a coupling agent and molten asphalt into the kneading pot, then closing a cover for kneading, and after the kneading is finished, rolling, crushing, grinding, sieving, press-forming and roasting to obtain the carbon graphite material. The prepared carbon graphite material has good mechanical strength, wear resistance, homogeneity and stability.
Description
Technical Field
The invention belongs to the technical field of carbon graphite materials, and particularly relates to a low-density wear-resistant carbon graphite material with independent micropores and a preparation method thereof.
Background
Carbon graphite materials are widely used in aero-engine bearing seal systems, hydraulic seal systems and fuel seal systems due to their excellent mechanical, high temperature resistance and self-lubricating properties. However, with the continuous expansion of the aviation industry, the actual working conditions put higher requirements on the comprehensive performance of the graphite sealing material. At present, the traditional process for preparing the carbon graphite sealing material is to use calcined coke with larger particle size and artificial graphite as aggregate, and asphalt as a binder, and then prepare a green body carbon graphite material after mixing kneading, sheet rolling, crushing, molding and multiple times of dipping and roasting treatment. The carbon graphite material prepared by the process has large particle size of the selected aggregate and needs to be optimized in aggregate matching design, so that the prepared carbon graphite material has large pore diameter and is easy to communicate among pores, and the carbon graphite material has poor comprehensive properties such as mechanical strength, wear resistance, homogeneity, stability and airtightness, and further cannot meet the requirements of the existing sealing material.
In addition, the poor homogeneity and stability are also attributed to the fact that the primary structure of the original blank graphite material is influenced to a certain extent by introducing a dipping densification process in the later stage, and meanwhile, the impregnant pitch is difficult to fully infiltrate the hole wall of the blank, so that the gradient density difference between the surface and the interior of the blank graphite material is caused, and the homogeneity and stability of the blank graphite material are influenced finally.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a low-density wear-resistant carbon graphite material with independent micropores and a preparation method thereof.
The technical scheme of the invention is realized as follows:
a preparation method of a low-density wear-resistant carbon graphite material with independent micropores specifically comprises the following steps:
s1: accurately weighing 60-80 parts of graphite fine powder, 1-10 parts of superfine artificial graphite powder, 1-10 parts of superfine modified raw coke powder, 1-10 parts of carbon black, 1-2 parts of dispersing agent, 40-50 parts of asphalt, 1-5 parts of coupling agent and 100-250 parts of ethanol-acetone mixed solution for later use; the volume ratio of ethanol to acetone in the ethanol-acetone mixed solution is 1;
s2: adding a dispersing agent into the ethanol-acetone mixed solution, uniformly stirring, and then sequentially adding superfine artificial graphite powder and carbon black for ultrasonic dispersion to obtain mixed slurry;
s3: placing the fine graphite powder and the superfine modified raw coke powder into a Raymond mill, mixing and milling for 1-10 min to obtain mixed fine powder;
s4: and putting the mixed fine powder and the mixed slurry into a kneading pot for kneading, when the temperature of the material rises to 180-200 ℃, putting a coupling agent and molten asphalt into the kneading pot, then closing the kneading pot for kneading, after kneading, flaking, crushing, grinding and sieving to obtain pressed powder, then performing compression molding to obtain a green block, and finally roasting to obtain the carbon graphite material.
Furthermore, the D50 of the graphite fine powder is less than or equal to 6 mu m, and the graphite fine powder is prepared by taking the forged asphalt coke or the forged needle coke as a raw material and adopting an air flow mill.
Further, the carbon black is one or two of N220 carbon black, N326 carbon black, N330 carbon black, N339 carbon black, modified carbon black and mesocarbon microbeads; the asphalt is one or two of low-temperature asphalt, medium-temperature asphalt, high-temperature asphalt and modified asphalt.
Further, the dispersing agent is one or two of borate, aminopropylamine dioleate and carboxymethyl cellulose; the coupling agent is one or two of aluminate, phthalate ester and dioxy-acetic acid phthalate ester.
Further, when preparing the mixed slurry, firstly adding the superfine artificial graphite powder into the mixed solution of the dispersing agent and the ethanol for ultrasonic dispersion for 10-30 min, and then adding the carbon powder for ultrasonic dispersion for 10-30 min.
Further, when kneading, the mixed fine powder is firstly put into a kneading pot and mixed for 10-20 min at 100-110 ℃, the rotation speed of the kneading pot is 10-50 r/min, and the cover is opened to rotate forwards; after the material temperature reaches 100-110 ℃, putting the mixed slurry into a kneading pot, kneading for 0.5-1 h, wherein the rotation speed of the kneading pot is 10-50 r/min, and opening the cover to rotate forwards; after the water is completely removed, the temperature of the material is raised to 180-200 ℃, the asphalt in a molten state is put into a kneading pot, simultaneously a coupling agent is put into the kneading pot, the rotating speed of the kneading pot is 10-50 r/min, the forward rotation and the reverse rotation are alternately carried out, and the cover is closed to knead for 0.5-1 h.
Further, when the pressed powder is prepared, the paste obtained by kneading is quickly put into a sheet rolling machine for rolling for 3 to 4 times, the thickness of the rolled sheet is 1 to 2.5mm, the temperature of the rolled sheet is 180 to 200 ℃, the rotating speed is 10 to 25r/min, the sheet material is kept stand for 5 to 10 hours after the rolling is finished, then crushing and grinding are carried out, the crushed and ground material passes through a 100 to 400-mesh screen and then is kept stand for 5 to 10 hours, so that the pressed powder is prepared.
Further, the step of preparing the green block body by the pressed powder comprises the following steps: pressing the pressed powder under 1-10 MPa to prepare a primary blank block, carrying out vacuum packaging, and standing for 5-10 h; placing the mixture in a cold isostatic pressing device, pressing the mixture for 0.5 to 1 hour at the pressure of between 150 and 200MPa, then carrying out gradient pressure relief, taking out the mixture, removing the packaging bag, and standing the mixture for 5 to 10 hours to obtain the product with the density of between 1.59 and 1.62g/cm 3 The green block of (1).
Further, the roasting process is as follows: placing the green body block in a stainless steel crucible, filling the buried burning material, then placing the crucible in a roasting furnace, introducing argon, roasting for 2-4 h at 900-1200 ℃, cooling to 150-300 ℃ under program control, and naturally cooling to room temperature to obtain the product with the volume density of 1.60-1.64 g/cm 3 The roasted block is the carbon graphite material.
The invention also provides a low-density wear-resistant carbon graphite material with independent micropores, which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts graphite fine powder (D50 is less than or equal to 6 mu m) as main aggregate, superfine artificial stone powdered ink (D50 =6 mu m), superfine modified green coke powder (D50 =5 mu m and contains specific volatile component activity) and carbon black (primary particle size is 30 nm) as secondary aggregate, and the carbon black as a wear-resistant agent can improve the mechanical property and the wear resistance of the carbon graphite material. The main aggregate and the secondary aggregate with different particle sizes are adopted for matching, and a homogeneous carbon skeleton is formed in a particle size stacking mode and is of a primary skeleton structure. Meanwhile, the large and small particles can generate an arch bridge effect when being stacked, welding spots are formed among the particles for consolidation, the communication of air holes is blocked in a sand bag plugging-like mode, the aperture of the air holes is reduced, a relatively independent non-communicated microporous structure is formed, and the structure is a secondary welding structure, so that the open porosity can be effectively reduced, and the prepared carbon graphite material has low volume density and good air tightness.
And the surface of the carbon black contains rich oxygen-containing functional groups such as hydroxyl, carboxyl, carbonyl and the like, so that the carbon black can easily act with other aggregate particles, the formation of sintering necks among the particles is promoted, and the synchronous thermal shrinkage among different particles is realized. The superfine modified green coke powder has self-sintering performance, and has large volume shrinkage in the heat treatment process, thereby being beneficial to densification. The mode of carbon black chain sealing and raw coke powder leaking stoppage is adopted, the structure is a three-stage protection structure, the welding spot combination among particles is further enhanced, and the formation of an independent non-communicated microporous structure is promoted.
2. The invention adopts a liquid phase mixing process and adds a dispersing agent to disperse ultrafine particles such as carbon black and the like, effectively avoids the agglomeration phenomenon of the carbon black, and simultaneously introduces a coupling agent in the kneading process, so as to effectively improve the fluidity of the binder asphalt, further promote the formation of sintering necks among aggregate particles during roasting, improve the synchronous volume thermal contraction capacity of different components of the carbon graphite material, and realize structure-function integration.
Ultrafine particles such as carbon black are uniformly dispersed in the aggregate, so that the homogeneity of the carbon graphite material can be effectively improved, crack expansion can be hindered, the bonding strength among the aggregate particles is improved, the wear rate is reduced, and the wear resistance and stability of the carbon graphite material are improved.
3. The invention adopts the mixed solution of ethanol and acetone as the solvent, the ethanol and the acetone are both low boiling point solvents, contain polar molecules and are volatile, and when the ethanol and the acetone are mixed, the volatilization degree can be reduced due to the hydrogen bond effect between the ethanol and the acetone molecules. And the acetone is easy to dissolve grease substances, and the ethanol containing nonpolar hydroxyl can also dissolve some nonpolar substances, so that graphite powder and other weak polar fine powder and lipid dispersing agents can be effectively dissolved.
4. The borate, aminopropylamine dioleate, carboxymethyl cellulose and other dispersing agents adopted by the invention have good matching property with the carbonaceous aggregate, and are adsorbed on the surfaces of particles to form a compact adsorption layer to prevent flocculation and coalescence among the particles, thereby achieving the effect of dispersion stability. In addition, it can reduce the surface tension or interfacial tension to make the liquid droplet smaller, thereby achieving the dispersion effect.
5. The invention does not need multiple times of dipping and roasting, has simple process, can effectively reduce the production cost, shortens the production period and realizes short-flow production and preparation.
Drawings
FIG. 1 is a graph of flexural strength and compressive strength of the carbon graphite material prepared in example 1 and a corresponding cross-sectional micro-topography.
FIG. 2 is a graph showing the friction coefficient and the surface of the graphite material prepared in example 1.
Fig. 3-flexural strength and compressive strength plots and corresponding cross-sectional micro-topography plots for the carbon graphite material prepared in example 2.
FIG. 4-scanning electron micrographs of the surface and friction coefficient profile of the carbon graphite material prepared in example 2.
Fig. 5-flexural strength and compressive strength plots and corresponding cross-sectional micro-topography plots for the carbon graphite material prepared in example 3.
FIG. 6 is a graph showing the friction coefficient and the surface of the graphite material prepared in example 3 under a scanning electron microscope.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
Example 1
1) The calcined asphalt coke is purchased from a raw material manufacturer, and then a graphite fine powder with the D50 less than or equal to 6 mu m is prepared by adopting an air flow mill for standby.
2) Accurately weighing 70 parts of graphite fine powder prepared in the step 1), 10 parts of superfine artificial stone toner, 10 parts of superfine modified green coke powder, 5 parts of N339 carbon black and N326 carbon black respectively, and 1 part of borate dispersant.
3) 200 parts of 1.
4) And (3) placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and milling for 1min, and preparing to obtain mixed fine powder.
5) Accurately weighing 25 parts of high-temperature asphalt (with a softening point of 112 ℃) and 15 parts of modified asphalt (with a softening point of 105 ℃) and weighing 5 parts of phthalate coupling agent.
6) Putting the mixed fine powder prepared in the step 4) into a kneading pot, mixing for 10min at 110 ℃, wherein the rotation speed of the kneading pot is 15r/min, and opening a cover to rotate positively; after the material temperature reaches 100 ℃, putting the slurry prepared in the step 3) into a kneading pot, kneading for 30min, wherein the rotation speed of the kneading pot is 25r/min, and opening the cover to rotate positively; after the water is completely removed, the temperature of the material is raised to 185 ℃, asphalt in a molten state is added into a kneading pot, a coupling agent is simultaneously added, kneading is carried out for 1h, the rotation speed of the kneading pot is 50r/min, forward rotation and reverse rotation are alternately carried out, and the kneading is carried out by closing a cover. After kneading, the paste obtained by kneading is quickly put into a flaking machine for flaking for 3 times, the flaking thickness is 1.5mm, the flaking temperature is 185 ℃, the rotating speed is 25r/min, after flaking, the flaky material is kept stand for 10h, then is crushed and ground, and is kept stand for 10h after being screened by a 200-mesh screen, so that the pressed powder is prepared.
7) Pressing the pressed powder prepared in the step 6) under 5MPa to prepare a primary blank block, carrying out vacuum packaging, and standing for 10 hours; placing in cold isostatic pressing equipment, pressing at 200MPa for 0.5h, performing gradient pressure relief, taking out the sample, removing the packaging bag, and standing for 10h to obtain the final product with density of 1.59g/cm 3 The green block of (1).
8) Placing the green body block prepared in the step 7) into a stainless steel crucible, filling the embedded burning material, adjusting the green body block to a proper position, placing the crucible into a roasting furnace, and introducing gas during the roasting processRoasting at 1200 deg.C for 4h under argon, cooling to 150 deg.C under program control, and naturally cooling to room temperature to obtain final product with density of 1.60g/cm 3 The fired block (carbon graphite material).
The fracture-resistant and compression-resistant diagram and the corresponding cross-sectional topography of the carbon graphite material prepared in this example are shown in fig. 1, where fig. 1 (a) and fig. 1 (c) are respectively a fracture-resistant strength diagram and a compression-resistant strength diagram of the carbon graphite material, and fig. 1 (b) and fig. 1 (d) are respectively cross-sectional micro-topography diagrams of the carbon graphite material. As can be seen from FIGS. 1 (a) and 1 (c), the flexural strength and compressive strength of the carbon graphite material were 79.69MPa and 235.77MPa, respectively. As can be seen from fig. 1 (b) and 1 (d), the structure between the aggregates is dense, the pore diameter between the particles is small, and no cracks are evident, so that the prepared carbon graphite material exhibits excellent breaking and compression strength.
The coefficient of friction curve of the carbon graphite material obtained in this example is shown in fig. 2 (a), and the load is 500 g. As can be seen from FIG. 2 (a), the carbon graphite material of this example gradually decreased the friction coefficient from 0.165 to 0.13 within 30min of the test at room temperature, the average friction coefficient was 0.1382, and the wear rate was 5.107X 10 after measuring the loss of wear quality -6 cm 3 /(N · m), frictional wear properties are good. As shown in fig. 2 (b), the surface scanning electron microscope image of the carbon graphite material obtained in this example showed that no communicating channels were formed between the pores, the pore diameter was about 10 μm, and the open porosity measured by the boiling method was 3.11%, which was good in airtightness.
Example 2
1) The calcined asphalt coke is purchased from a raw material manufacturer, and then a graphite fine powder with the D50 less than or equal to 6 mu m is prepared by adopting an air flow mill for standby.
2) Accurately weighing 72 parts of graphite fine powder prepared in the step 1), 8 parts of superfine artificial graphite powder, 10 parts of superfine modified green coke powder, 5 parts of N326 carbon black and mesocarbon microbeads respectively, and 1 part of borate ester dispersing agent.
3) Weighing 200 parts of 1.
4) And (3) placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and milling for 1min, and preparing to obtain mixed fine powder.
5) High temperature asphalt (softening point 112 ℃) 25 parts, modified asphalt (softening point 105 ℃) 20 parts and phthalate coupling agent 5 parts are accurately weighed.
6) Putting the mixed fine powder prepared in the step 4) into a kneading pot, mixing for 10min at 110 ℃, wherein the rotation speed of the kneading pot is 15r/min, and opening a cover to rotate positively; after the material temperature reaches 110 ℃, putting the slurry prepared in the step 3) into a kneading pot, kneading for 30min, wherein the rotation speed of the kneading pot is 25r/min, and opening the cover to rotate positively; after the water is completely removed, the temperature of the material is raised to 185 ℃, asphalt in a molten state is added into a kneading pot, a coupling agent is simultaneously added, kneading is carried out for 1h, the rotation speed of the kneading pot is 50r/min, forward rotation and reverse rotation are alternately carried out, and the kneading is carried out by closing a cover. After kneading is finished, the paste obtained by kneading is quickly put into a sheet rolling machine for rolling for 3 times, the thickness of the rolled sheet is 1.5mm, the temperature of the rolled sheet is 185 ℃, the rotating speed is 25r/min, after the rolling is finished, the sheet material is kept stand for 10h, then is crushed and ground, and after the sheet material passes through a 200-mesh screen, the sheet material is kept stand for 10h, so that the pressed powder is prepared.
7) Pressing the pressed powder prepared in the step 6) at 5MPa to prepare a primary blank block, carrying out vacuum packaging, and standing for 10 hours; placing in cold isostatic pressing equipment, pressing at 200MPa for 0.5h, performing gradient pressure relief, taking out the sample, removing the packaging bag, standing for 10h to obtain the product with density of 1.59g/cm 3 The green block of (1).
8) Placing the green body block prepared in the step 7) into a stainless steel crucible, filling the embedded burning material, adjusting the green body block to a proper position, placing the crucible into a roasting furnace, introducing argon gas in the roasting process, roasting at 1200 ℃ for 4 hours, cooling to 150 ℃ under program control, and naturally cooling to room temperature to obtain the green body block with the density of 1.61g/cm 3 The fired block (carbon graphite material) of (1).
The fracture-resistant and compression-resistant graph and the corresponding profile topography of the carbon graphite material prepared in this example are shown in fig. 3, where fig. 3 (a) and 3 (c) are respectively a fracture-resistant strength graph and a compression-resistant strength graph of the carbon graphite material, and fig. 3 (b) and 3 (d) are respectively a cross-sectional micro-topography graph of the carbon graphite material. As can be seen from FIGS. 3 (a) and 3 (c), the flexural strength and compressive strength of the graphite material were 82.46MPa and 240.91MPa, respectively. As can be seen from fig. 3 (b) and 3 (d), the structure between the aggregates is dense, the pore diameter between the particles is small, and no cracks are evident, so that the prepared carbon graphite material exhibits excellent breaking and compression strength.
The coefficient of friction curve of the graphite carbon material obtained in this example is shown in fig. 4 (a), and the load is 500 g. As shown in fig. 4 (a), the friction coefficient of the carbon graphite material obtained in this example is stabilized at about 0.15, the average friction coefficient thereof is 0.1580, and the wear rate calculated after measuring the loss of wear mass is 5.326 × 10 -6 cm 3 /(N.m), the frictional wear properties are good. As shown in fig. 4 (b), the surface scanning electron microscope image of the graphite material obtained in this example showed that no communicating channel was formed between the pores, the pore diameter was 10 μm or less, the open porosity was 2.85% as measured by the boiling method, and the air-tightness was good.
Example 3
1) The calcined pitch coke is purchased from a raw material factory, and then a graphite fine powder with the D50 less than or equal to 6 mu m is prepared by adopting an airflow mill for standby.
2) Accurately weighing 75 parts of graphite fine powder prepared in the step 1), 5 parts of superfine artificial graphite powder, 10 parts of superfine modified raw coke powder, 5 parts of modified carbon black and N339 carbon black respectively, and 1 part of borate dispersant.
3) Weighing 200 parts of 1.
4) And (3) placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and milling for 1min, and preparing to obtain mixed fine powder.
5) 20 parts of high-temperature asphalt (softening point 112 ℃) and 28 parts of modified asphalt (softening point 105 ℃) are accurately weighed, and 5 parts of phthalate coupling agent is weighed.
6) Putting the mixed fine powder prepared in the step 4) into a kneading pot, mixing for 10min at 110 ℃, wherein the rotation speed of the kneading pot is 15r/min, and opening a cover to rotate positively; after the material temperature reaches 105 ℃, putting the slurry prepared in the step 3) into a kneading pot, kneading for 30min, wherein the rotation speed of the kneading pot is 25r/min, and opening the cover to rotate positively; after the water is completely removed, the temperature of the material is raised to 185 ℃, asphalt in a molten state is added into a kneading pot, a coupling agent is simultaneously added, kneading is carried out for 1h, the rotation speed of the kneading pot is 50r/min, forward rotation and reverse rotation are alternately carried out, and the kneading is carried out by closing a cover. After kneading, the paste obtained by kneading is quickly put into a flaking machine for flaking for 3 times, the flaking thickness is 1.5mm, the flaking temperature is 185 ℃, the rotating speed is 25r/min, after flaking, the flaky material is kept stand for 10h, then is crushed and ground, and is kept stand for 10h after being screened by a 200-mesh screen, so that the pressed powder is prepared.
7) Pressing the pressed powder prepared in the step 6) under 5MPa to prepare a primary blank block, carrying out vacuum packaging, and standing for 10 hours; placing in cold isostatic pressing equipment, pressing at 200MPa for 0.5h, performing gradient pressure relief, taking out the sample, removing the packaging bag, standing for 10h to obtain the product with density of 1.61g/cm 3 The green block of (1).
8) Placing the green body block prepared in the step 7) into a stainless steel crucible, filling the embedded burning material, adjusting the green body block to a proper position, placing the crucible into a roasting furnace, introducing argon gas in the roasting process, roasting at 1200 ℃ for 4 hours, cooling to 150 ℃ under program control, and naturally cooling to room temperature to obtain the green body block with the density of 1.63g/cm 3 The fired block (carbon graphite material).
The fracture-resistant and compression-resistant diagram and the corresponding profile topography of the carbon graphite material prepared in this example are shown in fig. 5, fig. 5 (a) and 5 (c) are respectively a fracture-resistant strength and compression-resistant strength diagram of the carbon graphite material, and fig. 5 (b) and 5 (d) are respectively a cross-sectional micro-topography diagram of the carbon graphite material. As can be seen from fig. 5 (a) and 5 (c), the flexural strength and compressive strength of the carbon graphite material were 86.77MPa and 259.41MPa, respectively. As can be seen from fig. 5 (b) and 5 (d), the structure between the aggregates is dense, the pore diameter between the particles is small, and no cracks are evident, so that the prepared carbon graphite material exhibits excellent flexural strength and compressive strength.
The coefficient of friction curve of the graphite carbon material obtained in this example is shown in fig. 6 (a), and the load is 500 g. As can be seen from FIG. 6 (a), the carbon obtained in this example was tested at room temperature for a period of 30minThe friction coefficient of the graphite material is stabilized at about 0.12, the average friction coefficient is 0.1254, and the wear rate is calculated to be 4.929 multiplied by 10 after the wear quality loss is measured -6 cm 3 /(N.m), the frictional wear properties are good. As shown in fig. 6 (b), the surface scanning electron microscope image of the graphite material obtained in this example showed that no communicating channel was formed between the pores, the pore diameter was 10 μm or less, and the open porosity measured by the boiling method was 2.56%, and the air-tightness was good.
In summary, the raw material ratios adopted in examples 1 to 3 and the basic performance parameters of the prepared carbon graphite material are shown in table 1.
As can be seen from table 1: 1) The carbon graphite material prepared by the invention meets the following performance indexes of standard HB5366-86 carbon graphite sealing material for aviation: the breaking strength is more than or equal to 49MPa, the compressive strength is more than or equal to 118MPa, the Shore hardness is more than or equal to 60HS, the volume density is more than or equal to 1.60g/cm < 3 >, and the friction coefficient is less than or equal to 0.25. Compared with the M106 material mentioned in HB5366-86, the flexural strength and compressive strength of the carbon graphite material prepared by the invention are respectively improved by 1.62 times and 2 times.
2) From examples 1 to 3, it is found that the bulk density of the material is 1.6g/cm or more 3 Its flexural strength and compressive strength are excellent, and the high strength is attributed to the following 2 reasons: a. the superfine modified green coke powder and the carbon black have rich edge carbon atoms, high chemical activity and rich heteroatoms. The high chemical activity is beneficial to promoting the formation of sintering necks among the aggregate particles of the green body material, thereby promoting the self-sintering property, the self-bonding property and the mechanical property; abundant heteroatoms are beneficial to increasing the wettability of asphalt to aggregates and increasing the interface bonding force. b. The fine aggregate selected by the invention has large surface area and defects, is favorable for increasing the interface bonding force and endows the material with excellent mechanical properties.
Form homogeneity carbon skeleton (one-level skeleton texture) with the mode that different grain grades were piled up, form the solder joint consolidation between the granule to the pore UNICOM is blocked to similar sand hill leaking stoppage mode, for second grade welded structure, adopts the carbon black chain to seal + the mode of raw coke powder leaking stoppage simultaneously, further strengthens the inter-granule solder joint and combines, reduces the pore diameter, for tertiary protective structure, promotes independent non-intercommunication microporous structure's formation, thereby promotes homogeneity, stability, gas tightness, yield and mechanical strength of charcoal graphite material. The Shore hardness of the carbon graphite material prepared by the method is about 100HS, and the friction coefficient is about 0.12-0.15, which also shows that the wear resistance of the carbon graphite material can be effectively improved by introducing the superfine modified raw coke powder and the carbon black.
Table 1 raw material ratios adopted in examples 1 to 3 and basic performance parameters of carbon graphite materials prepared by the methods
| Example 1 | Example 2 | Example 3 | |
| Graphite powder/ |
70 | 72 | 75 |
| Superfine artificial graphite powder/ |
10 | 8 | 5 |
| Superfine modified raw coke powder/ |
10 | 10 | 10 |
| Carbon black per |
10 | 10 | 10 |
| Dispersant/part | 1 | 1 | 1 |
| Asphalt/ |
40 | 45 | 48 |
| Coupling agent/ |
5 | 5 | 5 |
| Compressive strength/MPa | 235.77 | 240.91 | 259.41 |
| Flexural strength/MPa | 79.69 | 82.46 | 86.77 |
| Shore hardness/HS | 99 | 101 | 105 |
| Bulk density/g/cm 3 | 1.60 | 1.61 | 1.63 |
| Resistivity/μ Ω · m | 33.42 | 34.19 | 30.14 |
| Coefficient of friction/. Mu. | 0.1382 | 0.1580 | 0.1254 |
Finally, it should be noted that the above-mentioned examples of the present invention are only examples for illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. It is not exhaustive here for all embodiments. Obvious changes and modifications of the present invention are also within the scope of the present invention.
Claims (10)
1. A preparation method of a low-density wear-resistant carbon graphite material with independent micropores is characterized by comprising the following steps:
s1: accurately weighing 60 to 80 parts of graphite fine powder, 1 to 10 parts of superfine artificial graphite powder, 1 to 10 parts of superfine modified green coke powder, 1 to 10 parts of carbon black, 1 to 2 parts of dispersing agent, 40 to 50 parts of asphalt, 1 to 5 parts of coupling agent and 100 to 250 parts of ethanol-acetone mixed solution for later use; the volume ratio of ethanol to acetone in the ethanol-acetone mixed solution is 1 to 1;
s2: adding a dispersing agent into the ethanol-acetone mixed solution, uniformly stirring, and then sequentially adding superfine artificial graphite powder and carbon black for ultrasonic dispersion to obtain mixed slurry;
s3: placing the fine graphite powder and the superfine modified raw coke powder into a Raymond mill, mixing and grinding for 1 to 10min to obtain mixed fine powder;
s4: and putting the mixed fine powder and the mixed slurry into a kneading pot for kneading, when the temperature of the material rises to 180-200 ℃, putting a coupling agent and molten asphalt into the kneading pot, then closing a cover for kneading, after kneading, rolling, crushing, grinding and sieving to prepare pressing powder, then pressing and molding to obtain a green block, and finally roasting to obtain the carbon graphite material.
2. The method for preparing the low-density wear-resistant carbon graphite material with the independent micropores according to claim 1, wherein D50 of the graphite fine powder is less than or equal to 6 microns, and the low-density wear-resistant carbon graphite material is prepared by using forged pitch coke or forged needle coke as a raw material and adopting a jet mill.
3. The method for preparing the low-density wear-resistant carbon graphite material with the independent micropores according to the claim 1, wherein the carbon black is one or two of N220 carbon black, N326 carbon black, N330 carbon black, N339 carbon black, modified carbon black and mesocarbon microbeads; the asphalt is one or two of low-temperature asphalt, medium-temperature asphalt, high-temperature asphalt and modified asphalt.
4. The method for preparing the low-density wear-resistant carbon graphite material with the independent micropores according to the claim 1, wherein the dispersant is one or two of borate, aminopropylamine dioleate and carboxymethyl cellulose; the coupling agent is one or two of aluminate, phthalate ester and dioxy-acetyl phthalate ester.
5. The preparation method of the low-density wear-resistant carbon graphite material with the independent micropores according to claim 1, wherein when the mixed slurry is prepared, the superfine artificial graphite powder is added into a mixed solution of a dispersing agent and ethanol for ultrasonic dispersion for 10 to 30min, and then the carbon powder is added for ultrasonic dispersion for 10 to 30min.
6. The preparation method of the low-density wear-resistant carbon graphite material with the independent micropores is characterized in that when kneading, the mixed fine powder is firstly put into a kneading pot and mixed for 10 to 20min at the temperature of 100 to 110 ℃, the rotation speed of the kneading pot is 10 to 50r/min, and a cover is opened and the carbon graphite material is rotated forwards; after the temperature of the materials reaches 100 to 110 ℃, putting the mixed slurry into a kneading pot, kneading for 0.5 to 1h, wherein the rotation speed of the kneading pot is 10 to 50r/min, and opening the cover to rotate positively; after the water is completely removed, heating the materials to 180-200 ℃, putting molten asphalt into a kneading pot, putting a coupling agent into the kneading pot at the same time, wherein the rotation speed of the kneading pot is 10-50 r/min, rotating forward and backward alternately, and closing the cover to knead for 0.5-1 h.
7. The preparation method of the low-density wear-resistant carbon graphite material with the independent micropores is characterized in that when the pressed powder is prepared, the paste obtained by kneading is rapidly put into a sheet mill for 3 to 4 times, the thickness of the rolled sheet is 1 to 2.5mm, the temperature of the rolled sheet is 180 to 200 ℃, the rotating speed is 10 to 25r/min, the sheet-shaped material is kept still for 5 to 10 hours after the rolling is finished, and then the crushed and ground powder is passed through a screen with 100 to 400 meshes and kept still for 5 to 10 hours, so that the pressed powder is prepared.
8. The method for preparing the low-density wear-resistant carbon graphite material with the independent micropores as claimed in claim 1, wherein the step of preparing the green block body by the pressed powder comprises the following steps: pressing the powder under 1 to 10MPa to prepare a blank block, carrying out vacuum packaging, and standing for 5 to 10 hours; placing the mixture in a cold isostatic pressing device, pressing the mixture for 0.5 to 1 hour under the pressure of 150 to 200MPa, performing gradient pressure relief, taking out the mixture, removing a packaging bag, and standing the mixture for 5 to 10 hours to obtain the material with the density of 1.59 to 1.62g/cm 3 The green block of (1).
9. The method for preparing the low-density wear-resistant carbon graphite material with the independent micropores as claimed in claim 1, wherein the roasting process comprises: placing the green block body in a stainless steel crucible, filling the green block body into a buried sintering material, then placing the crucible in a roasting furnace, introducing argon, roasting for 2-4 h at 900-1200 ℃, cooling to 150-300 ℃ under program control, and naturally cooling to room temperature to obtain the green block body with the volume density of 1.60-1.64 g/cm 3 The roasted block is the carbon graphite material.
10. A low-density wear-resistant carbon graphite material with independent micropores is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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