CN114014660A - Preparation method of high-performance wear-resistant material added with sulfonated graphene - Google Patents

Preparation method of high-performance wear-resistant material added with sulfonated graphene Download PDF

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CN114014660A
CN114014660A CN202011518620.6A CN202011518620A CN114014660A CN 114014660 A CN114014660 A CN 114014660A CN 202011518620 A CN202011518620 A CN 202011518620A CN 114014660 A CN114014660 A CN 114014660A
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sulfonated graphene
asphalt
wear
roasting
resistant material
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董直强
梁世林
殷景峰
马庆春
刘文峰
王雨晨
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Harbin Electric Carbon Plant Co ltd
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Harbin Electric Carbon Plant Co ltd
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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
    • 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
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00—Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/425—Graphite
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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
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention discloses a preparation method of a high-performance wear-resistant material added with sulfonated graphene, belonging to the technical field of inorganic non-metallic graphite sealing materials. The invention solves the problems that the existing graphite sealing ring has complex preparation process and the performance of the wear-resistant material can not meet the more rigorous use requirement. The invention takes micro powder (the granularity is less than or equal to 10 mu) as a main raw material, adopts sulfonated graphene solution with the concentration of 10 percent as an additive, improves the hardness and graphitization degree of a graphite matrix, greatly improves the strength of a graphite product, and meets the more rigorous use requirement of the existing graphite high-performance wear-resistant material.

Description

Preparation method of high-performance wear-resistant material added with sulfonated graphene
Technical Field
The invention relates to a preparation method of a high-performance wear-resistant material added with sulfonated graphene, belonging to the technical field of inorganic non-metallic graphite sealing materials.
Background
The fuel pump is the most basic component of the fuel supply system of the engine, and is used for extracting fuel from a fuel tank during the operation of the engine, continuously delivering the fuel to the engine through a fuel supply pipeline at a certain pressure, secondarily pressurizing the fuel by the high-pressure fuel pump, and supplying a fixed amount of fuel to each cylinder according to the operation sequence of the engine. The mechanical seal graphite sealing ring is arranged in the conventional fuel pump, but the problems of overproof mechanical seal oil leakage and white smoke emission can also occur in the working process of the mechanical seal graphite sealing ring. The existing mechanical sealing graphite sealing ring is generally made of graphite impregnating resin, when the temperature rise exceeds 200 ℃, the impregnating resin graphite sealing ring can be decomposed to form hard particles and separate out volatile matters to form blisters, when the sealing end face line speed is high, the PV value of the sealing end face of the friction pair is increased, the sealing section is damaged, the abrasion is aggravated, and the leakage amount exceeds the standard. Therefore, it is necessary to provide a method for preparing a material capable of improving the wear resistance of the graphite sealing material.
Disclosure of Invention
The invention provides a preparation method of a high-performance wear-resistant material added with sulfonated graphene, aiming at solving the problems that the existing graphite sealing ring preparation process is complex and the performance of the wear-resistant material cannot meet the more rigorous use requirement.
A preparation method of a high-performance wear-resistant material added with sulfonated graphene comprises the following steps:
step 1, fully and uniformly mixing the superfine coke powder, the graphite powder and the sulfonated graphene solution to obtain a mixture, adding asphalt into the mixture for the first time, carrying out kneading treatment for 2 hours at the temperature of 100-plus-material 180 ℃, then adding the asphalt for the second time, continuing the kneading treatment for 2 hours at the temperature of 100-plus-material 180 ℃, and cooling to obtain a material;
step 2, crushing and grinding the material obtained in the step 1 to obtain pressed powder with the particle size of below 70 microns, and performing isostatic pressing on the pressed powder to obtain a blank;
step 3, mixingSequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the blank obtained in the step 2 to obtain a product with the density of more than 1.90g/cm3The Shore hardness is 70-90, and the graphitization degree is more than 60%.
Further, the mass concentration of the sulfonated graphene in the sulfonated graphene solution in the step 1 is 10%.
Furthermore, in the step 1, the superfine coke powder and the graphite powder are mixed according to the proportion that the content of the superfine coke powder is 80-90 wt% and the content of the graphite powder is 10-20 wt%, and then sulfonated graphene solution with the total mass of the superfine coke powder and the graphite powder being 5-15% is added and fully mixed to obtain a mixture.
Furthermore, the grain diameter of the superfine coke powder in the step 1 is less than 10 μm, and the grain diameter of the graphite powder is less than 45 μm.
Further, in the step 1, the mass of the asphalt added for the first time is 30-40% of the total mass of the mixture, and the mass of the asphalt added for the second time is 20-30% of the total mass of the mixture.
Further, in the step 1, the softening point of the asphalt is 70-100 ℃, and the carbon residue rate is 30-50 wt%.
Further, the isostatic compaction processing pressure in step 2 is 100-200 MPa.
Further, the first roasting, the second roasting and the third roasting treatment conditions are as follows: heating to 1300 ℃ at the heating rate of 10-15 ℃/h, and keeping the temperature for 2 h.
Further, the conditions of the first asphalt impregnation and the second asphalt impregnation in the step 3 are as follows: dipping for 5-20h by using asphalt as a dipping agent under the conditions that the temperature is 150-300 ℃ and the pressure is 1-3 MPa.
Further, the graphitization treatment conditions in step 3 are as follows: the graphitization temperature is 2300-2500 ℃, and the heat preservation is carried out for 4 h.
The invention has the following beneficial effects: the invention takes micro powder (the granularity is less than or equal to 10 mu) as a main raw material, adopts sulfonated graphene solution with the concentration of 10 percent as an additive, improves the hardness and graphitization degree of a graphite matrix, greatly improves the strength of a graphite product, and meets the more rigorous use requirement of the existing graphite high-performance wear-resistant material. And the roasting process provided by the application is beneficial to improving the yield.
Drawings
Fig. 1 is a flow chart of a preparation process of a high-performance wear-resistant material added with sulfonated graphene.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
as shown in fig. 1, firstly, the superfine coke powder with the particle size of less than 10 μ and the graphite powder with the particle size of less than 50 μ are mixed according to the content of 80 wt% of the superfine coke powder and 20 wt% of the graphite powder, and then the sulfonated graphene solution with the total amount of 10% of the superfine coke powder and the graphite powder is added and fully mixed to obtain a mixture, wherein the mass concentration of the sulfonated graphene in the sulfonated graphene solution is 10%. And then adding asphalt with the softening point of 93 ℃ and the carbon residue rate of 40 wt% into the mixture, wherein the adding amount of the asphalt is 30 wt% of the total amount of the mixture, kneading the mixture at the temperature of 180 ℃ for 2h, adding the asphalt with the weight percentage of 30 wt% of the total amount of the mixture again, kneading the mixture again at the temperature of 180 ℃ for 2h, and cooling the mixture after the kneading is finished.
Crushing and grinding the cooled mixture until the particle size is below 70 mu to prepare the pressed powder, and then pressing the pressed powder under the conditions of 100-200MPa and 200MPa to obtain the blank.
Sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the obtained blank to obtain the product with the density of 1.90g/cm3Shore hardness 72, degree of graphitization 60%.
Wherein, the first roasting, the second roasting and the third roasting treatment conditions are as follows: heating to 1300 ℃ at the heating rate of 15 ℃/h, and keeping the temperature for 2 h. The first asphalt impregnation and the second asphalt impregnation treatment conditions are as follows: impregnating for 20h by using asphalt as an impregnant under the conditions that the temperature is 300 ℃ and the pressure is 3 MPa. The graphitization temperature is 2500 ℃, and the heat preservation is carried out for 4 h.
Example 2:
as shown in fig. 1, firstly, the superfine coke powder with the particle size of less than 10 μ and the graphite powder with the particle size of less than 50 μ are mixed according to the content of 80 wt% of the superfine coke powder and 20 wt% of the graphite powder, and then the sulfonated graphene solution with the total amount of 10% of the superfine coke powder and the graphite powder is added and fully mixed to obtain a mixture, wherein the mass concentration of the sulfonated graphene in the sulfonated graphene solution is 10%. And then adding asphalt with the softening point of 93 ℃ and the carbon residue rate of 40 wt% into the mixture, wherein the adding amount of the asphalt is 35 wt% of the total amount of the mixture, kneading the mixture at the temperature of 150 ℃ for 2h, adding the asphalt with the weight percent of 25 wt% of the total amount of the mixture again, kneading the mixture again at the temperature of 150 ℃ for 2h, and cooling the mixture after the kneading is finished.
Crushing and grinding the cooled mixture until the particle size is below 70 mu to prepare the pressed powder, and then pressing the pressed powder under the conditions of 100-200MPa and 200MPa to obtain the blank.
Sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the obtained blank to obtain the product with the density of 1.92g/cm3Shore hardness 78, degree of graphitization 61%.
Wherein, the first roasting, the second roasting and the third roasting treatment conditions are as follows: heating to 1300 ℃ at the heating rate of 15 ℃/h, and keeping the temperature for 2 h. The first asphalt impregnation and the second asphalt impregnation treatment conditions are as follows: impregnating for 10h by using asphalt as an impregnant under the conditions that the temperature is 200 ℃ and the pressure is 2 MPa. The graphitization temperature is 2400 ℃, and the heat preservation is carried out for 4 hours.
Example 3:
as shown in fig. 1, firstly, the superfine coke powder with the particle size of less than 10 μ and the graphite powder with the particle size of less than 50 μ are mixed according to the content of 80 wt% of the superfine coke powder and 20 wt% of the graphite powder, and then the sulfonated graphene solution with the total amount of 10% of the superfine coke powder and the graphite powder is added and fully mixed to obtain a mixture, wherein the mass concentration of the sulfonated graphene in the sulfonated graphene solution is 10%. And then adding asphalt with the softening point of 93 ℃ and the carbon residue rate of 40 wt% into the mixture, wherein the adding amount of the asphalt is 40 wt% of the total amount of the mixture, kneading for 2h at the temperature of 120 ℃, adding the asphalt with the weight percent of 20 wt% of the total amount of the mixture again, kneading for 2h at the temperature of 120 ℃, and cooling after the kneading is finished.
Crushing and grinding the cooled mixture until the particle size is below 70 mu to prepare the pressed powder, and then pressing the pressed powder under the conditions of 100-200MPa and 150MPa to obtain the blank.
Sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the obtained blank to obtain the product with the density of 1.91g/cm3Shore hardness 75, degree of graphitization 60%.
Wherein, the first roasting, the second roasting and the third roasting treatment conditions are as follows: heating to 1300 ℃ at the heating rate of 10 ℃/h, and keeping the temperature for 2 h. The first asphalt impregnation and the second asphalt impregnation treatment conditions are as follows: impregnating for 5h by using asphalt as an impregnant under the conditions that the temperature is 150 ℃ and the pressure is 1 MPa. The graphitization temperature is 2300 ℃, and the heat preservation is carried out for 4 hours.

Claims (10)

1. A preparation method of a high-performance wear-resistant material added with sulfonated graphene is characterized by comprising the following steps:
step 1, fully and uniformly mixing the superfine coke powder, the graphite powder and the sulfonated graphene solution to obtain a mixture, adding asphalt into the mixture for the first time, carrying out kneading treatment for 2 hours at the temperature of 100-plus-material 180 ℃, then adding the asphalt for the second time, continuing the kneading treatment for 2 hours at the temperature of 100-plus-material 180 ℃, and cooling to obtain a material;
step 2, crushing and grinding the material obtained in the step 1 to obtain pressed powder with the particle size of below 70 microns, and performing isostatic pressing on the pressed powder to obtain a blank;
step 3, sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the blank obtained in the step 2 to obtain the product with the density of more than 1.90g/cm3The Shore hardness is 70-90, and the graphitization degree is more than 60%.
2. The method for preparing the high-performance wear-resistant material added with the sulfonated graphene according to claim 1, wherein the mass concentration of the sulfonated graphene in the sulfonated graphene solution in the step 1 is 10%.
3. The preparation method of the sulfonated graphene-added high-performance wear-resistant material according to claim 2, wherein in the step 1, the mixture is prepared by mixing the superfine coke powder with the graphite powder with the content of 80-90 wt%, and adding the sulfonated graphene solution with the total mass of the superfine coke powder and the graphite powder of 5-15%, and fully and uniformly mixing.
4. The method for preparing the high-performance wear-resistant material added with the sulfonated graphene according to claim 1, 2 or 3, wherein the particle size of the superfine coke powder in the step 1 is less than 10 μm, and the particle size of the graphite powder is less than 45 μm.
5. The preparation method of the high-performance anti-wear material added with the sulfonated graphene according to claim 1, wherein the mass of the asphalt added for the first time in the step 1 is 30-40% of the total mass of the mixture, and the mass of the asphalt added for the second time is 20-30% of the total mass of the mixture.
6. The method for preparing the high-performance anti-wear material added with the sulfonated graphene according to claim 1, wherein the asphalt softening point in step 1 is 70-100 ℃, and the carbon residue rate is 30-50 wt%.
7. The method as claimed in claim 1, wherein the isostatic compaction pressure in step 2 is 100-200 MPa.
8. The method for preparing the high-performance wear-resistant material added with the sulfonated graphene according to claim 1, wherein the first roasting, the second roasting and the third roasting treatment conditions are as follows: heating to 1300 ℃ at the heating rate of 10-15 ℃/h, and keeping the temperature for 2 h.
9. The method for preparing the high-performance anti-wear material added with the sulfonated graphene according to claim 1, wherein the first asphalt impregnation and the second asphalt impregnation in step 3 are carried out under the following conditions: dipping for 5-20h by using asphalt as a dipping agent under the conditions that the temperature is 150-300 ℃ and the pressure is 1-3 MPa.
10. The method for preparing the high-performance wear-resistant material added with the sulfonated graphene according to claim 1, wherein the graphitization treatment conditions in the step 3 are as follows: the graphitization temperature is 2300-2500 ℃, and the heat preservation is carried out for 4 h.
CN202011518620.6A 2020-12-21 2020-12-21 Preparation method of high-performance wear-resistant material added with sulfonated graphene Pending CN114014660A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105948014A (en) * 2016-04-27 2016-09-21 山东前昊炭素有限公司 Coke/sulfonated graphene carbon-graphite material for sealing piece and preparation method thereof
CN106673657A (en) * 2016-12-30 2017-05-17 苏州高通新材料科技有限公司 Special carbon material and production method thereof
WO2017084608A1 (en) * 2015-11-17 2017-05-26 苏州聚宜工坊信息科技有限公司 Heating membrane assembly for use in wearable device and a garment
CN109133926A (en) * 2018-08-28 2019-01-04 大同新成新材料股份有限公司 A kind of sealed graphite and preparation method thereof
CN109627513A (en) * 2018-12-24 2019-04-16 苏州圣瑞赛新材料科技有限公司 High abrasion high-barrier heat conductive rubber, preparation method and application
US20200223699A1 (en) * 2017-04-28 2020-07-16 Hangzhou Gaox1 Technology Co., Ltd. Paper ball-like graphene microsphere, composite material thereof, and preparation method therefor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017084608A1 (en) * 2015-11-17 2017-05-26 苏州聚宜工坊信息科技有限公司 Heating membrane assembly for use in wearable device and a garment
CN105948014A (en) * 2016-04-27 2016-09-21 山东前昊炭素有限公司 Coke/sulfonated graphene carbon-graphite material for sealing piece and preparation method thereof
CN106673657A (en) * 2016-12-30 2017-05-17 苏州高通新材料科技有限公司 Special carbon material and production method thereof
US20200223699A1 (en) * 2017-04-28 2020-07-16 Hangzhou Gaox1 Technology Co., Ltd. Paper ball-like graphene microsphere, composite material thereof, and preparation method therefor
CN109133926A (en) * 2018-08-28 2019-01-04 大同新成新材料股份有限公司 A kind of sealed graphite and preparation method thereof
CN109627513A (en) * 2018-12-24 2019-04-16 苏州圣瑞赛新材料科技有限公司 High abrasion high-barrier heat conductive rubber, preparation method and application

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