CN114014658A - Preparation method of oxidation-resistant graphite material matrix - Google Patents

Preparation method of oxidation-resistant graphite material matrix Download PDF

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CN114014658A
CN114014658A CN202011518698.8A CN202011518698A CN114014658A CN 114014658 A CN114014658 A CN 114014658A CN 202011518698 A CN202011518698 A CN 202011518698A CN 114014658 A CN114014658 A CN 114014658A
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oxidation
temperature
powder
preparing
graphite material
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马庆春
张锐
曲春浴
王雨晨
贾目跃
姜浩
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Harbin Electric Carbon Plant Co ltd
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Harbin Electric Carbon Plant Co ltd
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    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a preparation method of an antioxidant graphite material matrix, and belongs to the technical field of inorganic non-metallic graphite sealing materials. The invention solves the problems of complex preparation process and low oxidation resistance of the conventional graphite sealing ring. The graphite matrix is prepared by taking graphitized carbon black as a main raw material and superfine petroleum coke powder and boric acid as auxiliary materials, two-stage production is adopted, the oxidation resistance of the graphite matrix is greatly improved, the microstructure of the material is improved by isostatic pressing, oxidation factors are reduced, and the obtained graphite matrix has high volume density, high graphitization degree and high oxidation resistance.

Description

Preparation method of oxidation-resistant graphite material matrix
Technical Field
The invention relates to a preparation method of an antioxidant graphite material matrix, 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 graphite sealing ring is generally prepared by 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 surface line speed is higher, the PV value of the sealing end surface of the friction pair is increased, the sealing section is damaged, the abrasion is intensified, and the leakage amount exceeds the standard. Therefore, the high temperature resistance of the graphite sealing ring has a serious influence on the service life of the graphite sealing ring, and therefore, the preparation method of the oxidation-resistant graphite material substrate is necessary.
Disclosure of Invention
The invention provides a preparation method of an antioxidant graphite material substrate, aiming at solving the problems of complex preparation process and low oxidation resistance of the existing graphite sealing ring.
A preparation method of an oxidation-resistant graphite material matrix comprises the following steps:
step 1, preparing ultrafine powder at one stage:
step 2, uniformly mixing the stage ultrafine powder, the soil-like graphite powder, the ultrafine petroleum coke powder, the high wear-resistant carbon black and boric acid obtained in the step 1 to obtain a mixture, adding asphalt into the mixture, and kneading the mixture for 2 to 3 hours at the temperature of 100 ℃ and 180 ℃;
step 3, after the kneading treatment is finished, carrying out sheet rolling treatment at the temperature of 130-150 ℃, wherein the thickness of the obtained rolled sheet is less than 1 mm;
step 4, cooling the rolled sheet obtained in the step 3, then carrying out crushing and grinding treatment to obtain pressed powder with the particle size of below 70 microns, and carrying out isostatic pressing treatment on the pressed powder to obtain a blank;
step 5, the step4, sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the blank to obtain a product, wherein the density of the product is more than 1.90g/cm3Shore hardness of 60-80, and graphitization degree greater than 85%.
Further, the specific operation process of step 1 is as follows: mixing high-wear-resistance carbon black and medium-temperature asphalt according to the mass ratio of 1:1 at the temperature of 150-.
Further, the graphitization treatment conditions in step 1 are as follows: the temperature is 2300-2500 ℃, and the temperature is kept for 4 h.
Further, in the step 2, mixing the materials according to the proportion that the content of the superfine powder is 50-60 wt%, the content of the earthy graphite powder is 5-15 wt%, the content of the superfine petroleum coke powder is 10-25 wt%, the content of the high wear-resistant carbon black is 5-10 wt% and the content of the boric acid is 5-10 wt%; the particle size of the earthy graphite powder is less than 20 microns, the particle size of the superfine petroleum coke powder is less than 10 microns, and the particle size of the high-wear-resistance carbon black is 1-3 microns.
Further, in the step 2, the softening point of the asphalt is 70-100 ℃, and the carbon residue rate is 30-50 wt%.
Further, the adding mass of the asphalt in the step 2 is 60-80% of the total mass of the mixture.
Further, the isostatic compaction processing pressure in step 4 is 150-.
Further, the conditions of the first roasting, the second roasting and the third roasting in the step 5 are as follows: heating to 1300 ℃ at the heating rate of 5-10 ℃/h, and keeping the temperature for 2 h.
Further, the conditions of the first asphalt impregnation and the second asphalt impregnation in the step 5 are as follows: the asphalt is used as impregnant for impregnation treatment for 20 hours at the temperature of 180-250 ℃ and the pressure of 2-3 MPa.
Further, the graphitization treatment conditions in step 5 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 method takes graphitized carbon black as a main raw material, takes superfine petroleum coke powder and boric acid as auxiliary materials, adopts two-stage production, greatly improves the oxidation resistance of the graphite matrix, improves the microstructure of the material by isostatic pressing, improves the density, reduces oxidation factors, and obtains the graphite matrix with high volume density, high graphitization degree and high oxidation resistance.
Drawings
FIG. 1 is a flow chart of a process for preparing a one-stage ultrafine powder;
FIG. 2 is a flow chart of a preparation process of an oxidation-resistant graphite material matrix.
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, one-stage ultra-fine powder is prepared:
firstly, mixing high-wear-resistance carbon black and medium-temperature asphalt according to the mass ratio of 1:1 at the temperature of 150 ℃, then performing compression molding on the mixture into a cylinder under the conditions of the temperature of 150 ℃ and the pressure of 40MPa, then heating the cylinder to 800 ℃ at the heating rate of 20 ℃/h, preserving the temperature for 2h, preserving the temperature for 4h at 2500 ℃ to complete graphitization treatment, and finally grinding the cylinder into one-stage ultrafine powder with the particle size diameter of less than 5 mu m.
As shown in fig. 2, preparing an oxidation-resistant graphite material matrix:
(1) fully and uniformly mixing 55 wt% of coke powder, 5 wt% of earthy graphite powder, 30 wt% of superfine petroleum coke powder, 5 wt% of high-wear-resistant carbon black and 5 wt% of boric acid in one stage to obtain a mixture.
(2) Adding asphalt with the softening point of 75 ℃ and the carbon residue rate of 35 wt% into the mixture, wherein the adding amount of the asphalt is 60% of the total mass of the mixture, kneading the mixture for 2h at the temperature of 180 ℃, rolling the mixture into sheets at the temperature of 150 ℃, wherein the thickness of the rolled sheets is less than 1mm, cooling the rolled sheets, crushing and grinding the sheets into powder with the particle size of less than 70 mu, and preparing the pressed powder. And carrying out isostatic pressing treatment on the pressed powder at 200MPa to obtain a blank.
(3) Sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the obtained blank to obtain a product with the density of 1.85g/cm3Shore hardness 65, graphitization degree 75%.
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 25h by using asphalt as an impregnant under the conditions that the temperature is 250 ℃ 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, one-stage ultra-fine powder is prepared:
firstly, mixing high-wear-resistance carbon black and medium-temperature asphalt according to the mass ratio of 1:1 at the temperature of 160 ℃, then performing compression molding on the mixture into a cylinder under the conditions of the temperature of 140 ℃ and the pressure of 40MPa, then heating the cylinder to 800 ℃ at the heating rate of 30 ℃/h, preserving the temperature for 2h, preserving the temperature for 4h at 2500 ℃ to complete graphitization treatment, and finally grinding the cylinder into one-stage ultrafine powder with the particle size diameter of less than 5 mu m.
As shown in fig. 2, preparing an oxidation-resistant graphite material matrix:
(1) fully and uniformly mixing 60 wt% of coke powder, 10 wt% of earthy graphite powder, 15 wt% of superfine petroleum coke powder, 10 wt% of high-wear-resistant carbon black and 5 wt% of boric acid to obtain a mixture.
(2) Then adding asphalt with the softening point of 80 ℃ and the carbon residue rate of 40 wt% into the mixture, wherein the adding amount of the asphalt is 70% of the total mass of the mixture, kneading the mixture for 2h at the temperature of 150 ℃, then rolling the mixture into sheets at the temperature of 150 ℃, wherein the thickness of the rolled sheets is less than 1mm, cooling the rolled sheets, crushing and grinding the sheets into powder with the particle size of less than 70 mu, and preparing the pressed powder. And carrying out isostatic pressing treatment on the pressed powder at 200MPa to obtain a blank.
(3) Sequentially carrying out primary roasting, primary asphalt impregnation, secondary roasting, secondary asphalt impregnation, tertiary roasting and graphitization treatment on the obtained blank to obtain a product with the density of 1.87g/cm3Shore hardness 70, graphitization degree 80%.
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 20h 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, one-stage ultra-fine powder is prepared:
firstly, mixing high-wear-resistance carbon black and medium-temperature asphalt according to the mass ratio of 1:1 at the temperature of 180 ℃, then performing compression molding on the mixture into a cylinder under the conditions of the temperature of 140 ℃ and the pressure of 30MPa, then heating the cylinder to 800 ℃ at the heating rate of 25 ℃/h, preserving the temperature for 2h, preserving the temperature for 4h at 2300 ℃ to complete graphitization treatment, and finally grinding the cylinder into one-stage ultrafine powder with the particle size diameter of less than 5 microns.
As shown in fig. 2, preparing an oxidation-resistant graphite material matrix:
(1) fully and uniformly mixing 60 wt% of coke powder, 15 wt% of earthy graphite powder, 10 wt% of superfine petroleum coke powder, 10 wt% of high-wear-resistant carbon black and 5 wt% of boric acid to obtain a mixture.
(2) Then adding asphalt with the softening point of 100 ℃ and the carbon residue rate of 50 wt% into the mixture, wherein the adding amount of the asphalt is 80% of the total mass of the mixture, kneading the mixture for 3h at the temperature of 120 ℃, then rolling the mixture into sheets at the temperature of 150 ℃, wherein the thickness of the rolled sheets is less than 1mm, cooling the rolled sheets, crushing and grinding the sheets into powder with the particle size of less than 70 mu, and preparing the pressed powder. And carrying out isostatic pressing treatment on the pressed powder at 150MPa to obtain a blank.
(3) Sequentially roasting the obtained blank for the first time, impregnating the obtained blank with asphalt for the first time, roasting the obtained blank for the second time, impregnating the obtained blank with asphalt for the second time, roasting the obtained blank for the third time and grinding the obtained blankThe product is obtained by the inking treatment, and the density of the product is 1.90g/cm3Shore hardness 75, graphitization degree 85%.
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 20 hours by using asphalt as an impregnant under the conditions that the temperature is 180 ℃ and the pressure is 3 MPa. The graphitization temperature is 2400 ℃, and the heat preservation is carried out for 4 hours.

Claims (10)

1. The preparation method of the oxidation-resistant graphite material matrix is characterized by comprising the following steps of:
step 1, preparing ultrafine powder at one stage:
step 2, uniformly mixing the stage ultrafine powder, the soil-like graphite powder, the ultrafine petroleum coke powder, the high wear-resistant carbon black and boric acid obtained in the step 1 to obtain a mixture, adding asphalt into the mixture, and kneading the mixture for 2 to 3 hours at the temperature of 100 ℃ and 180 ℃;
step 3, after the kneading treatment is finished, carrying out sheet rolling treatment at the temperature of 130-150 ℃, wherein the thickness of the obtained rolled sheet is less than 1 mm;
step 4, cooling the rolled sheet obtained in the step 3, then carrying out crushing and grinding treatment to obtain pressed powder with the particle size of below 70 microns, and carrying out isostatic pressing treatment on the pressed powder to obtain a blank;
and 5, 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 4 to obtain the product.
2. The method for preparing the oxidation-resistant graphite material matrix according to claim 1, wherein the specific operation process of the step 1 is as follows: mixing high-wear-resistance carbon black and medium-temperature asphalt according to the mass ratio of 1:1 at the temperature of 150-.
3. The method for preparing the oxidation-resistant graphite material substrate according to claim 2, wherein the graphitization treatment conditions in the step 1 are as follows: the temperature is 2300-2500 ℃, and the temperature is kept for 4 h.
4. The method for preparing an oxidation-resistant graphite material substrate according to claim 1, wherein the step 2 comprises mixing the raw materials in a ratio of 50-60 wt% of ultrafine powder, 5-15 wt% of earthy graphite powder, 10-25 wt% of ultrafine petroleum coke powder, 5-10 wt% of highly wear-resistant carbon black and 5-10 wt% of boric acid in one stage; the particle size of the earthy graphite powder is less than 20 microns, the particle size of the superfine petroleum coke powder is less than 10 microns, and the particle size of the high-wear-resistance carbon black is 1-3 microns.
5. The method for preparing the oxidation-resistant graphite material substrate according to claim 1, wherein the pitch softening point in the step 2 is 70-100 ℃ and the carbon residue rate is 30-50 wt%.
6. The method for preparing the oxidation-resistant graphite material matrix according to claim 1 or 5, wherein the asphalt is added in the step 2 in an amount of 60-80% of the total mass of the mixture.
7. The method for preparing the oxidation-resistant graphite material substrate as claimed in claim 1, wherein the isostatic compaction treatment pressure in step 4 is 150-200 MPa.
8. The method for preparing the oxidation-resistant graphite material matrix according to claim 1, wherein the first roasting, the second roasting and the third roasting in the step 5 are carried out under the following conditions: heating to 1300 ℃ at the heating rate of 5-10 ℃/h, and keeping the temperature for 2 h.
9. The method for preparing the oxidation-resistant graphite material matrix according to claim 1, wherein the first pitch impregnation and the second pitch impregnation in the step 5 are carried out under the following conditions: the asphalt is used as impregnant for impregnation treatment for 20 hours at the temperature of 180-250 ℃ and the pressure of 2-3 MPa.
10. The method for preparing the oxidation-resistant graphite material substrate according to claim 1, wherein the graphitization treatment in the step 5 is performed under the following conditions: the graphitization temperature is 2300-2500 ℃, and the heat preservation is carried out for 4 h.
CN202011518698.8A 2020-12-21 2020-12-21 Preparation method of oxidation-resistant graphite material matrix Pending CN114014658A (en)

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Cited By (3)

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CN114824989A (en) * 2022-03-09 2022-07-29 哈尔滨电碳厂有限责任公司 Preparation method of high-wear-resistance metal graphite electric brush
CN114804876A (en) * 2022-03-09 2022-07-29 哈尔滨电碳厂有限责任公司 Preparation method of high-wear-resistance end face sealing graphite material
CN115124344A (en) * 2022-03-09 2022-09-30 哈尔滨电碳厂有限责任公司 Preparation method of ablation-resistant oxidation-resistant carbon-ceramic composite material matrix

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CN114824989A (en) * 2022-03-09 2022-07-29 哈尔滨电碳厂有限责任公司 Preparation method of high-wear-resistance metal graphite electric brush
CN114804876A (en) * 2022-03-09 2022-07-29 哈尔滨电碳厂有限责任公司 Preparation method of high-wear-resistance end face sealing graphite material
CN115124344A (en) * 2022-03-09 2022-09-30 哈尔滨电碳厂有限责任公司 Preparation method of ablation-resistant oxidation-resistant carbon-ceramic composite material matrix
CN114824989B (en) * 2022-03-09 2024-01-30 哈尔滨电碳厂有限责任公司 Preparation method of high-wear-resistance metal graphite brush

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