CN115231922A - Preparation method of graphite product - Google Patents

Preparation method of graphite product Download PDF

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CN115231922A
CN115231922A CN202210491416.2A CN202210491416A CN115231922A CN 115231922 A CN115231922 A CN 115231922A CN 202210491416 A CN202210491416 A CN 202210491416A CN 115231922 A CN115231922 A CN 115231922A
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graphite
parts
binder
powder
average particle
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贺世斌
徐玉洪
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Zigong Garanfat Composite Products Co ltd
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Zigong Garanfat Composite Products Co ltd
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Abstract

The invention belongs to the technical field of graphite product production, and discloses a preparation method of a graphite product, which comprises the following steps: the composite material comprises the following raw materials in parts by weight: 20-30 parts of graphite, 30-60 parts of calcined coke, 40-100 parts of binder, 1-5 parts of lubricant and 1-5 parts of wear-resisting agent are subjected to batching, kneading and grinding to obtain powder with the average particle size of 5-35 mu m, the obtained powder and additives including the binder and a release agent are added into a rapid stirring granulator with the rotating speed of 5000-30000r/min and stirred for 0.5-2h at the stirring temperature of 100-120 ℃, so that granules are obtained, wherein the mass ratio of the powder to the binder is 100:40-100, wherein the weight ratio of the release agent to the powder is 0.1-1. The graphite product adopts a near-net-shape processing mode, the surface area of a green body is large, the discharge of volatile matters is facilitated during sintering, the product is not easy to crack, and the rapid sintering can be realized; meanwhile, the processing amount can be greatly reduced, the material utilization rate is improved, the production cost is reduced, mass production is easy to realize, and the method has obvious progress compared with the prior art.

Description

Preparation method of graphite product
Technical Field
The invention belongs to the technical field of graphite product production, and particularly relates to a preparation method of a graphite product.
Background
Graphite products are a common material in industrial production, and can be mainly used for producing refractory materials, including refractory bricks and crucibles, and appliances, so that the graphite products are widely applied in industry and life.
However, the existing graphite carbon products are basically high in energy consumption and pollution, the production period of blanks is as long as 3-6 months, subsequent processing is complex and low in efficiency, with the high-speed development of economy in China, some new equipment falls to the home, the traditional carbon products cannot meet the technical requirements, and the preparation of the graphite products with near-net shape, excellent performance, high processing efficiency and low cost is basically realized under the technical background that the carbon graphite products are required to be low in hardness, high in strength, high in wear resistance, free from powder falling and free from black oil in some fields.
Disclosure of Invention
The present invention is directed to a method for preparing a graphite product, which solves the above problems of the prior art.
In order to achieve the above purpose, the invention provides the following technical scheme: a method of making a graphite article, comprising the steps of: s1, preparing the following raw materials in parts by weight: 20-30 parts of graphite, 30-60 parts of calcined coke, 40-100 parts of binder, 1-5 parts of lubricant and 1-5 parts of wear-resistant agent are subjected to batching, kneading and grinding to obtain powder with the average particle size of 5-35 mu m;
s2, adding the obtained powder and additives including a binder and a release agent into a rapid stirring granulator with the rotating speed of 5000-30000r/min, and stirring for 0.5-2h at the stirring temperature of 100-120 ℃ to obtain granules;
wherein the mass ratio of the powder to the binder is 100:40-100, wherein the weight ratio of the release agent to the powder is 0.1-1;
s3, performing near-net forming on the granulated material obtained in the step S2 on a hydraulic press to obtain a graphite green body;
and S4, sintering the graphite green body, and then performing finish machining on the graphite green body.
Preferably, the graphite is selected from one or two of natural graphite and artificial graphite, and the average particle size of the graphite is 10-50 μm.
Preferably, the calcined coke is selected from one or two of calcined petroleum coke and calcined asphalt coke, and the average particle size of the calcined coke is 10-50 μm.
Preferably, the binder is selected from modified asphalt with a softening point of 105-120 ℃, the quinoline insoluble content of the binder is 6-10%, and the toluene insoluble content of the binder is 20-30%.
Preferably, the toluene insoluble substance comprises one or more of polyammoniate, polyvinyl alcohol, polyvinyl chloride, glycerol ethanol and paraffine ethyl ether.
Preferably, the lubricant is selected from one or two of tungsten disulfide and molybdenum disulfide;
the wear-resisting agent is selected from one or more of silicon carbide, silicon dioxide, aluminum oxide, aluminum dihydrogen phosphate, magnesium silicate and wollastonite;
the release agent is selected from one or more of stearic acid, oleic acid, N' -ethylene bis stearamide, paraffin and zinc stearate.
Preferably, the raw material also comprises 0.1-10 parts by weight of spray carbon black.
Preferably, the raw material also comprises 0.1-5 parts by weight of chopped glass fiber, and the length of the chopped glass fiber is 1-5 mm.
Preferably, the near net shape pressure in S3 is 100-300MPa.
Preferably, the sintering temperature in the S4 is 800-1200 ℃, and the heat preservation time is 1-5h.
The invention has the following beneficial effects:
1. the graphite product adopts a near-net forming mode, the surface area of a green body is large, volatile matters are discharged conveniently during sintering, the product is not easy to crack, and quick sintering can be realized; meanwhile, the processing amount can be greatly reduced, the material utilization rate is improved, the production cost is reduced, mass production is easy to realize, and the method has obvious progress compared with the prior art.
2. The invention improves the fluidity of the powder by granulating the powder, the powder can be more uniformly filled into a forming die, the powder can better flow in the die during pressing, and the stability of the product is improved.
3. The carbon-graphite material prepared by adopting graphite and calcined coke as main raw materials and adopting the modified asphalt with high residual carbon value and high strength after roasting as a binder has the characteristics of high strength and high hardness of the carbon material and the lubricating characteristic of the graphite material, and the added wear-resisting agent and lubricant further improve the wear resistance of the material, and can be suitable for a long-term dry friction environment during operation.
4. In order to ensure the reliability of the graphite product, spray carbon black and glass fiber can be added as reinforcing components, the spray carbon black can further improve the wear resistance of the material, the chopped glass fiber can also moderately improve the wear resistance of the material while improving the strength, and the two additives as the carbonaceous raw materials can not change the percentage content of carbon in the final material.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, in an embodiment of the present invention, a method for preparing a graphite product includes the following steps: s1, preparing the following raw materials in parts by weight: 20-30 parts of graphite, 30-60 parts of calcined coke, 40-100 parts of binder, 1-5 parts of lubricant and 1-5 parts of wear-resistant agent are subjected to batching, kneading and grinding to obtain powder with the average particle size of 5-35 mu m;
s2, adding the obtained powder and additives including a binder and a release agent into a rapid stirring granulator with the rotating speed of 5000-30000r/min, and stirring for 0.5-2h at the stirring temperature of 100-120 ℃ to obtain granules;
wherein the mass ratio of the powder to the binder is 100:40-100, wherein the weight ratio of the release agent to the powder is 0.1-1;
s3, performing near-net forming on the granulated material obtained in the step S2 on a hydraulic press to obtain a graphite green body;
and S4, sintering the graphite green body, and then performing finish machining on the graphite green body.
Wherein the graphite is selected from one or two of natural graphite and artificial graphite, and the average particle diameter of the graphite is 10-50 μm.
Wherein the calcined coke is selected from one or two of calcined petroleum coke and calcined asphalt coke, and the average particle size of the calcined coke is 10-50 μm.
Wherein the binder is selected from modified asphalt with a softening point of 105-120 ℃, the quinoline insoluble content of the binder is 6-10%, and the toluene insoluble content of the binder is 20-30%.
Wherein the toluene insoluble substance comprises one or more of ammonium polyacrylate, polyvinyl alcohol, polyvinyl chloride, glycerol ethanol and paraffine ethyl ether.
Wherein, the lubricant is selected from one or two of tungsten disulfide and molybdenum disulfide;
the wear-resisting agent is selected from one or more of silicon carbide, silicon dioxide, aluminum oxide, aluminum dihydrogen phosphate, magnesium silicate and wollastonite;
the release agent is selected from one or more of stearic acid, oleic acid, N' -ethylene bis stearamide, paraffin and zinc stearate.
Wherein the raw material also comprises 0.1 to 10 weight parts of spray carbon black.
Wherein the raw material also comprises 0.1-5 parts by weight of chopped glass fiber, and the length of the chopped glass fiber is 1-5 mm.
Wherein the near net shape pressure in S3 is 100-300Mpa.
Wherein the sintering temperature in S4 is 800-1200 ℃, and the heat preservation time is 1-5h.
(1) Example 1:
the graphite bearing for the pump of the embodiment is prepared by the following steps:
1) Mixing, kneading and grinding 25 parts of natural graphite, 37 parts of calcined petroleum coke, 32 binder, 2 parts of tungsten disulfide and 4 parts of silicon carbide to obtain powder with the average particle size of 34.8 mu m, wherein the average particle size of the natural graphite is 35.2 mu m, the average particle size of the calcined petroleum coke is 18.6 mu m, the modified asphalt has the softening point of 106 ℃, the quinoline insoluble content is 8.5 percent, and the toluene insoluble content is 28.3 percent;
2) Adding 100 parts of powder and 0.5 part of ammonium polyacrylate into a rapid stirring granulator for granulation to obtain a granulated material with the average particle size of 65.7 mu m, wherein the rotating speed of a motor of the rapid stirring granulator is 8000 rpm, the stirring time is 2 hours, and the stirring temperature is 105 ℃;
3) Carrying out near net molding on the granulated material on a hydraulic press, wherein the molding pressure is 200MPa, and obtaining a graphite green body;
4) Sintering the graphite rotor green body at 1100 ℃, wherein the heat preservation time at 1100 ℃ is 2h;
5) And (6) finishing.
The implementation results are as follows: the graphite bearing had a bulk density of 1.72g/cm3, a Shore hardness of 65 (HSD), a resistivity of 35 μ Ω m, and an elastic modulus of 15GPa, and the amount of wear of the graphite bearing was 0.124mm after 6000 hours according to the test method for working durability in GB/T8872-2002.
(2) Example 2:
the graphite bearing for the pump of the embodiment is prepared by the following steps:
1) 30 parts of artificial graphite, 32 parts of calcined asphalt coke, 24 parts of binder, 1 part of molybdenum disulfide and 3 parts of silicon are kneaded and ground to obtain powder with the average particle size of 28.5 mu m, the average particle size of natural graphite is 28.8 mu m, the average particle size of calcined petroleum coke is 25.5 mu m, the modified asphalt softening point is 112 ℃, the quinoline insoluble content is 6.8 percent, and the toluene insoluble content is 22.5 percent;
2) Adding 100 parts of powder, 38 parts of water, 0.8 part of paraffin ether and 0.9 part of zinc stearate into a rapid stirring granulator for granulation to obtain a granulated material with the average particle size of 55.8 mu m, wherein the rotating speed of a motor of the rapid stirring granulator is 10000 revolutions per minute, the stirring time is 1.5 hours, and the stirring temperature is 105 ℃;
3) Molding the granulated material on a hydraulic press at the near net shape pressure of 180MPa to obtain a graphite rotor green body;
4) Sintering the green body of the graphite rotor at 1000 ℃, and keeping the temperature at 1000 ℃ for 3.5h;
5) And (7) finishing.
The implementation results are as follows: the graphite rotor had a bulk density of 1.75g/cm3, a Shore hardness of 69 (HSD), a resistivity of 24 μ Ω m, and an elastic modulus of 12GPa, and a graphite bearing end face wear of 0.097mm after 6000 hours according to the working durability test method in GB/T8872-2002.
(3) Example 3:
the graphite bearing for the pump of the embodiment is prepared by the following steps:
1) Mixing, kneading and grinding 15 parts of artificial graphite, 10 parts of natural graphite, 58 binder, 38 parts of modified asphalt, 3 parts of glass fiber, 2 parts of tungsten disulfide, 2 parts of SiO2 and 5 parts of spray carbon black to obtain powder with the average particle size of 21.2 mu m, wherein the average particle size of the mixture of the artificial graphite and the natural graphite is 28.2 mu m, the average particle size of calcined petroleum coke is 18.9 mu m, the softening point of the modified asphalt is 117 ℃, the quinoline insoluble content is 8.2 percent, and the toluene insoluble content is 35.8 percent;
2) Adding 100 parts of powder, 85 parts of water, 0.7 part of paraffin ether and 0.5 part of zinc stearate into a rapid stirring granulator for granulation to obtain a granulated material with the average particle size of 72.4 mu m, wherein the rotating speed of a motor of the rapid stirring granulator is 8000 revolutions per minute, the stirring time is 2 hours, and the stirring temperature is 118 ℃;
3) Carrying out near net molding on the granulated material on a hydraulic press, wherein the molding pressure is 220MPa, and obtaining a green body of the graphite bearing rotor;
4) Sintering the green graphite rotor blank at 900 ℃, and keeping the temperature of 900 ℃ for 4h;
5) And (6) finishing.
The implementation results are as follows: the graphite (bearing) rotor has a volume density of 1.68g/cm3, a Shore hardness of 75 (HSD), a resistivity of 45 [ mu ] omega m and an elastic modulus of 22GPa, and the graphite bearing wear of 0.063mm is obtained after 6000-ten thousand fatigue test cycles according to the working durability test method in GB/T8872-2002.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. A method for preparing a graphite product is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing a raw material composition by weight: 20-30 parts of graphite, 30-60 parts of calcined coke, 40-100 parts of binder, 1-5 parts of lubricant and 1-5 parts of wear-resistant agent are subjected to batching, kneading and grinding to obtain powder with the average particle size of 5-35 mu m;
s2, adding the obtained powder and additives including a binder and a release agent into a rapid stirring granulator with the rotating speed of 5000-30000r/min, and stirring for 0.5-2h at the stirring temperature of 100-120 ℃ to obtain granules;
wherein the mass ratio of the powder to the binder is 100:40-100, wherein the weight ratio of the release agent to the powder is 0.1-1;
s3, performing near-net forming on the granulated material obtained in the step S2 on a hydraulic press to obtain a graphite green body;
and S4, sintering the graphite green body, and then performing finish machining on the graphite green body.
2. The method of manufacturing a graphite article according to claim 1, wherein: the graphite is selected from one or two of natural graphite and artificial graphite, and the average particle diameter of the graphite is 10-50 μm.
3. The method of claim 1, wherein the graphite article comprises: the calcined coke is selected from one or two of calcined petroleum coke and calcined asphalt coke, and the average particle size of the calcined coke is 10-50 μm.
4. The method of claim 1, wherein the graphite article comprises: the binder is selected from modified asphalt with a softening point of 105-120 ℃, the quinoline insoluble content of the binder is 6-10%, and the toluene insoluble content of the binder is 20-30%.
5. The method of claim 4, wherein: the toluene insoluble substance comprises one or more of ammonium polyacrylate, polyvinyl alcohol, polyvinyl chloride, glycerol ethanol and paraffin ether.
6. The method of claim 1, wherein the graphite article comprises: the lubricant is selected from one or two of tungsten disulfide and molybdenum disulfide;
the anti-wear agent is selected from one or more of silicon carbide, silicon dioxide, aluminum oxide, aluminum dihydrogen phosphate, magnesium silicate and wollastonite;
the release agent is selected from one or more of stearic acid, oleic acid, N' -ethylene bis stearamide, paraffin and zinc stearate.
7. The method of claim 1, wherein the graphite article comprises: the raw material also comprises 0.1-10 parts by weight of spray carbon black.
8. The method of claim 1, wherein the graphite article comprises: the raw material also comprises 0.1-5 parts by weight of chopped glass fiber, and the length of the chopped glass fiber is 1-5 mm.
9. The method of claim 1, wherein the graphite article comprises: and the near net forming pressure in the S3 is 100-300Mpa.
10. The method of claim 1, wherein the graphite article comprises: the sintering temperature in S4 is 800-1200 ℃, and the heat preservation time is 1-5h.
CN202210491416.2A 2022-05-07 2022-05-07 Preparation method of graphite product Pending CN115231922A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115677350A (en) * 2022-11-22 2023-02-03 苏州东南佳新材料股份有限公司 Preparation method of carbon shaft sleeve for new energy automobile electronic water pump

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115677350A (en) * 2022-11-22 2023-02-03 苏州东南佳新材料股份有限公司 Preparation method of carbon shaft sleeve for new energy automobile electronic water pump
CN115677350B (en) * 2022-11-22 2024-05-24 苏州东南佳新材料股份有限公司 Preparation method of carbon shaft sleeve for new energy automobile electronic water pump

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