CN115181380B - High-temperature-resistant polytetrafluoroethylene-based composite material, preparation method thereof and application of composite material as high-temperature sealing material - Google Patents

High-temperature-resistant polytetrafluoroethylene-based composite material, preparation method thereof and application of composite material as high-temperature sealing material Download PDF

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CN115181380B
CN115181380B CN202210972932.7A CN202210972932A CN115181380B CN 115181380 B CN115181380 B CN 115181380B CN 202210972932 A CN202210972932 A CN 202210972932A CN 115181380 B CN115181380 B CN 115181380B
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fiber
polytetrafluoroethylene
composite material
temperature
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CN115181380A (en
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李宋
谢海
王廷梅
张海军
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Lanzhou Zhongke Jurun New Material Co ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/34—Silicon-containing compounds
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
    • C08K5/3445—Five-membered rings

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Abstract

The invention belongs to the technical field of inorganic materials, and particularly relates to a high-temperature-resistant polytetrafluoroethylene-based composite material, a preparation method thereof and application of the composite material as a high-temperature sealing material. The invention provides a high-temperature-resistant polytetrafluoroethylene-based composite material which comprises the following components in parts by mass: 65-85 parts of polytetrafluoroethylene, 10-20 parts of fiber reinforced filler, 1-5 parts of dimethyl imidazole cobalt and 5-15 parts of ceramic powder. According to the invention, the high-temperature stability of the composite material is improved by the cooperation of the dimethylimidazole cobalt and the ceramic powder, and simultaneously polytetrafluoroethylene is modified together with the fiber reinforced filler, so that the high-temperature resistance and durability of the composite material can be improved, the mechanical property of the composite material is improved, the composite material is endowed with excellent thermal stability, tensile property, wear resistance and sealing property, and the composite material has great application prospects in the field of high-temperature sealing.

Description

High-temperature-resistant polytetrafluoroethylene-based composite material, preparation method thereof and application of composite material as high-temperature sealing material
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a high-temperature-resistant polytetrafluoroethylene-based composite material, a preparation method thereof and application of the composite material as a high-temperature sealing material.
Background
Aeroengines are known as "industrial flowers" as "hearts" of aircraft, and are one of decisive factors for improving the performance of the aircraft and updating. The sealing device in the transmission and lubrication system of the aeroengine is one of key core components, so that the effective use of lubricating oil is ensured, the environment-controlled air-entraining pollution of the aircraft is prevented, and the sealing device is one of important influencing factors influencing the engine to reach the design service life index.
The conventional polytetrafluoroethylene lip sealing material is mostly used under normal temperature conditions, is difficult to use for a long time under high temperature conditions (about 150 ℃), and cannot ensure the reliability. The main reason is that the material has poor thermal stability and low mechanical strength under the conditions of high temperature and high load. Therefore, it is important to improve the temperature stability and mechanical bearing capacity of the polytetrafluoroethylene composite material.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant polytetrafluoroethylene-based composite material, a preparation method thereof and application of the high-temperature-resistant polytetrafluoroethylene-based composite material as a high-temperature sealing material.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a high-temperature-resistant polytetrafluoroethylene-based composite material which comprises the following components in parts by mass:
65-85 parts of polytetrafluoroethylene, 10-20 parts of fiber reinforced filler, 1-5 parts of dimethyl imidazole cobalt and 5-15 parts of ceramic powder.
Preferably, the particle size of the dimethylimidazole cobalt is 300-600 nm.
Preferably, the ceramic powder has a Mohs hardness of 5 to 8 and an average diameter of 10 to 25. Mu.m.
Preferably, the fiber reinforced filler comprises one or more of glass fiber, carbon fiber and aramid fiber.
Preferably, the length of the carbon fiber is 20-50 μm, and the diameter is 5-10 μm;
the diameter of the glass fiber is 5-15 mu m, and the length-diameter ratio is 10:1;
the length of the aramid fiber is less than 125 mu m, and the diameter is 5-15 mu m.
The invention provides a preparation method of the high-temperature-resistant polytetrafluoroethylene-based composite material, which comprises the following steps:
mixing polytetrafluoroethylene, fiber reinforced filler, dimethyl imidazole cobalt and ceramic powder to obtain a mixture;
cold pressing the mixture to obtain a blank;
and sintering the blank to obtain the high-temperature-resistant polytetrafluoroethylene-based composite material.
Preferably, the sintering temperature is 375 ℃, and the sintering heat preservation time is 90-150 min.
Preferably, the cold pressing pressure is 60MPa; the dwell time of the cold pressing is 30min; the temperature rising rate from room temperature to the sintering temperature was 10 ℃/min.
Preferably, the polytetrafluoroethylene has a particle size of 75 μm.
The invention provides the application of the high-temperature-resistant polytetrafluoroethylene-based composite material or the high-temperature-resistant polytetrafluoroethylene-based composite material prepared by the preparation method in the technical scheme as a high-temperature sealing material.
The invention provides a high-temperature-resistant polytetrafluoroethylene-based composite material which comprises the following components in parts by mass: 65-85 parts of polytetrafluoroethylene, 10-20 parts of fiber reinforced filler, 1-5 parts of dimethyl imidazole cobalt and 5-15 parts of ceramic powder. According to the invention, the high-temperature stability of the composite material is improved by the cooperation of the dimethylimidazole cobalt and the ceramic powder, and simultaneously polytetrafluoroethylene is modified together with the fiber reinforced filler, so that the high-temperature resistance and durability of the composite material can be improved, the mechanical property of the composite material is improved, the excellent thermal stability, tensile property, wear resistance and sealing property of the composite material are endowed, and the composite material has a great application prospect in the field of high-temperature sealing. The test results of the examples show that the tensile strength of the high-temperature-resistant polytetrafluoroethylene-based composite material provided by the invention under the service condition of 150 ℃ under the high temperature condition is 20.2-27.4 MPa, the friction coefficient is 0.001-0.0025, the abrasion mark width is 2.2-3.7 mm, and the sealing leakage amount is 1.1-3.4 mL.
The invention provides a preparation method of the high-temperature-resistant polytetrafluoroethylene-based composite material, which comprises the following steps: mixing polytetrafluoroethylene, fiber reinforced filler, dimethyl imidazole cobalt and ceramic powder to obtain a mixture; cold pressing the mixture to obtain a blank; and sintering the blank to obtain the high-temperature-resistant polytetrafluoroethylene-based composite material. According to the preparation method provided by the invention, polytetrafluoroethylene, fiber reinforced filler dimethyl imidazole cobalt and ceramic powder are sequentially mixed, cold-pressed and sintered, so that the fiber reinforced filler dimethyl imidazole cobalt and ceramic powder are used for modifying polytetrafluoroethylene together, and the composite material is excellent in heat stability, tensile property, wear resistance and sealing property, simple in preparation method and suitable for industrial production.
Drawings
FIG. 1 is an electron micrograph of dimethylimidazole cobalt used in an embodiment of the present invention;
FIG. 2 is an electron micrograph of a ceramic powder used in an embodiment of the invention.
Detailed Description
The invention provides a high-temperature-resistant polytetrafluoroethylene-based composite material which comprises the following components in parts by mass:
65-85 parts of polytetrafluoroethylene, 10-20 parts of fiber reinforced filler, 1-5 parts of dimethyl imidazole cobalt and 5-15 parts of ceramic powder.
In the present invention, all preparation materials/components are commercially available products well known to those skilled in the art unless specified otherwise.
The high temperature resistant polytetrafluoroethylene-based composite material provided by the invention comprises 65-85 parts by mass of polytetrafluoroethylene, preferably 65-80 parts by mass, and more preferably 65-78 parts by mass.
In a specific embodiment of the present invention, the high temperature resistant polytetrafluoroethylene-based composite material specifically includes 65 parts, 67 parts, 69 parts, 70 parts, 75 parts, 77 parts, or 78 parts polytetrafluoroethylene.
Based on the parts by weight of the polytetrafluoroethylene, the polytetrafluoroethylene composite material provided by the invention comprises 10-20 parts of fiber reinforced filler, and particularly 10 parts, 15 parts or 20 parts are preferable.
In the present invention, the fiber-reinforced filler preferably includes one or more of glass fiber, carbon fiber and aramid fiber.
As a specific embodiment of the present invention, the fiber-reinforced filler is carbon fiber and aramid fiber, and the mass ratio of the carbon fiber to the aramid fiber is preferably 1:1.
As a specific embodiment of the present invention, the fiber-reinforced filler is glass fiber.
As a specific embodiment of the present invention, the fiber-reinforced filler is an aramid fiber and a glass fiber, and the mass ratio of the aramid fiber to the glass fiber is preferably 1:1.
In the present invention, the carbon fiber preferably has a length of 20 to 50 μm and a diameter of 5 to 10 μm;
in the present invention, the glass fiber preferably has a diameter of 5 to 15 μm and an aspect ratio of 10:1;
in the present invention, the length of the aramid fiber is preferably < 125. Mu.m, and the diameter is preferably 5 to 15. Mu.m, more preferably 10. Mu.m.
In the invention, the fiber reinforced filler and the fiber reinforced filler with the parameters can further realize that the fiber reinforced filler cooperates with the dimethyl imidazole cobalt and the ceramic powder to improve the tensile strength performance of the composite material under the high-temperature condition
Based on the parts by weight of the polytetrafluoroethylene, the high-temperature resistant polytetrafluoroethylene composite material provided by the invention comprises 1-5 parts of dimethyl imidazole cobalt, and particularly preferably 1 part, 3 parts or 5 parts.
In the invention, the dimethyl imidazole cobalt is named MOF, ZIF-67, and is called ZIF-67 for short. How the physical parameters are
In the present invention, the particle size of the dimethylimidazole cobalt is 300 to 600nm, more preferably 350 to 550nm.
According to the invention, the MOF with good thermal stability, ZIF-67, is added into polytetrafluoroethylene, the MOF with good thermal stability, the thermal decomposition temperature is more than 400 ℃, and the tensile strength of the composite material can be improved, and the friction coefficient can be reduced.
Based on the parts by weight of the polytetrafluoroethylene, the high-temperature-resistant polytetrafluoroethylene composite material provided by the invention comprises 5-15 parts of ceramic powder, and particularly preferably 5 parts, 7 parts, 10 parts or 15 parts.
In the present invention, the ceramic powder preferably has a Mohs hardness of 5 to 8, and an average diameter of 10 to 25. Mu.m, more preferably 12 to 20. Mu.m.
The invention provides a ceramic powder which is a light non-metal multifunctional material and mainly comprises SiO (silicon dioxide) and is added into polytetrafluoroethylene 2 And Al 2 O 3 Good dispersibility, good chemical stability, good plasticity, high heat-resistant temperature, small density and low loss on ignition; the durability and the high temperature resistance of the composite material can be improved, the mechanical property of the composite material can be improved, and the production cost of the composite material can be reduced.
The invention provides a preparation method of the high-temperature-resistant polytetrafluoroethylene-based composite material, which comprises the following steps:
mixing polytetrafluoroethylene, fiber reinforced filler, dimethyl imidazole cobalt and ceramic powder to obtain a mixture;
cold pressing the mixture to obtain a blank;
and sintering the blank to obtain the high-temperature-resistant polytetrafluoroethylene-based composite material.
According to the invention, polytetrafluoroethylene, fiber reinforced filler, dimethyl imidazole cobalt and ceramic powder are mixed to obtain a mixture.
In the present invention, the particle size of the polytetrafluoroethylene is 75. Mu.m.
In an embodiment of the present invention, the polytetrafluoroethylene is purchased from japan gold fluorination limited.
In the present invention, the fiber-reinforced filler preferably includes one or more of glass fiber, carbon fiber and aramid fiber.
In the present invention, the carbon fiber is provided by Jiangsu Nantong carbon fiber Co.
In the present invention, the glass fiber is provided by Nanjing glass fiber institute.
In the present invention, the aramid fiber is provided by Shanghai Jinbai Utility Co., ltd
In the invention, the dimethyl imidazole cobalt is purchased from Jiangsu Xianfeng nano materials science and technology Co.
In the invention, the ceramic powder is purchased from Fucai mineral products limited company in Donghai county.
In the present invention, the mixing is preferably performed in a high temperature mixer (FW 177).
In the present invention, the mixing is preferably performed under stirring, and the stirring speed is preferably 18000 to 22000r/min.
In the present invention, the mixing is preferably mechanical mixing.
In the present invention, the total time of the mixing is preferably 2min; the heat dissipation is preferably carried out for 1h every 30s of the mixing.
After the mixture is obtained, the mixture is cold-pressed to obtain a blank.
In the present invention, the mixture is preferably dried before the cold pressing. In the present invention, the temperature of the drying is preferably 120℃and the soak temperature of the drying is preferably 2 hours.
In the present invention, the pressure of the cold pressing is preferably 60MPa.
In the present invention, the dwell time of the cold pressing is preferably 30min.
In the present invention, the temperature of the cold pressing is preferably room temperature.
In the present invention, the present invention preferably fills the mixture into a mold before the cold pressing. The invention preferably performs molding at the same time of cold pressing, and demolding to obtain a molded blank.
The invention has no special requirements on the material and the shape of the die, and the material and the shape of the die are selected according to the actual requirements of the polytetrafluoroethylene composite material.
After the blank is obtained, the blank is sintered to obtain the high-temperature-resistant polytetrafluoroethylene-based composite material.
In the present invention, the sintering is preferably performed in a polytetrafluoroethylene sintering furnace.
In the present invention, the sintering temperature is preferably 375 ℃.
In the present invention, the holding time for sintering is preferably 90 to 150 minutes, more preferably 95 to 145 minutes.
In the present invention, the rate of temperature rise from room temperature to the sintering temperature is preferably 10 ℃/min.
In the present invention, the unsintered polytetrafluoroethylene macromolecule is a mixture of crystalline and amorphous regions. During sintering, when the temperature reaches 327 ℃, the crystal area begins to disappear and is converted into an amorphous colloid. The better sintering temperature of the polytetrafluoroethylene product can lead the diffusion process of the molecular chain to be carried out rapidly. The movement result of the molecular chain eliminates the internal stress generated by directional fibrosis and the like of the polytetrafluoroethylene in the pushing process, so that the polytetrafluoroethylene interface disappears, and the polytetrafluoroethylene macromolecular chain tightly wraps the filler, so that the polytetrafluoroethylene composite material becomes a whole, and the mechanical strength of the composite material is improved.
In the invention, after the sintering is completed, the high-temperature-resistant polytetrafluoroethylene-based composite material is preferably naturally cooled to room temperature.
The invention provides the application of the high-temperature-resistant polytetrafluoroethylene-based composite material or the high-temperature-resistant polytetrafluoroethylene-based composite material prepared by the preparation method in the technical scheme as a high-temperature sealing material.
In the invention, the high-temperature-resistant polytetrafluoroethylene-based composite material is particularly preferably a sealing material of an aeroengine.
The technical solutions provided by the present invention are described in detail below with reference to the drawings and examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
69g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (10 g of aramid fiber, 10g of carbon fiber, 20-50 mu m in length and 7 mu m in diameter, and less than 125 mu m in length and 10 mu m in diameter) of aramid fiber, 10g of ZIF-671g (particle size of 300-600 nm) and 10g of ceramic powder (with Mohs hardness of 5-8 and average diameter of 15 mu m) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating from room temperature to 375 ℃, keeping the temperature at the temperature of 375 ℃ at a speed of 10 ℃/min, and freely cooling after sintering.
Example 2
67g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (10 g of aramid fiber, 10g of carbon fiber, 20-50 mu m in length and 7 mu m in diameter; 125 mu m in length and 10 mu m in diameter of the aramid fiber), 673g of ZIF-673g (particle size of 300-600 nm), 10g of ceramic powder (5-8 in Mohs hardness and 15 mu m in average diameter) and mechanical mixing in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s) are weighed. And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating from room temperature to 375 ℃, keeping the temperature at the temperature of 375 ℃ at a speed of 10 ℃/min, and freely cooling after sintering.
Example 3
65g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (10 g of aramid fiber, 10g of carbon fiber, 20-50 mu m in length and 7 mu m in diameter; 125 mu m in length and 10 mu m in diameter of the aramid fiber), 675g of ZIF-675g (particle size of 300-600 nm), 10g of ceramic powder (5-8 in Mohs hardness and 15 mu m in average diameter) and mechanical mixing in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s) are weighed. And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating from room temperature to 375 ℃, keeping the temperature at the temperature of 375 ℃ at a speed of 10 ℃/min, and freely cooling after sintering.
Example 4
75g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (glass fiber of 15g, glass fiber diameter of 10 mu m and length-diameter ratio of 10:1), ZIF-675g (particle size of 300-600 nm) and 5g of ceramic powder (Mohs hardness of 5-8 and average diameter of 15 mu m) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating to 375 ℃ from room temperature, keeping the temperature at 375 ℃ for 120min at a heating rate of 10 ℃/min, and freely cooling after sintering.
Example 5
70g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (glass fiber of 15g, glass fiber diameter of 10 mu m and length-diameter ratio of 10:1), ZIF-675g (particle size of 300-600 nm) and 10g of ceramic powder (Mohs hardness of 5-8 and average diameter of 15 mu m) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating to 375 ℃ from room temperature, keeping the temperature at 375 ℃ for 120min at a heating rate of 10 ℃/min, and freely cooling after sintering.
Example 6
65g of polytetrafluoroethylene (particle size of 75 μm), reinforcing filler (glass fiber 15g, glass fiber diameter of 10 μm and length-diameter ratio of 10:1), ZIF-675g (particle size of 300-600 nm), 15g of ceramic powder (Mohs hardness of 5-8 and average diameter of 15 μm) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating to 375 ℃ from room temperature, keeping the temperature at 375 ℃ for 120min at a heating rate of 10 ℃/min, and freely cooling after sintering.
Example 7
74g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (aramid fiber 5g, glass fiber diameter of 10 mu m, length-diameter ratio of 10:1; aramid fiber length < 125 mu m, diameter of 10 mu m), ZIF-671g (particle size of 300-600 nm), 15g of ceramic powder (Mohs hardness of 5-8, average diameter of 10-25 mu m) and mechanical mixing in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s) are weighed. And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating from room temperature to 375 ℃, keeping the temperature at the temperature of 375 ℃ for 150min at the heating rate of 10 ℃/min, and freely cooling after sintering.
Example 8
77g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (5 g of aramid fiber and 5g of glass fiber, wherein the diameter of the glass fiber is 10 mu m, the length-diameter ratio of the glass fiber is 10:1, the length of the aramid fiber is less than 125 mu m, the diameter of the aramid fiber is 10 mu m), 673g of ZIF-673g (particle size of 300-600 nm), 10g of ceramic powder (Mohs hardness of 5-8, average diameter of 10-25 mu m) and the materials are weighed and mechanically mixed in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s). And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating from room temperature to 375 ℃, keeping the temperature at the temperature of 375 ℃ for 150min at the heating rate of 10 ℃/min, and freely cooling after sintering.
Example 9
78g of polytetrafluoroethylene (particle size of 75 μm), reinforcing filler (aramid fiber 5g, glass fiber diameter of 10 μm, length-diameter ratio of 10:1; aramid fiber length < 125 μm, diameter of 10 μm), ZIF-675g (particle size of 300-600 nm), 7g of ceramic powder (Mohs hardness of 5-8, average diameter of 10-25 μm) and mechanical mixing in a high-speed mixer (FW 177) for 2min (radiating for 1h every 30 s) are weighed. And drying the mixed materials for 2 hours at 120 ℃, and cooling to room temperature for standby. And uniformly filling the mixed materials into a grinding tool, performing cold pressing and preforming under the pressure of 60MPa, maintaining the pressure for 30min, and demolding to form a blank. Placing the blank into a sintering furnace for sintering, gradually heating from room temperature to 375 ℃, keeping the temperature at the temperature of 375 ℃ for 150min at the heating rate of 10 ℃/min, and freely cooling after sintering.
Comparative example 1
70g of polytetrafluoroethylene (particle size of 75 mu m), 10g of reinforcing filler (10 g of aramid fiber, 10g of carbon fiber, 20-50 mu m in length and 7 mu m in diameter, and 10 mu m in diameter of the aramid fiber) and 10g of ceramic powder are weighed, and are mechanically mixed in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 1.
Comparative example 2
80g of polytetrafluoroethylene (particle size of 75 μm), reinforcing filler (glass fiber of 15g, glass fiber diameter of 10 μm and length-diameter ratio of 10:1) and ZIF-675g (particle size of 300-600 nm) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 4.
Comparative example 3
80g of polytetrafluoroethylene (particle size of 75 mu m) and reinforcing filler (10 g of aramid fiber and 10g of carbon fiber, wherein the length of the carbon fiber is 20-50 mu m, the diameter of the carbon fiber is 7 mu m, the length of the aramid fiber is less than 125 mu m, the diameter of the aramid fiber is 10 mu m) are weighed, and the materials are mechanically mixed in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 1.
Comparative example 4
69g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (glass fiber 15g, glass fiber diameter of 10 mu m and length-diameter ratio of 10:1), ZIF-676g (particle size of 300-600 nm) and 10g of ceramic powder (Mohs hardness of 5-8 and average diameter of 10-25 mu m) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 5.
Comparative example 5
69g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (glass fiber 15g, glass fiber diameter of 10 mu m and length-diameter ratio of 10:1), ZIF-675g (particle size of 300-600 nm) and 11g of ceramic powder (Mohs hardness of 5-8 and average diameter of 10-25 mu m) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 5.
Comparative example 6
55g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (aramid fiber 15, carbon fiber 15g, length of the carbon fiber of 20-50 mu m and diameter of 7 mu m, length of the aramid fiber of less than 125 mu m and diameter of 10 mu m), ZIF-675g (particle size of 300-600 nm), 10g of ceramic powder (Mohs hardness of 5-8 and average diameter of 10-25 mu m) and mechanical mixing in a high-speed stirrer (FW 177) for 2min (radiating for 1h every 30 s) are weighed. The remaining steps were the same as in example 5.
Comparative example 7
50g of polytetrafluoroethylene (particle size of 75 mu m), reinforcing filler (20 g of aramid fiber, 20g of carbon fiber, 20-50 mu m in length of carbon fiber and 7 mu m in diameter, and less than 125 mu m in length of aramid fiber and 10 mu m in diameter) and 10g of ceramic powder (with Mohs hardness of 5-8 and average diameter of 10-25 mu m) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 5.
Comparative example 8
Polytetrafluoroethylene 55 (particle size of 75 μm), reinforcing filler (20 g of aramid fiber, 20g of carbon fiber, 20-50 μm of length of carbon fiber and 7 μm of diameter, and less than 125 μm of length of aramid fiber and 10 μm of diameter) and ZIF-675g (particle size of 300-600 nm) are weighed and added into a high-speed stirrer (FW 177) to be mechanically mixed for 2min (radiating for 1h every 30 s). The remaining steps were the same as in example 5.
Test case
Test conditions:
tensile strength: the test was carried out according to GB/T1040.2-2006, the sample gauge (50.0.+ -. 0.5) mm, tested using a universal tester, the draw rate was 50mm/min, 3 samples were tested and their average value calculated.
Coefficient of friction: a high-speed ring block friction and wear testing machine is adopted for testing, and the sealing pair piece material of the lip sealing typical structure of the parts such as the accessory case, the oil sliding cavity and the like of the researched aeroengine is 16Cr3NiWMoVNbE (HRC is more than or equal to 50, GB/T12444-2006). The test ring rotation speed is 200r/min, the time is 4h, the load is 200N, the medium temperature is 150 ℃, 3 test samples are tested for each group, and the average friction value is calculated.
Sealing test: according to GB/T21283.4 sealing element is part 4 of a rotating shaft lip seal ring of thermoplastic material: performance test procedure lip seal test was performed. The medium is Mobil No. II lubricating oil, and the single sealing period is 24 hours, including room temperature (14 hours, 5000 rpm), 150 ℃ (6 hours, 10000 rpm), shutdown cooling for 4 hours, and the whole test is 10 cycles. Table 1 shows the results of examples and comparative examples.
Table 1 results of examples and comparative examples
Analysis of results:
it can be seen from examples 1 to 3 that the mechanical properties, tribological properties and sealing properties of the composite materials are improved with increasing ZIF-67 content. The main reasons are that ZIF-67 has excellent thermal stability and good carrying capacity.
It can be seen from examples 4 to 6 that the mechanical properties, tribological properties and sealing properties of the composite materials are improved with increasing ceramic powder content. The main reasons are that ceramic powders have excellent thermal stability and good carrying capacity.
From examples 7 to 9, it was found that the ZIF-67 and ceramic powders at different levels had different abilities to improve the mechanical properties, tribological properties and sealing properties of the composite materials.
From comparative examples 1 to 3 and examples 1 and 4, it was found that when the contents of polytetrafluoroethylene and reinforcing filler were within the prescribed ranges, there was no ZIF-67 or no ceramic powder added, and the mechanical properties, tribological properties and sealing properties of the composite materials were degraded. When both are not added at the same time, the mechanical properties, tribological properties and sealing properties of the material are severely degraded.
From comparative examples 4 and 5 and example 5, it was found that when the contents of polytetrafluoroethylene and reinforcing filler were within the prescribed range, the mechanical properties, tribological properties and sealing properties of the composite material were severely degraded, while the ZIF-67 or ceramic powder contents were not within the prescribed range. The ZIF-67 or ceramic can generate agglomeration phenomenon when exceeding a specified range, and the performance of the composite material is reduced.
From comparative examples 6 to 8 and example 5, it was found that when the contents of polytetrafluoroethylene and reinforcing filler were not within the prescribed range, the mechanical properties, tribological properties and sealing properties of the composite material were not improved as much as those of polytetrafluoroethylene and reinforcing filler when ZIF-67 or ceramic powder or both were added.
In summary, ZIF-67 and ceramic powder filler with proper ranges have an enhancement effect on the mechanical property, tribological property and sealing property of the composite material. And the appropriate amount of polytetrafluoroethylene and reinforcing filler also affect the overall properties of the material.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.

Claims (6)

1. The high-temperature-resistant polytetrafluoroethylene-based composite material is characterized by comprising the following components in parts by weight:
69 parts of polytetrafluoroethylene, 20 parts of fiber reinforced filler, 1 part of dimethyl imidazole cobalt and 10 parts of ceramic powder; the fiber reinforced filler is carbon fiber and aramid fiber, and the mass ratio of the carbon fiber to the aramid fiber is 1:1;
or the components with the following mass portions: 67 parts of polytetrafluoroethylene, 20 parts of fiber reinforced filler, 3 parts of dimethyl imidazole cobalt and 10 parts of ceramic powder; the fiber reinforced filler is carbon fiber and aramid fiber, and the mass ratio of the carbon fiber to the aramid fiber is 1:1;
or the components with the following mass portions: 65 parts of polytetrafluoroethylene, 20 parts of fiber reinforced filler, 5 parts of dimethyl imidazole cobalt and 10 parts of ceramic powder; the fiber reinforced filler is carbon fiber and aramid fiber, and the mass ratio of the carbon fiber to the aramid fiber is 1:1;
or the components with the following mass portions: 75 parts of polytetrafluoroethylene, 15 parts of fiber reinforced filler, 5 parts of dimethyl cobalt imidazole and 5 parts of ceramic powder; the fiber reinforced filler is glass fiber;
or the components with the following mass portions: 70 parts of polytetrafluoroethylene, 15 parts of fiber reinforced filler, 5 parts of dimethyl imidazole cobalt and 10 parts of ceramic powder; the fiber reinforced filler is glass fiber;
or the components with the following mass portions: 65 parts of polytetrafluoroethylene, 15 parts of fiber reinforced filler, 5 parts of dimethyl imidazole cobalt and 15 parts of ceramic powder; the fiber reinforced filler is glass fiber;
or the components with the following mass portions: 74 parts of polytetrafluoroethylene, 10 parts of fiber reinforced filler, 1 part of dimethyl cobalt imidazole and 15 parts of ceramic powder; the fiber reinforced filler is aramid fiber and glass fiber, and the mass ratio of the aramid fiber to the glass fiber is 1:1;
or the components with the following mass portions: 77 parts of polytetrafluoroethylene, 10 parts of fiber reinforced filler, 3 parts of dimethyl imidazole cobalt and 10 parts of ceramic powder; the fiber reinforced filler is aramid fiber and glass fiber, and the mass ratio of the aramid fiber to the glass fiber is 1:1;
or the components with the following mass portions: 78 parts of polytetrafluoroethylene, 10 parts of fiber reinforced filler, 5 parts of dimethyl imidazole cobalt and 7 parts of ceramic powder; the fiber reinforced filler is aramid fiber and glass fiber, and the mass ratio of the aramid fiber to the glass fiber is 1:1;
the particle size of the dimethyl imidazole cobalt is 300-600 nm; the Mohs hardness of the ceramic powder is 5-8, and the average diameter is 10-25 mu m; the fiber reinforced filler comprises one or more of glass fiber, carbon fiber and aramid fiber; the length of the carbon fiber is 20-50 mu m, and the diameter is 5-10 mu m; the diameter of the glass fiber is 5-15 mu m, and the length-diameter ratio is 10:1; the length of the aramid fiber is less than 125 mu m, and the diameter is 5-15 mu m.
2. The method for preparing the high temperature resistant polytetrafluoroethylene-based composite material as claimed in claim 1, comprising the steps of:
mixing polytetrafluoroethylene, fiber reinforced filler, dimethyl imidazole cobalt and ceramic powder to obtain a mixture;
cold pressing the mixture to obtain a blank;
and sintering the blank to obtain the high-temperature-resistant polytetrafluoroethylene-based composite material.
3. The method according to claim 2, wherein the sintering temperature is 375 ℃, and the sintering holding time is 90-150 min.
4. The method of claim 2, wherein the cold pressing is at a pressure of 60MPa; the dwell time of the cold pressing is 30min; the temperature rising rate from room temperature to the sintering temperature was 10 ℃/min.
5. The method according to claim 2, wherein the polytetrafluoroethylene has a particle size of 75 μm.
6. The use of the high temperature resistant polytetrafluoroethylene-based composite material according to claim 1 or the high temperature resistant polytetrafluoroethylene-based composite material prepared by the preparation method according to any one of claims 2 to 5 as a high temperature sealing material.
CN202210972932.7A 2022-08-15 2022-08-15 High-temperature-resistant polytetrafluoroethylene-based composite material, preparation method thereof and application of composite material as high-temperature sealing material Active CN115181380B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113943488A (en) * 2021-08-31 2022-01-18 暨南大学 Composite material based on polytetrafluoroethylene-coated MOFs material and preparation method thereof
CN114621545A (en) * 2022-04-18 2022-06-14 中国科学院兰州化学物理研究所 High-wear-resistance composite material and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113943488A (en) * 2021-08-31 2022-01-18 暨南大学 Composite material based on polytetrafluoroethylene-coated MOFs material and preparation method thereof
CN114621545A (en) * 2022-04-18 2022-06-14 中国科学院兰州化学物理研究所 High-wear-resistance composite material and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
李建军主编.《塑料配方设计》.中国轻工业出版社，,2019,(第3版),第177-178页. *
聚四氟乙烯改性技术的研究;谢刚等;合成材料老化与应用;第36卷(第01期);第32-39页 *

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