CN113621210B - Polytetrafluoroethylene composite material and preparation method and application thereof - Google Patents

Polytetrafluoroethylene composite material and preparation method and application thereof Download PDF

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CN113621210B
CN113621210B CN202110994028.1A CN202110994028A CN113621210B CN 113621210 B CN113621210 B CN 113621210B CN 202110994028 A CN202110994028 A CN 202110994028A CN 113621210 B CN113621210 B CN 113621210B
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polytetrafluoroethylene
parts
composite material
particle size
polyimide
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CN113621210A (en
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张新瑞
谢海
李宋
王齐华
王廷梅
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions 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; Compositions of derivatives of such polymers
    • C08L27/02Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18Homopolymers or copolymers or tetrafluoroethene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention relates to the technical field of lubricating and sealing materials, in particular to a polytetrafluoroethylene composite material and a preparation method and application thereof. The polytetrafluoroethylene composite material provided by the invention comprises the following preparation raw materials in parts by weight: 60-70 parts of polytetrafluoroethylene resin; 20-30 parts of tin bronze powder; 5-10 parts of polyimide; 1-5 parts of glass fiber; 1-5 parts of graphite; 0.5-2 parts of inorganic nano filler; 0.05-0.2 part of a coupling agent; the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are in a micron order. The polytetrafluoroethylene composite material can have high strength and toughness.

Description

Polytetrafluoroethylene composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of lubricating and sealing materials, in particular to a polytetrafluoroethylene composite material and a preparation method and application thereof.
Background
The Chinese academy of engineering in the study of the current situation and development strategy of the science and engineering of tribology indicates that about 1/3% of the global primary energy is consumed by friction and 60% of the machine parts fail due to wear. Frictional wear not only results in a great deal of material and parts waste, but can directly result in catastrophic failure. With the increasingly severe service conditions of the novel equipment, severe working conditions such as wide temperature range, heavy load, high speed, strong impact, poor lubrication and the like put high requirements on the lubricating and wear-resisting properties of the material.
The polytetrafluoroethylene wear-resistant composite material has excellent designability and can be widely applied to a high-end equipment pneumatic-hydraulic servo system as a wear-resistant part. However, the traditional polytetrafluoroethylene wear-resistant composite material has the problems of weak bearing capacity, poor wear resistance and the like, cannot meet the use requirement, and can meet the use requirement of harsh working conditions only by filling and modifying. In order to improve the bearing capacity and the wear resistance, the prior art generally realizes the purpose of adding fibers, solid lubricants and other special nano functional fillers, but after the fillers are filled, the tensile strength and the toughness of the fillers are reduced, and the high bearing capacity and the high elongation at break are difficult to realize.
Disclosure of Invention
The invention aims to provide a polytetrafluoroethylene composite material, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a polytetrafluoroethylene composite material which comprises the following preparation raw materials in parts by weight:
Figure BDA0003233302270000011
Figure BDA0003233302270000021
the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are in a micron order.
Preferably, the coupling agent comprises trimethoxy silane N- [3- (trimethoxysilyl) propyl ] ethylenediamine and/or 3-aminopropyltriethoxysilane.
Preferably, the inorganic nano filler comprises one or more of nano silicon carbide, nano silicon nitride and nano silicon dioxide;
the particle size of the inorganic nano filler is 15-40 nm.
Preferably, the particle size of the polytetrafluoroethylene resin is 50-100 μm;
the particle size of the tin bronze powder is 1-2 mu m;
the particle size of the polyimide is 38-45 mu m;
the diameter of the glass fiber is 8-14 μm, and the length-diameter ratio is (8-10): 1;
the particle size of the graphite is 1-10 mu m.
Preferably, the grade of the tin bronze powder is 663.
The invention also provides a preparation method of the polytetrafluoroethylene composite material in the technical scheme, which comprises the following steps:
mixing a coupling agent, inorganic nano-filler, glass fiber, polytetrafluoroethylene resin, polyimide, graphite, tin bronze powder and absolute ethyl alcohol to obtain a mixture;
pressing and forming the mixture to obtain a blank;
sintering the blank to obtain the polytetrafluoroethylene composite material;
the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are in a micron order.
Preferably, the mass ratio of the coupling agent to the absolute ethyl alcohol is 1: (2000-4000).
Preferably, the press forming comprises a forward press and an inverted press which are sequentially carried out;
the pressure of the forward pressing is 15-25 MPa, and the pressure maintaining time is 1-6 min;
the pressure of the inverted pressing is 30-50 MPa, and the pressure maintaining time is 5-8 min.
Preferably, the sintering process comprises: after the temperature is increased from room temperature to 270-280 ℃ at the heating rate of 3-5 ℃/min and is preserved for 20-40 min, the temperature is increased from 270-280 ℃ to 325-345 ℃ at the heating rate of 1-2 ℃/min and is preserved for 20-40 min, then the temperature is increased from 325-345 ℃ to 360-365 ℃ at the heating rate of 1-2 ℃/min and is preserved for 100-200 min, then the temperature is reduced from 360-365 ℃ to 270-280 ℃ at the cooling rate of 0.5-1 ℃/min and is preserved for 150-200 min, and the furnace cooling is carried out.
The invention also provides the application of the polytetrafluoroethylene composite material in the technical scheme or the polytetrafluoroethylene composite material prepared by the preparation method in the technical scheme in the field of lubrication and sealing.
The invention provides a polytetrafluoroethylene composite material which comprises the following preparation raw materials in parts by weight: 60-70 parts of polytetrafluoroethylene resin; 20-30 parts of tin bronze powder; 5-10 parts of polyimide; 1-5 parts of glass fiber; 1-5 parts of graphite; 0.5-2 parts of inorganic nano filler; 0.05-0.2 part of a coupling agent; the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are in a micron order. The tin bronze powder can remarkably improve the bearing resistance, heat conduction and wear resistance of the polytetrafluoroethylene; the glass fiber can improve the mechanical property of the polytetrafluoroethylene wear-resistant composite material and play a role in modifying the polytetrafluoroethylene so as to stabilize the friction coefficient of the polytetrafluoroethylene wear-resistant composite material; the polyimide has good compatibility with polytetrafluoroethylene resin, and can play a role in enhancing and toughening at the same time; the inorganic nano filler has a synergistic composite effect with the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite, so that the strength and toughness of the material can be improved, and the wear resistance of the material can be obviously improved; the coupling agent can modify inorganic nano-filler and glass fiber, improve the dispersibility of the inorganic nano-filler and the glass fiber in a polytetrafluoroethylene resin matrix and improve the interface bonding force between the inorganic nano-filler and the polytetrafluoroethylene resin matrix. Thereby improving the strength and toughness of the polytetrafluoroethylene wear-resistant composite material.
Detailed Description
The invention provides a polytetrafluoroethylene composite material which comprises the following preparation raw materials in parts by mass:
Figure BDA0003233302270000031
the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are in a micron order.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
The polytetrafluoroethylene composite material comprises, by weight, 60-70 parts of polytetrafluoroethylene resin, preferably 62-68 parts of polytetrafluoroethylene resin, and more preferably 64-65 parts of polytetrafluoroethylene resin. In the present invention, the particle size of the polytetrafluoroethylene resin is preferably 50 to 100 μm, and more preferably 60 to 80 μm.
The preparation raw materials of the polytetrafluoroethylene composite material comprise, by weight, 20-30 parts of tin bronze powder, preferably 22-27 parts of tin bronze powder, and more preferably 23-26 parts of tin bronze powder. In the present invention, the grade of the tin bronze powder is preferably 663. In the present invention, the particle size of the tin bronze powder is preferably 1 to 2 μm. In the invention, the tin bronze powder can effectively solve the problem that pure copper powder is easy to oxidize in air to generate copper oxide.
The preparation raw materials of the polytetrafluoroethylene composite material comprise 5-10 parts of polyimide by weight, preferably 6-8 parts by weight of polytetrafluoroethylene resin. In the present invention, the polyimide is preferably a thermoplastic polyimide; the present invention does not specifically limit the kind of the thermoplastic polyimide, and the thermoplastic polyimide may be produced by a process known to those skilled in the art. In the present invention, the particle size of the polyimide is preferably 38 to 45 μm, and more preferably 40 to 42 μm.
The polytetrafluoroethylene composite material comprises, by weight, 1-5 parts of glass fiber, preferably 2-4 parts, and more preferably 2.5-3.5 parts. In the invention, the diameter of the glass fiber is preferably 8-14 μm, and more preferably 10-12 μm; the length-diameter ratio is preferably (8-10): 1, more preferably (8.5 to 9.5): 1.
the preparation raw materials of the polytetrafluoroethylene composite material comprise 1-5 parts of graphite, more preferably 2-4 parts, and most preferably 2.5-3.5 parts by weight of the polytetrafluoroethylene resin. In the present invention, the particle size of the graphite is preferably 1 to 10 μm, and more preferably 4 to 7 μm.
Based on the weight parts of the polytetrafluoroethylene resin, the preparation raw materials of the polytetrafluoroethylene composite material comprise 0.5-2 parts of inorganic nano-filler, and preferably 0.8-1.3 parts. In the invention, the inorganic nano filler preferably comprises one or more of nano silicon carbide, nano silicon nitride and nano silicon dioxide; when the inorganic nano-filler is more than two of the specific choices, the proportion of the specific substances is not limited in any way, and the specific substances can be mixed according to any proportion. In the present invention, the particle size of the inorganic nanofiller is preferably 15 to 40nm, more preferably 20 to 35nm, and most preferably 25 to 30 nm.
Based on the weight parts of the polytetrafluoroethylene resin, the raw materials for preparing the polytetrafluoroethylene composite material comprise 0.05-0.2 parts of coupling agent, preferably 0.1-0.15 parts. In the present invention, the coupling agent preferably comprises trimethoxy silane N- [3- (trimethoxysilyl) propyl ] ethylenediamine and/or 3-aminopropyltriethoxysilane, more preferably trimethoxy silane N- [3- (trimethoxysilyl) propyl ] ethylenediamine; when the coupling agents are more than two of the above specific choices, the present invention does not have any special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion.
The invention also provides a preparation method of the polytetrafluoroethylene composite material in the technical scheme, which comprises the following steps:
mixing a coupling agent, inorganic nano-filler, glass fiber, polytetrafluoroethylene resin, polyimide, graphite, tin bronze powder and absolute ethyl alcohol to obtain a mixture;
pressing and forming the mixture to obtain a blank;
sintering the blank to obtain the polytetrafluoroethylene composite material;
the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are micron-sized.
The invention mixes coupling agent, inorganic nano-filler, glass fiber, polytetrafluoroethylene resin, polyimide, graphite, tin bronze powder and absolute ethyl alcohol to obtain a mixture.
In the present invention, the mixing preferably comprises the steps of:
after the coupling agent and the absolute ethyl alcohol are mixed for the first time, the inorganic nano filler and the glass fiber are sequentially added for the second mixing, and finally, the polytetrafluoroethylene resin, the polyimide, the graphite and the tin bronze powder are sequentially added for the third mixing.
In the present invention, the mass ratio of the coupling agent to the absolute ethyl alcohol is preferably 1: (2000 to 4000), more preferably 1: (2500-3500).
In the present invention, the first mixing, the second mixing and the third mixing are all preferably performed under stirring conditions; the rotation speed of the stirring is preferably 100-200 rpm independently, more preferably 120-180 rpm, and most preferably 140-160 rpm. In the invention, the time of the first mixing is preferably 0.5-1 h, and more preferably 0.6-0.8 h; the second mixing time is preferably 0.5-1 h, and more preferably 0.6-0.8 h; the time for the third mixing is preferably 1 to 2 hours, and more preferably 1.3 to 1.6 hours.
After the mixing is finished, the invention also preferably comprises filtering and drying which are carried out in sequence; the filtration and drying of fluorine in the present invention are not subject to any particular limitation, and may be carried out by a procedure well known to those skilled in the art.
After the mixture is obtained, the invention also preferably comprises the steps of sequentially crushing and sieving the mixture; in the present invention, the rotation speed of the pulverization is preferably 24000 rpm; the time for crushing is preferably 30-50 s, and more preferably 35-45 s. In the present invention, the pulverization is preferably carried out in a small-sized universal pulverizer. In the invention, the aperture of the sieve used for sieving is preferably 35-70 meshes. In the specific embodiment of the invention, the addition amount of the mixture is preferably 200-400 g, more preferably 230-250 g, relative to a pulverizer with the diameter of 177mm and the depth of 70 mm;
after the mixture is obtained, the mixture is pressed and formed to obtain the wool blank.
In the present invention, the press forming preferably includes forward pressing and inverted pressing in this order. In the invention, the pressure of the forward pressing is preferably 15-25 MPa, and more preferably 18-22 MPa; the pressure maintaining time is preferably 1-6 min, and more preferably 1.2-2 min. In the invention, the pressure of the inverted pressing is preferably 30-50 MPa, more preferably 35-45 MPa, and most preferably 38-42 MPa; the pressure maintaining time is preferably 5-8 min, and more preferably 6-7 min. In the invention, the purpose of carrying out compression molding by adopting a combination of inverted compression and forward compression is to ensure uniform stress and uniform density of each part.
After the press-forming, the present invention preferably further comprises demolding; the demolding process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art.
After obtaining the rough blank, sintering the rough blank to obtain the polytetrafluoroethylene composite material.
In the present invention, the sintering process preferably includes: after the temperature is increased from room temperature to 270-280 ℃ at the heating rate of 3-5 ℃/min and is preserved for 20-40 min, the temperature is increased from 270-280 ℃ to 325-345 ℃ at the heating rate of 1-2 ℃/min and is preserved for 20-40 min, then the temperature is increased from 325-345 ℃ to 360-365 ℃ at the heating rate of 1-2 ℃/min and is preserved for 100-200 min, then the temperature is reduced from 360-365 ℃ to 270-280 ℃ at the cooling rate of 0.5-1 ℃/min and is preserved for 150-200 min, and the furnace cooling is carried out; more preferably, the method comprises the steps of heating from room temperature to 273-276 ℃ at a heating rate of 4 ℃/min, keeping the temperature for 25-35 min, heating from 273-276 ℃ to 330-340 ℃ at a heating rate of 1.3-1.5 ℃/min, keeping the temperature for 25-35 min, heating from 330-340 ℃ to 362-363 ℃ at a heating rate of 1.4-1.6 ℃/min, keeping the temperature for 130-160 min, cooling from 362-363 ℃ to 273-276 ℃ at a cooling rate of 0.6-0.8 ℃/min, keeping the temperature for 160-180 min, and cooling with a furnace.
In the present invention, the sintering process described above functions as a process for integrally sintering polytetrafluoroethylene powder and other fillers.
The invention also provides the application of the polytetrafluoroethylene composite material in the technical scheme or the polytetrafluoroethylene composite material prepared by the preparation method in the technical scheme in the field of lubrication and sealing. The method of the present invention is not particularly limited, and the method may be performed by a method known to those skilled in the art.
The polytetrafluoroethylene composite material provided by the present invention, the preparation method and the application thereof are described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Dispersing 0.1g N, - [3- (trimethoxysilyl) propyl ] ethylenediamine in 300g of absolute ethyl alcohol, stirring for 0.5h, adding 1g of nano silicon carbide (particle size of 20nm) and 5g of glass fiber (diameter of 14 μm and length-diameter ratio of 8:1), stirring for 0.5h, adding 70g of polytetrafluoroethylene resin (particle size of 50 μm), 5g of polyimide (particle size of 45 μm), 3g of graphite (particle size of 5 μm) and 20g of tin bronze powder (trade name 663, particle size of 2 μm), stirring for 1h, filtering, and drying to obtain a mixture;
placing the mixture into a small universal pulverizer, wherein the adding amount is 300g each time, the rotating speed is 24000rpm, the time is 30s, after sieving through a 45-mesh sieve, adding the sieved mixture into a mold, firstly adopting 25MPa pressure to forward press for 1min to compact, adopting 50MPa pressure to reversely press for 5min, and demolding to obtain a blank;
and (2) putting the blank material into a sintering furnace for sintering, heating from room temperature to 270 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 20min, heating from 270 ℃ to 325 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 100min, heating from 325 ℃ to 360 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 200min, cooling from 360 ℃ to 270 ℃, and cooling along with the furnace to obtain the polytetrafluoroethylene composite material.
Example 2
Dispersing 0.06g N, - [3- (trimethoxysilyl) propyl ] ethylenediamine in 200g of absolute ethyl alcohol, stirring for 1h, adding 0.5g of nano silicon carbide (particle size of 15nm), 0.5g of nano silicon nitride (particle size of 30nm) and 3g of glass fiber (diameter of 12 μm, length-diameter ratio of 10:1), stirring for 1h, adding 65g of polytetrafluoroethylene resin (particle size of 70 μm), 10g of polyimide (particle size of 38 μm), 1g of graphite (particle size of 1 μm) and 25g of tin bronze powder (trade name 663, particle size of 1 μm), stirring for 1h, filtering, and drying to obtain a mixture;
putting the mixture into a small universal pulverizer, wherein the adding amount is 350g each time, the rotating speed is 24000rpm, the time is 40s, after sieving by a 70-mesh sieve, adding the sieved mixture into a mold, firstly adopting the pressure of 20MPa for forward pressing for 2min for compaction, adopting the pressure of 45MPa for inverted pressing for 7min, and demolding to obtain a blank;
and (2) putting the blank material into a sintering furnace for sintering, heating from room temperature to 275 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 30min, heating from 275 ℃ to 330 ℃ at the heating rate of 1.5 ℃/min, keeping the temperature for 30min, heating from 330 ℃ to 365 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 150min, cooling from 365 ℃ to 270 ℃, keeping the temperature for 180min, and cooling along with the furnace to obtain the polytetrafluoroethylene composite material.
Example 3
Dispersing 0.08g N, - [3- (trimethoxysilyl) propyl ] ethylenediamine in 400g of absolute ethyl alcohol, stirring for 0.6h, adding 1g of nano silicon dioxide (particle size of 30nm) and 4g of glass fiber (diameter of 8 μm and length-diameter ratio of 8:1), stirring for 0.6h, adding 60g of polytetrafluoroethylene resin (particle size of 100 μm), 5g of polyimide (particle size of 45 μm), 2g of graphite (particle size of 10 μm) and 30g of tin bronze powder (trade name 663, particle size of 1.5 μm), stirring for 1.5h, filtering, and drying to obtain a mixture;
putting the mixture into a small-sized universal pulverizer, wherein the adding amount is 400g each time, the rotating speed is 24000rpm, the time is 50s, after sieving by a 35-mesh sieve, adding the sieved mixture into a mold, firstly adopting the pressure of 15MPa for forward pressing for 1min for compaction, adopting the pressure of 40MPa for inverted pressing for 5min, and demolding to obtain a blank;
and (2) putting the blank material into a sintering furnace for sintering, heating from room temperature to 270 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 20min, heating from 270 ℃ to 325 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 20min, heating from 325 ℃ to 365 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 100min, cooling from 365 ℃ to 270 ℃, keeping the temperature for 200min, and cooling along with the furnace to obtain the polytetrafluoroethylene composite material.
Example 4
Dispersing 0.1g N, - [3- (trimethoxysilyl) propyl ] ethylenediamine in 350g of absolute ethyl alcohol, stirring for 0.8h, adding 0.5g of nano silicon dioxide (particle size of 40nm), 0.5g of nano silicon nitride (particle size of 30nm) and 4g of glass fiber (diameter of 14 μm and length-diameter ratio of 9:1), stirring for 0.8h, adding 60g of polytetrafluoroethylene resin (particle size of 75 μm), 10g of polyimide (particle size of 38 μm), 5g of graphite (particle size of 10 μm) and 20g of tin bronze powder (trade name 663, particle size of 2 μm), stirring for 2h, filtering, and drying to obtain a mixture;
putting the mixture into a small universal pulverizer, wherein the adding amount is 250g each time, the rotating speed is 24000rpm, the time is 30s, after sieving with a 35-mesh sieve, adding the sieved mixture into a mold, firstly adopting the pressure of 20MPa for forward pressing for 1min for compaction, adopting the pressure of 30MPa for inverted pressing for 8min, and demolding to obtain a blank;
and (2) putting the blank material into a sintering furnace for sintering, heating from room temperature to 280 ℃ at the heating rate of 4 ℃/min, keeping the temperature for 30min, heating from 280 ℃ to 340 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 20min, heating from 340 ℃ to 365 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 120min, cooling from 365 ℃ to 280 ℃, keeping the temperature for 200min, and cooling along with the furnace to obtain the polytetrafluoroethylene composite material.
Example 5
Referring to example 2, the only difference is that the particle size of the polyimide is 75 μm.
Example 6
Referring to example 3, the only difference is that the tin bronze powder of grade 663 has a particle size of 45 μm.
Comparative example 1
Referring to example 2, the only difference is that 0.5g of nano silicon carbide and 0.5g of nano silicon nitride are not added.
Comparative example 2
With reference to example 4, the only difference is that N- [3- (trimethoxysilyl) propyl ] ethylenediamine is not added.
Comparative example 3
Referring to example 2, the only difference was that the compounded material comprised only 99g of polytetrafluoroethylene (particle size of 100 μm), 0.5g of nano-silicon carbide (particle size of 20nm) and 0.5g of nano-silicon nitride (particle size of 30 nm).
Test example
Testing the tensile strength of the polytetrafluoroethylene wear-resistant composite materials prepared in examples 1-6 and comparative examples 1-3 according to the GB/T1040.2-2006 standard;
testing the elongation at break of the polytetrafluoroethylene wear-resistant composite materials prepared in examples 1-6 and comparative examples 1-3 according to the GB/T1040.2-2006 standard;
testing the volume wear rate of the polytetrafluoroethylene wear-resistant composite materials prepared in the examples 1-6 and the comparative examples 1-3 according to the GB/T3960-2016 standard;
testing the compression deformation rate of the polytetrafluoroethylene wear-resistant composite materials prepared in the examples 1-6 and the comparative examples 1-3 according to the GB/T15048-1994 standard;
the test results are shown in table 1:
TABLE 1 Performance test results of the polytetrafluoroethylene abrasion-resistant composite materials prepared in examples 1-6 and comparative examples 1-3
Figure BDA0003233302270000101
As can be seen from table 1, by comparing example 2 with comparative example 1, it can be found that the increase of the polytetrafluoroethylene tensile strength, elongation at break, abrasion resistance and creep resistance can be simultaneously achieved by filling a small amount of the inorganic nanofiller; by comparing example 2 with example 5, it can be found that reducing the particle size of the filled polyimide, the abrasion resistance and compression set are slightly reduced, but the tensile strength and elongation at break of the material can be significantly improved; by comparing example 2 with example 6, it can be found that the tensile strength, elongation at break and wear resistance of the material can be significantly improved by reducing the particle size of the filled tin bronze powder; by comparing example 4 with comparative example 2, it can be seen that the tensile strength and abrasion resistance of the material can be remarkable by performing surface treatment on the inorganic nano-filler and the glass fiber; by comparing the example 2 with the comparative example 3, the improvement of the bearing and abrasion resistance of the polytetrafluoroethylene material by filling a small amount of the inorganic nano-filler is limited, and the improvement effect is better by combining the inorganic nano-filler and other fillers in a composite filling manner with the comparative example 1.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (7)

1. The polytetrafluoroethylene composite material is characterized by comprising the following preparation raw materials in parts by weight:
60-70 parts of polytetrafluoroethylene resin;
20-30 parts of tin bronze powder;
5-10 parts of polyimide;
1-5 parts of glass fiber;
1-5 parts of graphite;
0.5-2 parts of inorganic nano filler;
0.05-0.2 part of a coupling agent;
the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are micron-sized;
the coupling agent comprises trimethoxy silane N- [3- (trimethoxysilyl) propyl ] ethylenediamine and/or 3-aminopropyl triethoxysilane;
the particle size of the polytetrafluoroethylene resin is 50-100 mu m;
the particle size of the tin bronze powder is 1-2 mu m;
the particle size of the polyimide is 38-45 mu m;
the diameter of the glass fiber is 8-14 μm, and the length-diameter ratio is (8-10): 1;
the particle size of the graphite is 1-10 mu m;
the inorganic nano filler comprises one or more of nano silicon carbide, nano silicon nitride and nano silicon dioxide;
the particle size of the inorganic nano filler is 15-40 nm.
2. The polytetrafluoroethylene composite according to claim 1 wherein said tin bronze powder is designated 663.
3. A method for preparing a polytetrafluoroethylene composite as set forth in claim 1 or 2, comprising the steps of:
mixing a coupling agent, inorganic nano-filler, glass fiber, polytetrafluoroethylene resin, polyimide, graphite, tin bronze powder and absolute ethyl alcohol to obtain a mixture;
pressing and forming the mixture to obtain a blank;
sintering the blank to obtain the polytetrafluoroethylene composite material;
the particle sizes of the polytetrafluoroethylene resin, the tin bronze powder, the polyimide, the glass fiber and the graphite are in a micron order.
4. The method according to claim 3, wherein the mass ratio of the coupling agent to the absolute ethyl alcohol is 1: (2000-4000).
5. The production method according to claim 3, wherein the press-molding includes a forward press and an inverted press which are performed in this order;
the pressure of the forward pressing is 15-25 MPa, and the pressure maintaining time is 1-6 min;
the pressure of the inverted pressing is 30-50 MPa, and the pressure maintaining time is 5-8 min.
6. The method of claim 3, wherein the sintering comprises: after the temperature is increased from room temperature to 270-280 ℃ at the heating rate of 3-5 ℃/min and is preserved for 20-40 min, the temperature is increased from 270-280 ℃ to 325-345 ℃ at the heating rate of 1-2 ℃/min and is preserved for 20-40 min, then the temperature is increased from 325-345 ℃ to 360-365 ℃ at the heating rate of 1-2 ℃/min and is preserved for 100-200 min, then the temperature is reduced from 360-365 ℃ to 270-280 ℃ at the cooling rate of 0.5-1 ℃/min and is preserved for 150-200 min, and the furnace cooling is carried out.
7. Use of the polytetrafluoroethylene composite material according to claim 1 or 2 or the polytetrafluoroethylene composite material prepared by the preparation method according to any one of claims 3 to 6 in the field of lubrication and sealing.
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CN114907656B (en) * 2022-05-13 2023-02-17 中国科学院兰州化学物理研究所 Antistatic polytetrafluoroethylene sealing material and preparation method thereof
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