CN111286196B - Self-lubricating fabric liner composite material and preparation method and application thereof - Google Patents

Self-lubricating fabric liner composite material and preparation method and application thereof Download PDF

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CN111286196B
CN111286196B CN202010181690.0A CN202010181690A CN111286196B CN 111286196 B CN111286196 B CN 111286196B CN 202010181690 A CN202010181690 A CN 202010181690A CN 111286196 B CN111286196 B CN 111286196B
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self
temperature
lubricating
fabric liner
composite material
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CN111286196A (en
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王廷梅
段春俭
王齐华
陶立明
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
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    • B32B15/088—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyamides
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    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
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    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1057—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain
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    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
    • D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
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    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • B32B2255/02—Coating on the layer surface on fibrous or filamentary layer
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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Abstract

The invention provides a self-lubricating fabric liner composite material and a preparation method and application thereof, belonging to the technical field of self-lubricating materials. The invention utilizes the low-temperature lubrication characteristic of the polytetrafluoroethylene, takes the polytetrafluoroethylene as a low-temperature solid lubricant, and provides lubrication for the self-lubricating fabric liner under the condition of low temperature (-200 ℃); meanwhile, the multi-walled carbon nanotube is used as a medium-high temperature lubricant by utilizing the good bearing capacity and the lubricating property of the multi-walled carbon nanotube under the high temperature condition, so that the lubricating property of the self-lubricating fabric liner below 400 ℃ is ensured. According to the invention, the nano polytetrafluoroethylene and the multi-walled carbon nano tube are used as solid lubricants at different temperature sections, and the polyimide with a specific structure is simultaneously used as a binder under the synergistic effect of the nano polytetrafluoroethylene and the multi-walled carbon nano tube, so that the self-lubricating fabric liner composite material is endowed with excellent high-temperature and low-temperature resistant lubricating characteristics, and the self-lubricating fabric liner composite material suitable for high-temperature and low-temperature heavy load conditions is obtained.

Description

Self-lubricating fabric liner composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of self-lubricating materials, in particular to a self-lubricating fabric liner composite material and a preparation method and application thereof.
Background
The lubricating technology is one of key technologies for ensuring safe and reliable operation of space vehicles and aircrafts, and the space lubricating material and the technology are directly related to success or failure of space engineering, and have important influence on the service life under effective load. The ambient temperature of the spacecraft will typically vary from-150 c to 150 c. Such as infrared or far infrared detectors, liquid oxygen pumps and liquid hydrogen pumps, operate at ultra-low temperatures. In an operation and control system of an aerospace engine, a large number of low-speed oscillating joint bearings work under dynamic high-temperature/low-temperature alternating and heavy-load conditions, the performance of the oscillating joint bearings is very critical to the overall performance of the spacecraft, and the service life and the reliability of the oscillating joint bearings need to be continuously improved. The bearings are often lubricated with grease due to the high and low temperature environment. However, the working temperature range of the lubricating grease is generally-20-120 ℃, and the structure of the lubricating grease can be damaged at an accelerated speed at an excessively high temperature, so that the service life of the lubricating grease is shortened, the lubricating condition is damaged, the abrasion of a bearing is increased, and the torque is increased; too low a temperature causes the coefficient of friction between the friction pairs to increase and the torque to increase.
Based on the above analysis, the grease is difficult to satisfy the lubrication requirements of the knuckle bearing under the environment conditions of-150 ℃ to 150 ℃ or even more severe. However, the self-lubricating fabric liner can provide excellent high and low temperature resistance by the selectivity of the self-binder and the compound optimization mode of various solid lubricants, has good self-lubricating and wear-resisting characteristics, and more importantly has a longer storage period. At present, although there are reports on self-lubricating fabric liners, most emphasis is placed on formulation optimization of various solid lubricants, and little attention is paid to binder selection. For example, the adhesives disclosed in patent publications CN 109837132 a and CN105367993A are both phenolic resins. The phenolic resin is widely used as a binder due to excellent heat resistance, and the binding performance of the phenolic resin is reduced after the phenolic resin is subjected to high-temperature and low-temperature circulation (-50-200 ℃), so that lubrication failure is caused.
Disclosure of Invention
The invention aims to provide a self-lubricating fabric liner 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 preparation method of a self-lubricating fabric liner composite material, which comprises the following steps:
mixing 3, 4' -diaminodiphenyl ether, 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane, an organic aprotic solvent and pyromellitic dianhydride, and carrying out a polymerization reaction to obtain a polyamic acid solution;
mixing the polyamic acid solution with nano polytetrafluoroethylene and multi-walled carbon nanotubes, and dispersing to obtain an impregnation solution;
coating the impregnation liquid on the surface of the blended fiber cloth to obtain a composite fabric;
and curing and molding the composite fabric to obtain the self-lubricating fabric liner composite material.
Preferably, the molar ratio of the 3, 4' -diaminodiphenyl ether to the 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane is (1-9): 1;
the ratio of the molar amount of pyromellitic dianhydride to the total molar amount of 3, 4' -diaminodiphenyl ether and 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane is 1: 1.
Preferably, the organic aprotic solvent is N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide; the solid content of the polyamic acid solution is 15-20%.
Preferably, the polymerization reaction is carried out in a nitrogen atmosphere, the temperature of the polymerization reaction is room temperature, and the time of the polymerization reaction is 12-36 hours.
Preferably, the particle size of the nano polytetrafluoroethylene is 10-60 nm, and the mass of the nano polytetrafluoroethylene is 8-25% of that of the polyimide matrix in the self-lubricating fabric liner composite material;
the mass of the multi-wall carbon nano tube is 0.5-2.8% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
Preferably, the dispersion is carried out in a high-speed dispersion emulsifying machine, and the rotation speed of the dispersion is 10000-21000 r/min.
Preferably, the blended fiber cloth is blended cloth blended by polytetrafluoroethylene fibers and poly (p-phenylene terephthalamide) fibers according to equal weight, and the thickness of the blended fiber cloth is 0.05-1 mm;
and coating the impregnation liquid on the surface of the blended fiber cloth until the weight of the blended fiber cloth is increased by 30-65%.
Preferably, the pressure of the curing molding is 0.01-3 MPa, and the curing molding process is to heat the temperature from room temperature to 80-250 ℃, preserve heat for 0.5-8 h, then heat the temperature to 300-350 ℃, and preserve heat for 1-3 h.
The invention provides the self-lubricating fabric liner composite material prepared by the preparation method in the technical scheme.
The invention provides application of the self-lubricating fabric liner composite material in an environment with high-low temperature heavy-load conditions.
The invention provides a preparation method of a self-lubricating fabric liner composite material, which comprises the following steps: mixing 3, 4' -diaminodiphenyl ether, 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane, an organic aprotic solvent and pyromellitic dianhydride, and carrying out a polymerization reaction to obtain a polyamic acid solution; mixing the polyamic acid solution with nano polytetrafluoroethylene and multi-walled carbon nanotubes, and dispersing to obtain an impregnation solution; coating the impregnation liquid on the surface of the blended fiber cloth to obtain a composite fabric; and curing and molding the composite fabric to obtain the self-lubricating fabric liner composite material. The invention utilizes the low-temperature lubrication characteristic of the polytetrafluoroethylene, takes the polytetrafluoroethylene as a low-temperature solid lubricant, and provides lubrication for the self-lubricating fabric liner under the condition of low temperature (-200 ℃); meanwhile, the multi-walled carbon nanotube is used as a medium-high temperature lubricant by utilizing the good bearing capacity and the lubricating property of the multi-walled carbon nanotube under the high temperature condition, so that the lubricating property of the self-lubricating fabric liner below 400 ℃ is ensured. According to the invention, the nano polytetrafluoroethylene and the multi-walled carbon nano tube are used as solid lubricants at different temperature sections, and the polyimide with a specific structure is simultaneously used as a binder under the synergistic effect of the nano polytetrafluoroethylene and the multi-walled carbon nano tube, so that the self-lubricating fabric liner composite material is endowed with excellent high-temperature and low-temperature resistant lubricating characteristics, and the self-lubricating fabric liner composite material suitable for high-temperature and low-temperature heavy load conditions is obtained.
Drawings
FIG. 1 is an SEM image of a multi-walled carbon nanotube used in the present invention;
FIG. 2 is a TEM image of a multi-walled carbon nanotube used in the present invention;
FIG. 3 is a surface topography of a sample of the self-lubricating fabric liner composite prepared in example 2 after peel strength testing.
Detailed Description
The invention provides a preparation method of a self-lubricating fabric liner composite material, which comprises the following steps:
mixing 3, 4' -diaminodiphenyl ether, 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane, an organic aprotic solvent and pyromellitic dianhydride, and carrying out a polymerization reaction to obtain a polyamic acid solution;
mixing the polyamic acid solution with nano polytetrafluoroethylene and multi-walled carbon nanotubes, and dispersing to obtain an impregnation solution;
coating the impregnation liquid on the surface of the blended fiber cloth to obtain a composite fabric;
and curing and molding the composite fabric to obtain the self-lubricating fabric liner composite material.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The preparation method comprises the steps of mixing 3, 4' -diaminodiphenyl ether, 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane, an organic aprotic solvent and pyromellitic dianhydride, and carrying out polymerization reaction to obtain a polyamic acid solution. In the present invention, the molar ratio of the 3, 4' -diaminodiphenyl ether to 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane is preferably (1-9): 1, more preferably (3-8): 1, and still more preferably (5-6): 1. In the present invention, the ratio of the molar amount of pyromellitic dianhydride to the total molar amount of 3, 4' -diaminodiphenyl ether and 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane is preferably 1: 1. In the invention, the 3, 4' -diaminodiphenyl ether has good flexibility, the 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane has good bonding performance with metal, the polyimide prepared by polymerizing and curing the two diamines and pyromellitic dianhydride has excellent high and low temperature resistance, the polyimide with the structure not only has excellent high and low temperature resistance (-200-400 ℃) performance, outstanding thermal stability, unique self-lubricating property, but also has excellent bonding performance, and the polyimide plays a bonding role in a composite material.
In the present invention, the organic aprotic solvent is preferably N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide; the solid content of the polyamic acid solution is preferably 15-20%, and more preferably 16-18%.
In the invention, the mixing process preferably comprises the steps of mixing the 3, 4' -diaminodiphenyl ether, the 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane and the organic aprotic solvent, stirring the mixture at room temperature under a dry nitrogen atmosphere until the mixture is completely dissolved to obtain a diamine solution, and then adding the pyromellitic dianhydride into the diamine solution in 5-10 batches.
In the invention, the polymerization reaction is preferably carried out in a nitrogen atmosphere, the temperature of the polymerization reaction is preferably room temperature, and the time of the polymerization reaction is preferably 12-36 h, more preferably 15-30 h, and further preferably 24-30 h; the polymerization reaction is preferably carried out under stirring conditions, and the stirring process is not particularly limited in the invention, and processes well known in the art can be selected to ensure that the reaction is smoothly carried out.
After the polyamic acid solution is obtained, the polyamic acid solution is mixed with the nano polytetrafluoroethylene and the multi-walled carbon nano tubes and dispersed to obtain the impregnation liquid. In the invention, the particle size of the nano polytetrafluoroethylene is preferably 10-60 nm, more preferably 30-50 nm, the mass of the nano polytetrafluoroethylene is preferably 8-25%, more preferably 10-20%, and even more preferably 15% of the polyimide matrix in the self-lubricating fabric liner composite material, the mass fractions are based on the polyimide matrix in the finally formed self-lubricating fabric liner material, and the mass of imidization and dehydration in the imidization process during curing and forming is neglected in the calculation process of the mass fractions. In the invention, the mass of the multi-wall carbon nano tube is preferably 0.5-2.8% of that of the polyimide matrix in the self-lubricating fabric liner composite material, more preferably 1.0-2.5%, and further preferably 1.5-2.0%; the specification of the multi-walled carbon nanotube is not particularly limited, and a commercially available product known in the art may be selected. In the invention, the topography of the multi-walled carbon nanotube is shown in fig. 1-2, the outer diameter of the carbon nanotube is from several nanometers to dozens of nanometers, the inner diameter of the tube is small, the length is micron-sized, and the length-diameter ratio is very large and can reach 103-106. The mixing process is not particularly limited, and the nano polytetrafluoroethylene and the multi-walled carbon nano tubes are directly added into the polyamic acid solution.
In the invention, the nano polytetrafluoroethylene has excellent low-temperature lubricating property, and can provide lubrication for the self-lubricating fabric liner under the condition of low temperature (less than-200 ℃). In the invention, the multi-walled carbon nanotube has excellent high-temperature lubricating property, provides good load for the self-lubricating fabric liner, and under a heavy load condition, the reciprocating stress promotes the carbon nanotube to be partially cut, namely the outer carbon nanotube is cut, and the inner carbon nanotube is kept in a perfect state, which shows that the carbon nanobelts which are partially cut wrap the nanotubes which are not cut, wherein the carbon nanobelts (namely the multi-layer graphene or graphite) can ensure the lubricating property of the self-lubricating fabric liner below 400 ℃. The invention realizes the heavy-load high-low temperature lubrication of the self-lubricating fabric liner composite material by utilizing the nano polytetrafluoroethylene and the multi-walled carbon nano tube. When room-temperature and high-temperature lubrication is needed, the multi-walled carbon nanotube can show excellent lubricating performance under the high-temperature condition. And when the temperature is low, the polytetrafluoroethylene can show excellent lubricating performance.
In the invention, the dispersion is preferably carried out in a high-speed dispersion emulsifying machine, and the rotation speed of the dispersion is preferably 10000-21000 r/min, more preferably 15000-20000 r/min. In the dispersion process, the polyamic acid solution is uniformly mixed with the nano polytetrafluoroethylene and the multi-walled carbon nano tubes to obtain the impregnation liquid.
After the impregnation liquid is obtained, the impregnation liquid is coated on the surface of the blended fiber cloth to obtain the composite fabric. In the invention, the blended fiber cloth is preferably blended cloth blended by polytetrafluoroethylene fibers and poly (p-phenylene terephthamide) fibers according to equal weight, and the thickness of the blended fiber cloth is preferably 0.05-1 mm, more preferably 0.1-0.8 mm, and further preferably 0.5-0.6 mm. The source of the blended fiber cloth is not particularly limited, and the blended fiber cloth can be prepared according to the specification by adopting a method well known in the field.
Before the impregnation liquid is coated on the surface of the blended fiber cloth, the blended fiber cloth is preferably pretreated, and the pretreatment method is preferably to impregnate the blended fiber cloth into a solvent for 60min and then dry the blended fiber cloth in a blast oven at 100 ℃ for 24 h; the solvent is preferably a mixed solution of 3, 4-dihydroxyphenylethylamine, tris (hydroxymethyl) aminomethane and deionized water, the mass ratio of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane is preferably 4:3, and the mass ratio of the total mass of the 3, 4-dihydroxyphenylethylamine and the tris (hydroxymethyl) aminomethane to water is preferably 1: 10. the specific dosage of the solvent is not specially limited, and the blended fiber cloth can be completely soaked. The invention improves the sizing amount of the fiber surface by pretreating the blended fiber cloth and prevents the impregnation liquid from further penetrating so as to influence the bonding property of the self-lubricating fabric liner material and the substrate.
According to the invention, the impregnation liquid is coated on the surface of the blended fiber cloth preferably repeatedly for multiple times until the weight of the blended fiber cloth is increased by 30-65%, more preferably 35-60%, and further preferably 40-55%. In the process of multiple coating repetitions, the present invention preferably dries the coated fabric once per coating, and then applies the next coating until the target weight gain is achieved. In the invention, the drying temperature is preferably 80-100 ℃, the drying time is preferably 8-10 h, and the drying is preferably carried out in a forced air oven. The invention has no special limitation on the coating amount of single coating, and can ensure that the dipping solution is uniformly coated and the weight is increased for multiple times. In the invention, the impregnation liquid is coated on the surface of the blended fiber cloth to form a single-side coating, and the non-coating side of the blended fiber cloth is adhered to the surface of the bearing substrate. The coating method of the present invention is not particularly limited, and may be performed by a method known in the art.
After the composite fabric is obtained, the invention carries out curing molding on the composite fabric to obtain the self-lubricating fabric liner composite material. In the invention, the pressure for curing molding is preferably 0.01-3 MPa, the process for curing molding is preferably to be heated from room temperature to 80-250 ℃ (more preferably 100-200 ℃, and further preferably 120-160 ℃), to be kept warm for 0.5-8 h (more preferably 2-6 h, and further preferably 3-5 h), then to be heated to 300-350 ℃ (more preferably 320-340 ℃, and further preferably 330 ℃), to be kept warm for 1-3 h (more preferably 1.5-2.5 h); the temperature rise rate of the two temperature rises is 5-10 ℃/min independently, and more preferably 6-8 ℃/min. In the process of curing and forming, polyamic acid in the impregnation liquid is imidized to generate polyimide, and the self-lubricating fabric liner composite material is finally prepared and contains polyimide, nano polytetrafluoroethylene and multi-wall carbon nano tubes.
In order to test the performance of the self-lubricating fabric liner composite material, in the embodiment of the present invention, before performing curing molding, the present invention preferably uses the polyamic acid solution prepared by the above technical scheme to stick the composite fabric on the surface of the metal substrate, and then applies pressure and heats up to perform curing molding. In an embodiment of the invention, the metal substrate is preferably a titanium alloy, 304 steel, aluminium or bearing steel, the dimensions of the metal substrate preferably being 18 x 2 mm. The process of the present invention is not particularly limited, and may be any process known in the art.
The invention provides the self-lubricating fabric liner composite material prepared by the preparation method in the technical scheme. The high-low temperature friction coefficient of the self-lubricating fabric liner composite material prepared by the invention is 0.08-0.26, and the maximum peel strength is more than or equal to 2.8 KN/m.
The invention provides application of the self-lubricating fabric liner composite material in an environment with high-low temperature heavy-load conditions. The method for applying the self-lubricating fabric liner composite material is not particularly limited, and the method well known in the field can be selected, and the self-lubricating fabric liner composite material can be adhered to the surface of the metal knuckle bearing lining.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
In the following examples, the particle size of the nano polytetrafluoroethylene is 10 to 60nm, and the blended fiber cloth is blended cloth blended by polytetrafluoroethylene fibers and poly (p-phenylene terephthalamide) fibers according to equal weight.
Example 1
Mixing 32mmol (6.41g) of 3, 4' -diaminodiphenyl ether and 8mmol (1.99g) of 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane with 97g N-methyl pyrrolidone, stirring at room temperature under a dry nitrogen atmosphere until the mixture is completely dissolved to obtain a diamine solution, then adding 40mmol (8.72g) of pyromellitic dianhydride into the diamine solution in 5 batches, stirring at room temperature under a nitrogen atmosphere for 36 hours, and carrying out polymerization reaction to obtain a polyamic acid solution (the solid content is 15%);
adding 3.42g of nano polytetrafluoroethylene and 0.085g of multi-walled carbon nano tube into the polyamic acid solution, and uniformly mixing in a high-speed dispersion emulsifying machine at the speed of 10000r/min to obtain an impregnation solution;
soaking the blended fiber cloth (with the thickness of 1mm) in a solvent for 60min, and then drying in a blast oven at 100 ℃ for 24 h; the solvent is a mixed solution of 3, 4-dihydroxyphenylethylamine, tris (hydroxymethyl) aminomethane and deionized water, the mass ratio of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane is 4:3, and the mass ratio of the total mass of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane to water is 1: 10; obtaining pretreated blend fiber cloth;
coating the impregnation liquid on the single-side surface of the pretreated blended fiber cloth, then moving the cloth to a blast oven at 100 ℃ for drying for 8h, and repeating the coating-drying process for several times until the weight of the blended fiber cloth is increased by 30%, thus obtaining a composite fabric;
the prepared polyamic acid solution is used for sticking the composite fabric on the surface of a titanium alloy substrate (with the size of 18 multiplied by 2mm), and the pressure of 0.01MPa is applied, the temperature is raised to 80 ℃ from the room temperature at the speed of 10 ℃/min, the temperature is kept for 8h, then the temperature is raised to 350 ℃ at the same speed, the temperature is kept for 1h, and the self-lubricating fabric liner composite material is obtained; the mass of the nano polytetrafluoroethylene is 20% of that of the polyimide matrix in the self-lubricating fabric liner composite material, and the mass of the multi-wall carbon nano tube is 0.5% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
Example 2
Mixing 20mmol (4.00g) of 3, 4' -diaminodiphenyl ether and 20mmol (4.96g) of 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane with 100g N-methylpyrrolidone, stirring at room temperature under a dry nitrogen atmosphere until the mixture is completely dissolved to obtain a diamine solution, then adding 40mmol (8.72g) of pyromellitic dianhydride into the diamine solution in 10 batches, stirring at room temperature under a nitrogen atmosphere for 24 hours, and carrying out polymerization reaction to obtain a polyamic acid solution (the solid content is 15%);
adding 4.42g of nano polytetrafluoroethylene and 0.0884g of multi-walled carbon nanotubes into the polyamic acid solution, and uniformly mixing in a high-speed dispersion emulsifying machine at the speed of 15000r/min to obtain an impregnation solution;
soaking the blended fiber cloth (with the thickness of 0.05mm) in a solvent for 60min, and then drying in a blast oven at 100 ℃ for 24 h; the solvent is a mixed solution of 3, 4-dihydroxyphenylethylamine, tris (hydroxymethyl) aminomethane and deionized water, the mass ratio of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane is 4:3, and the mass ratio of the total mass of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane to water is 1: 10; obtaining pretreated blend fiber cloth;
coating the impregnation liquid on the single-side surface of the pretreated blended fiber cloth, then moving the cloth to a blast oven at 100 ℃ for drying for 10 hours, and repeating the coating-drying process for several times until the weight of the blended fiber cloth is increased by 50%, so as to obtain a composite fabric;
the prepared polyamic acid solution is used for sticking the composite fabric on the surface of a bearing steel substrate (the size is 18 multiplied by 2mm), applying pressure of 3MPa, heating to 250 ℃ from room temperature at the speed of 5 ℃/min, preserving heat for 0.5h, then heating to 300 ℃ at the same speed, preserving heat for 1h, and obtaining the self-lubricating fabric liner composite material; the mass of the nano polytetrafluoroethylene is 25% of that of the polyimide matrix in the self-lubricating fabric liner composite material, and the mass of the multi-wall carbon nano tube is 0.5% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
Example 3
Mixing 36mmol (7.21g) of 3, 4' -diaminodiphenyl ether and 4mmol (1.00g) of 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane with 68g N-methylpyrrolidone, stirring at room temperature under a dry nitrogen atmosphere until the mixture is completely dissolved to obtain a diamine solution, then adding 40mmol (8.72g) of pyromellitic dianhydride into the diamine solution in 8 batches, stirring at room temperature under a nitrogen atmosphere for 12 hours, and carrying out polymerization reaction to obtain a polyamic acid solution (the solid content is 20%);
4.2325g of nano polytetrafluoroethylene and 0.4740g of multi-walled carbon nano tubes are added into the polyamic acid solution and are uniformly mixed in a high-speed dispersion emulsifying machine at the speed of 21000r/min to obtain an impregnation solution;
soaking the blended fiber cloth (with the thickness of 1mm) in a solvent for 60min, and then drying in a blast oven at 100 ℃ for 24 h; the solvent is a mixed solution of 3, 4-dihydroxyphenylethylamine, tris (hydroxymethyl) aminomethane and deionized water, the mass ratio of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane is 4:3, and the mass ratio of the total mass of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane to water is 1: 10; obtaining pretreated blend fiber cloth;
coating the impregnation liquid on the single-side surface of the pretreated blended fiber cloth, then moving the cloth to a blast oven at 80 ℃ for drying for 10 hours, and repeating the coating-drying process for several times until the weight of the blended fiber cloth is increased by 65%, thus obtaining a composite fabric;
the prepared polyamic acid solution is used for sticking the composite fabric on the surface of a 304 steel substrate (the size is 18 multiplied by 2mm), and the pressure of 0.01MPa is applied, the temperature is raised to 80 ℃ from the room temperature at the speed of 5 ℃/min, the temperature is kept for 8h, then the temperature is raised to 350 ℃ at the same speed, the temperature is kept for 1h, and the self-lubricating fabric liner composite material is obtained; the mass of the nano polytetrafluoroethylene is 25% of that of the polyimide matrix in the self-lubricating fabric liner composite material, and the mass of the multi-wall carbon nano tube is 2.8% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
Example 4
Mixing 20mmol (4.00g) of 3, 4' -diaminodiphenyl ether and 20mmol (4.96g) of 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane with 100g N-methyl pyrrolidone, stirring at room temperature under a dry nitrogen atmosphere until the mixture is completely dissolved to obtain a diamine solution, then adding 40mmol (8.72g) of pyromellitic dianhydride into the diamine solution in 6 batches, stirring at room temperature under a nitrogen atmosphere for 24 hours, and carrying out polymerization reaction to obtain a polyamic acid solution (the solid content is 15%);
1.4144g of nano polytetrafluoroethylene and 0.4950g of multi-walled carbon nano tubes are added into the polyamic acid solution and are uniformly mixed in a high-speed dispersion emulsifying machine at the speed of 10000r/min to obtain an impregnation solution;
soaking the blended fiber cloth (with the thickness of 1mm) in a solvent for 60min, and then drying in a blast oven at 100 ℃ for 24 h; the solvent is a mixed solution of 3, 4-dihydroxyphenylethylamine, tris (hydroxymethyl) aminomethane and deionized water, the mass ratio of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane is 4:3, and the mass ratio of the total mass of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane to water is 1: 10; obtaining pretreated blend fiber cloth;
coating the impregnation liquid on the single-side surface of the pretreated blended fiber cloth, then moving the cloth to a blast oven at 100 ℃ for drying for 10 hours, and repeating the coating-drying process for several times until the weight of the blended fiber cloth is increased by 30%, so as to obtain a composite fabric;
the prepared polyamic acid solution is used for sticking the composite fabric on the surface of a 304 steel substrate (the size is 18 multiplied by 2mm), applying pressure of 3MPa, heating to 80 ℃ from room temperature at the speed of 5 ℃/min, preserving heat for 8h, then heating to 350 ℃ at the same speed, preserving heat for 1h, and obtaining the self-lubricating fabric liner composite material; the mass of the nano polytetrafluoroethylene is 8% of that of the polyimide matrix in the self-lubricating fabric liner composite material, and the mass of the multi-walled carbon nanotube is 2.8% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
Example 5
Mixing 36mmol (7.21g) of 3, 4' -diaminodiphenyl ether and 4mmol (1.00g) of 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane with 68g N-methylpyrrolidone, stirring at room temperature under a dry nitrogen atmosphere until the mixture is completely dissolved to obtain a diamine solution, then adding 40mmol (8.72g) of pyromellitic dianhydride into the diamine solution in 5 batches, stirring at room temperature under a nitrogen atmosphere for 12 hours, and carrying out polymerization reaction to obtain a polyamic acid solution (the solid content is 20%);
4.2325g of nano polytetrafluoroethylene and 0.0846g of multi-walled carbon nanotubes are added into the polyamic acid solution and are uniformly mixed in a high-speed dispersion emulsifying machine at the speed of 18000r/min to obtain an impregnation solution;
soaking the blended fiber cloth (with the thickness of 0.05mm) in a solvent for 60min, and then drying in a blast oven at 100 ℃ for 24 h; the solvent is a mixed solution of 3, 4-dihydroxyphenylethylamine, tris (hydroxymethyl) aminomethane and deionized water, the mass ratio of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane is 4:3, and the mass ratio of the total mass of the 3, 4-dihydroxyphenylethylamine to the tris (hydroxymethyl) aminomethane to water is 1: 10; obtaining pretreated blend fiber cloth;
coating the impregnation liquid on the single-side surface of the pretreated blended fiber cloth, then moving the cloth to a blast oven at 100 ℃ for drying for 10 hours, and repeating the coating-drying process for several times until the weight of the blended fiber cloth is increased by 65%, thus obtaining a composite fabric;
the prepared polyamic acid solution is used for sticking the composite fabric on the surface of a 304 steel substrate (the size is 18 multiplied by 2mm), and the pressure of 0.01MPa is applied, the temperature is raised to 80 ℃ from the room temperature at the speed of 5 ℃/min, the temperature is kept for 8h, then the temperature is raised to 350 ℃ at the same speed, the temperature is kept for 2h, and the self-lubricating fabric liner composite material is obtained; the mass of the nano polytetrafluoroethylene is 25% of that of the polyimide matrix in the self-lubricating fabric liner composite material, and the mass of the multi-wall carbon nano tube is 0.5% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
Comparative example 1
The only difference from example 3 is that: the process of adding nano polytetrafluoroethylene and multi-walled carbon nano tubes to prepare the dipping solution is not included, and the polyamic acid solution is directly coated on the surface of the pretreated blended fiber cloth.
Characterization and performance testing:
1) fig. 1 is an SEM image of a multi-walled carbon nanotube used in the present invention, and fig. 2 is a TEM image of a multi-walled carbon nanotube used in the present invention, and it can be seen from the figure that the multi-walled carbon nanotube used in the present invention has a hollow structure, an inner diameter of about 10nm, and an outer diameter of about 40 nm.
2) According to the method described in GB2790-1995, the self-lubricating fabric liner composite materials prepared in examples 1-3 and comparative example 1 are subjected to a peel strength test, a ball-disc high-low temperature friction machine is used for a friction test under a special working condition, and the dual selection is the GCr15 material; the metal matrix is bearing steel;
friction test conditions: the load is 20N, the linear velocity is 0.1m/s, and the diameter of the dual ball is 3 mm; the friction coefficient was repeated a minimum of three times and averaged, and the results are shown in table 1.
TABLE 1 Friction coefficient and Peel Strength data for composites prepared in examples 1-3 and comparative example 1
Figure BDA0002412746930000111
Figure BDA0002412746930000121
As can be seen from table 1, the composite materials of examples 1 to 3 include polyimide, nano polytetrafluoroethylene and multi-walled carbon nanotubes, while the fabric material of comparative example 1 only includes polyimide, and no polytetrafluoroethylene or multi-walled carbon nanotubes are added, so that the self-lubricating fabric liner composite material prepared in the examples has more excellent wear resistance, and the friction coefficient of the composite material can meet the high and low temperature lubricating performance under different high and low temperature conditions; meanwhile, polyimide is used as an adhesive, so that the maximum peel strength is high, and high-temperature and low-temperature lubrication of the self-lubricating fabric liner can be realized.
3) The sample of the self-lubricating fabric liner composite material prepared in example 2 after the peel strength test is characterized, the surface topography is shown in fig. 3, and as can be seen from fig. 3, the polyimide adhesive used in the invention has high bonding strength with the bearing steel matrix, even if 50% of impregnation liquid is coated on the surface of the blended fiber cloth. In addition, under the action of the tensile force, part of the fiber fabric still remains on the surface of the metal matrix, which indicates that the peel strength is high.
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 (10)

1. A method of making a self-lubricating fabric liner composite, comprising the steps of:
mixing 3, 4' -diaminodiphenyl ether, 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane, an organic aprotic solvent and pyromellitic dianhydride, and carrying out a polymerization reaction to obtain a polyamic acid solution;
mixing the polyamic acid solution with nano polytetrafluoroethylene and multi-walled carbon nanotubes, and dispersing to obtain an impregnation solution;
coating the impregnation liquid on the surface of the blended fiber cloth to obtain a composite fabric;
and curing and molding the composite fabric to obtain the self-lubricating fabric liner composite material.
2. The method according to claim 1, wherein the molar ratio of 3, 4' -diaminodiphenyl ether to 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane is (1-9: 1;
the ratio of the molar amount of pyromellitic dianhydride to the total molar amount of 3, 4' -diaminodiphenyl ether and 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane is 1: 1.
3. The production method according to claim 1, wherein the organic aprotic solvent is N-methylpyrrolidone, N-dimethylformamide, or N, N-dimethylacetamide; the solid content of the polyamic acid solution is 15-20%.
4. The method according to claim 1, wherein the polymerization reaction is carried out under a nitrogen atmosphere, the temperature of the polymerization reaction is room temperature, and the time of the polymerization reaction is 12 to 36 hours.
5. The preparation method of claim 1, wherein the particle size of the nano polytetrafluoroethylene is 10-60 nm, and the mass of the nano polytetrafluoroethylene is 8-25% of that of the polyimide matrix in the self-lubricating fabric liner composite material;
the mass of the multi-wall carbon nano tube is 0.5-2.8% of that of the polyimide matrix in the self-lubricating fabric liner composite material.
6. The method according to claim 1, wherein the dispersion is carried out in a high-speed dispersion emulsifier at 10000 to 21000 r/min.
7. The preparation method according to claim 1, wherein the blended fiber cloth is blended cloth blended by polytetrafluoroethylene fibers and poly (p-phenylene terephthalamide) fibers according to equal weight, and the thickness of the blended fiber cloth is 0.05-1 mm;
and coating the impregnation liquid on the surface of the blended fiber cloth until the weight of the blended fiber cloth is increased by 30-65%.
8. The preparation method according to claim 1, wherein the pressure of the curing molding is 0.01-3 MPa, and the curing molding process comprises raising the temperature from room temperature to 80-250 ℃ and keeping the temperature for 0.5-8 h, and then raising the temperature to 300-350 ℃ and keeping the temperature for 1-3 h.
9. A self-lubricating fabric liner composite material prepared by the preparation method of any one of claims 1 to 8.
10. Use of the self-lubricating fabric liner composite of claim 9 in an environment with high and low temperature heavy duty conditions.
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CN113389784B (en) * 2021-06-30 2022-03-04 上海大学 Intelligent desolventizing and pressurizing device and method for self-lubricating joint bearing gasket
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