CN106957503A - Polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material and preparation method thereof - Google Patents
Polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material and preparation method thereof Download PDFInfo
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- CN106957503A CN106957503A CN201710167674.4A CN201710167674A CN106957503A CN 106957503 A CN106957503 A CN 106957503A CN 201710167674 A CN201710167674 A CN 201710167674A CN 106957503 A CN106957503 A CN 106957503A
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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
- C08L27/00—Compositions 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
- C08L27/02—Compositions 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
- C08L27/12—Compositions 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
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention provides a kind of polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material and preparation method thereof, the polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material includes polytetrafluoroethylene (PTFE), polyimides and nano silicon, and its mass percent is：19~20% polyimides, 0.01~3% nano silicon, remaining be polytetrafluoroethylene (PTFE), the distribution form of each component is：Polyimides is evenly distributed in poly tetrafluoro ethylene matrix, and nano silicon then completely and is evenly distributed in polyimides.Its preparation method is：It is prepared by step (1) the self-lubricating material mixture；Step (2) the self-lubricating material shaping；Step (3) the self-lubricating material sintering.The features such as present invention has low-friction coefficient, high-wearing feature and preferable structural homogenity, can be applied to the occasions such as ball in self-lubricating knuckle bearing, self-lubricating bushing, self-lubricating machine tool guideway, self-lubricating retainer, with very high application value.
Description
Technical field
The invention belongs to macromolecular material self-lubricating technical field of modification, and in particular to a kind of polytetrafluoroethylene (PTFE)/polyamides is sub-
Amine/nano silicon self-lubricating material and preparation method thereof.
Background technology
Polytetrafluoroethylene (PTFE) has excellent corrosion resistance, heat resistance and self-lubricating property, is widely used in self-lubricating neck
The self-lubricating retainer of ball, self-lubricating bushing, self-lubricating machine tool guideway, rolling bearing in domain, such as self-lubricating knuckle bearing.But
Pure polytetrafluoroethylene (PTFE) mechanical property is relatively low, easy creep, wearability are poor, limits its application in self-lubricating field.
Filling-modified method is capable of the anti-wear performance of effective polytetrafluoroethylene (PTFE), mainly uses filler effectively to suppress
The peeling of polytetrafluoroethylene (PTFE) in friction process, so as to reach the purpose of reduction poly tetrafluoro ethylene matrix abrasion.Polytetrafluoroethylene (PTFE)
It is filling-modified mainly include inoganic particle modified and polymer modification, wherein, inorganic nano-particle be it is inoganic particle modified in compared with
It is effective a kind of, can increase substantially the anti-wear performance of polytetrafluoroethylmaterial material, but inorganic nano-particle easily reunite and with
The compatibility of polytetrafluoroethylene (PTFE) is poor, causes polytetrafluoroethylmaterial material institutional framework uneven, constrains the uniform force of material
Property and its actual application value.《Chinese patent》(application number：201410015514.4) by mix polytetrafluoroethylene (PTFE) and
Ti3SiC2Or Ti3AlC2Prepare ptfe composite, although the wearability of material, but Ti is greatly improved3SiC2
Or Ti3AlC2It is poor with polytetrafluoroethylene (PTFE) compatibility, it is scattered uneven in polytetrafluoroethylene (PTFE), reduce polytetrafluoroethylene (PTFE) material
The structural homogenity of material, has a strong impact on the service life of polytetrafluoroethylmaterial material.Compared with inorganic filler, polymer filler is with gathering
The compatibility of tetrafluoroethene preferably, can obtain the more uniform polytetrafluoroethylmaterial material of institutional framework, but its coefficient of friction is slightly larger.
Polyimides is the polymeric material that self lubricity is only second to polytetrafluoroethylene (PTFE), has the advantages that wearability is good, sub- by polyamides
Amine is modified to polytetrafluoroethylene (PTFE), can significantly improve the wearability of polytetrafluoroethylene (PTFE), but the larger friction system of polyimides
Number, causes the self-lubricating property of polytetrafluoroethylene (PTFE)/composite polyimide material poor.If adding poly- in polytetrafluoroethylene (PTFE) simultaneously
Synergy between compound and nanoparticulate fillers, filler can improve the anti-wear performance of ptfe composite simultaneously
And self-lubricating property, but equally exist inorganic nano-particle and easily reunite and its problem of with polytetrafluoroethylene (PTFE) poor compatibility, lead
Cause polytetrafluoroethylmaterial material institutional framework is uneven, inorganic nano-particle is easily peeled off, so as to weaken polytetrafluoroethylmaterial material
Performance.《Chinese patent》(application number：200510134995.1) a kind of fine powder enhancing polytetrafluoro of polypropylene is disclosed
The filling such as metal and metal oxide, nonmetal oxide, carbide can be added in the preparation method of vinyl material, its component
Thing, improves the dispersiveness and wearability of polytetrafluoroethylene (PTFE), but metallic, nonmetal oxide etc. and poly- four to a certain extent
The compatibility of PVF is poor, causes these fillers to be separated from polytetrafluoroethylene (PTFE), weares and teares to flour milling, makes the coefficient of friction of material
Increase.
At present, many methods modified using coupling agent improve the dispersiveness and its compatibility with polymer of nano-particle,
《Chinese patent》(application number：201210439088.8) by be blended silane coupler modify Nanometer Copper, polytetrafluoroethylene (PTFE) and
Polyimides, is prepared for a kind of preferable composite polyimide material of wearability；In addition,《Chinese patent》(application number：
201110142142.8) expanded graphite, basalt fibre and polytetrafluoro are improved by silane coupler or titanate coupling agent
Compatibility between ethene, poly phenyl ester, prepares a kind of polytetrafluoroethylmaterial material of high-mechanic low-friction coefficient.
Although these inventions improve inorganic filler and the compatibility of polytetrafluoroethylene (PTFE) and polyimides by coupling agent to a certain extent,
The anti-wear performance of composite is improved, but the not basic scattered uneven, nano-particle of nano-particle that solves is reunited and polymer
The poor defect of microstructure of composite structural homogeneity, has had a strong impact on the practicality of composite.
Therefore, while polytetrafluoroethylmaterial material wearability and self lubricity is improved, how inorganic nano-filler is improved
Dispersiveness in polytetrafluoroethylene (PTFE), preparing the polytetrafluoroethylmaterial material of uniform texture turns into urgent problem to be solved, right
There is higher practical value in promoting the application of polytetrafluoroethylmaterial material.
The content of the invention
To solve the above problems, the invention provides a kind of polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating
Material and preparation method thereof, it is intended to while improving polytetrafluoroethylmaterial material self lubricity and wearability, solves existing polytetrafluoro
The problem of vinyl material institutional framework is uneven.
The technical solution adopted for the present invention to solve the technical problems is：A kind of polytetrafluoroethylene (PTFE)/Polyimide/Nano two
Silica self-lubricating material, each group of the material is divided into polytetrafluoroethylene (PTFE), polyimides and nano silicon, its quality hundred
Point ratio is：Polyimides 19~21%, nano silicon 0.01~3%, surplus is polytetrafluoroethylene (PTFE), the distribution shape of each component
Formula is：Polyimides is evenly distributed in poly tetrafluoro ethylene matrix, and nano silicon is complete and is evenly distributed in polyamides
In imines.
The polytetrafluorethylepowder powder particle diameter is 1 μm~100 μm.
The nano silicon is spherical, 1~50nm of particle diameter, and by silane coupler modification.
The polyimides is：By 3,3 ˊ, it is poly- that 4,4 ˊ-oxydiphthalic is synthesized with 4,4 ˊ-diaminodiphenyl ether
Acid imide, particle diameter is 1 μm~74 μm, and contains equally distributed nano silicon in polyimides.
A kind of preparation method of polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material, the preparation method
Comprise the following steps that：
It is prepared by step (1) polytetrafluoroethylmaterial material/Polyimide/Nano silica mixture：
Take 7.7~7.999g polytetrafluorethylepowder powder to be scattered in absolute ethyl alcohol, then add 2.001~2.3g and prepare
Polyimide/Nano SiO 2 powder, 10~60min of magnetic agitation under normal temperature is well mixed, by mixture 80~
Dried at 100 DEG C；
Step (2) polytetrafluoroethylmaterial material/Polyimide/Nano silica shaping：
The mixture that step (1) is obtained obtains polytetrafluoro under normal temperature and 20~40MPa pressure after 5~30min of pressurize
The blank of ethene/Polyimide/Nano earth silicon material；
The sintering of step (3) polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material：
The blank of the polytetrafluoroethylene (PTFE) that step (2) is obtained/Polyimide/Nano earth silicon material is in air atmosphere
Under, with 3~5 DEG C/min heating rate, 50~70min of insulation after 100~120 DEG C is warming up to, then with 1~3 DEG C/min's
Heating rate, is warming up to 50~70min of insulation after 310~330 DEG C, then with 1~3 DEG C/min heating rate, is warming up to 340
100~140min is incubated after~380 DEG C, finally with 1~3 DEG C/min rate of temperature fall, 50 are incubated after being cooled to 310~330 DEG C
~70min, cools to the furnace after room temperature and obtains polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material.
The preparation method of the Polyimide/Nano SiO 2 powder, it is comprised the following steps that：
It is prepared by step (1) nano silicon dioxide dispersion：
Take 0.01~0.3g nano silicons to be put into acetone, 0.001~0.03g silane couplers are added dropwise, magnetic force is stirred
Rear 20~60min of sonic oscillation is mixed, is uniformly dispersed and stable nano silicon dioxide dispersion；
It is prepared by step (2) polyamic acid/nano grade silica particles：
6.00~6.20g 4,4 ˊ-diaminodiphenyl ether are added in the nano silicon dioxide dispersion of step (1), and
40~100min of magnetic agitation at 40~50 DEG C, then adds 9.00~9.50g 3,3 ˊ, 4,4 ˊ-oxydiphthalic,
At room temperature after 3~6h of magnetic agitation, the mixed liquor of generation polyamic acid/nano grade silica particles and acetone；
It is prepared by step (3) Polyimide/Nano SiO 2 powder：
In the polyamic acid/nano silicon and addition triethylamine, acetic anhydride and toluene in acetone mixture of step (2)
(addition of three kinds of raw materials be respectively polyamic acid/nano silicon quality 40~60%, 300~400%, 150~
250%), continue to stir 1~3h, after imidization is complete, after suction filtration, washing, product is dried, and with 1~5 DEG C/min
Heating rate, be incubated 2h after being warming up to 280 DEG C, cool to the furnace after room temperature, cross 200 mesh sieves, obtain Polyimide/Nano two
Silicon oxide powder.
The beneficial effects of the invention are as follows：In the polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material, receive
Rice silica is complete and is evenly distributed in polyimides, first, by the modification of silane coupler, nano silicon
Strengthen with the adhesion of polyimides, and improve dispersiveness of the nano silicon in polyimides；Secondly, polyamic acid
Exist with powder morphology, can effectively suppress the agglomeration of nano silicon, so as to ensure that nano silicon poly-
The uniformity being distributed in acid imide.In addition, because the compatibility of polyimides and polytetrafluoroethylene (PTFE) is preferable, it is ensured that polyimides/
The uniformity that nano grade silica particles disperse in poly tetrafluoro ethylene matrix and its adhesion with poly tetrafluoro ethylene matrix.Cause
This, the preparation method can reduce the reunion of nano silicon and the defect being easily peeled off in composite, use the method system
Standby polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material uniform texture, while having low friction system
The advantages of number, high-wearing feature, it can be applied to ball in self-lubricating knuckle bearing, self-lubricating bushing, self-lubricating machine tool guideway, self-lubricating
The occasions such as rolling bearing retainer, with very high application value.
Brief description of the drawings
Fig. 1 is the system of polytetrafluoroethylene (PTFE) provided in an embodiment of the present invention/Polyimide/Nano silica self-lubricating material
Standby flow chart.
Fig. 2 is the preparation flow figure of Polyimide/Nano SiO 2 powder.
Embodiment
It is an object of the invention to provide a kind of coefficient of friction is small, wearability is high and uniform texture polytetrafluoroethyl-ne
Alkene/Polyimide/Nano silica self-lubricating material and preparation method thereof, the key component of the material is polytetrafluoroethylene (PTFE),
Polyimides and nano silicon, its mass percent is：Nano silicon 0.01~3%, polyimides 20%, remaining
For polytetrafluoroethylene (PTFE), the distribution form of each component is：Nano silicon is evenly distributed in polyimides, while polyamides is sub-
Amine is evenly distributed in poly tetrafluoro ethylene matrix.
Embodiment 1
a:It is prepared by nano silicon dioxide dispersion：
Take 0.14g nano silicons to be put into acetone, 0.01g silane coupler (KH-560), magnetic agitation is added dropwise
Afterwards after 20~60min of sonic oscillation, stablized and finely dispersed nano silicon dioxide dispersion.
B. prepared by Polyimide/Nano SiO 2 powder：
6.00~6.20g 4,4 ˊ-diaminodiphenyl ether are added in nano silicon is scattered, and at 40~50 DEG C
40~100min of magnetic agitation, then adds 9.00~9.50g 3,3 ˊ, 4,4 ˊ-oxydiphthalic, increasingly generates polyamides
Amino acid/nano grade silica particles, at room temperature after 3~6h of magnetic agitation, adds triethylamine, acetic anhydride and the toluene (amount of addition
Respectively 40~60%, 300~400%, the 150 of polyamic acid/nano silicon quality~250%), continue to stir 1~
3h, makes imidization completely, and after suction filtration, acetone washing, product is dried, and with 1~5 DEG C/min heating rate, rises
2h is incubated after warm to 280 DEG C, crosses after 200 mesh sieves, obtains the dispersed Polyimide/Nano silica of nano silicon
Powder.
C. prepared by polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material：
7.98g polytetrafluoroethylene (PTFE) is taken to be scattered in absolute ethyl alcohol, the polyimides that then prepared by addition 2.02g steps b/
10~60min of magnetic agitation under nano grade silica particles, normal temperature, mixture is dried at 80~100 DEG C；
The mixture of drying is obtained into polytetrafluoroethylene (PTFE)/polyamides under normal temperature, 20~40MPa pressure after 5~30min of pressurize
The blank of imines/nanometer silicon dioxide material；
By the blank of polytetrafluoroethylene (PTFE)/Polyimide/Nano earth silicon material under air atmosphere, with 3~5 DEG C/min
Heating rate, be warming up to after 100~120 DEG C 50~70min of insulation, then with 1~3 DEG C/min heating rate, be warming up to
50~70min is incubated after 310~330 DEG C, then with 1~3 DEG C/min heating rate, is warming up to after 340~380 DEG C and is incubated
100~140min, finally with 1~3 DEG C/min rate of temperature fall, is cooled to 50~70min of insulation after 310~330 DEG C, cold with stove
But to obtaining polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material after room temperature.
Embodiment 2
a:It is prepared by nano silicon dioxide dispersion：
Take 0.42g nano silicons to be put into acetone, 0.04g silane coupler (KH-560), magnetic agitation is added dropwise
Afterwards after 20~60min of sonic oscillation, stablized and finely dispersed nano silicon dioxide dispersion.
B. prepared by Polyimide/Nano SiO 2 powder：
6.00~6.20g 4,4 ˊ-diaminodiphenyl ether are added in nano silicon is scattered, and at 40~50 DEG C
40~100min of magnetic agitation, then adds 9.00~9.50g 3,3 ˊ, 4,4 ˊ-oxydiphthalic, increasingly generates polyamides
Amino acid/nano grade silica particles, at room temperature after 3~6h of magnetic agitation, adds triethylamine, acetic anhydride and the toluene (amount of addition
Respectively 40~60%, 300~400%, the 150 of polyamic acid/nano silicon quality~250%), continue to stir 1~
3h, makes imidization completely, and after suction filtration, acetone washing, product is dried, and with 1~5 DEG C/min heating rate, rises
2h is incubated after warm to 280 DEG C, crosses after 200 mesh sieves, obtains the dispersed Polyimide/Nano silica of nano silicon
Powder.
C. prepared by polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material：
7.95g polytetrafluoroethylene (PTFE) is taken to be scattered in absolute ethyl alcohol, the polyimides that then prepared by addition 2.06g steps b/
10~60min of magnetic agitation under nano grade silica particles, normal temperature, mixture is dried at 80~100 DEG C.
The mixture of drying is obtained into polytetrafluoroethylene (PTFE)/polyamides under normal temperature, 20~40MPa pressure after 5~30min of pressurize
The blank of imines/nanometer silicon dioxide material.
By the blank of polytetrafluoroethylene (PTFE)/Polyimide/Nano earth silicon material under air atmosphere, with 3~5 DEG C/min
Heating rate, be warming up to after 100~120 DEG C 50~70min of insulation, then with 1~3 DEG C/min heating rate, be warming up to
50~70min is incubated after 310~330 DEG C, then with 1~3 DEG C/min heating rate, is warming up to after 340~380 DEG C and is incubated
100~140min, finally with 1~3 DEG C/min rate of temperature fall, is cooled to 50~70min of insulation after 310~330 DEG C, cold with stove
But to obtaining polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material after room temperature.
Embodiment 3
a:It is prepared by nano silicon dioxide dispersion：
Take 0.98g nano silicons to be put into acetone, 0.09g silane coupler (KH-560), magnetic agitation is added dropwise
Afterwards after 20~60min of sonic oscillation, stablized and finely dispersed nano silicon dioxide dispersion.
B. prepared by Polyimide/Nano SiO 2 powder：
6.00~6.20g 4,4 ˊ-diaminodiphenyl ether are added in nano silicon is scattered, and at 40~50 DEG C
40~100min of magnetic agitation, then adds 9.00~9.50g 3,3 ˊ, 4,4 ˊ-oxydiphthalic, increasingly generates polyamides
Amino acid/nano grade silica particles, at room temperature after 3~6h of magnetic agitation, adds triethylamine, acetic anhydride and the toluene (amount of addition
Respectively 40~60%, 300~400%, the 150 of polyamic acid/nano silicon quality~250%), continue to stir 1~
3h, makes imidization completely, and after suction filtration, acetone washing, product is dried, and with 1~5 DEG C/min heating rate, rises
2h is incubated after warm to 280 DEG C, crosses after 200 mesh sieves, obtains the dispersed Polyimide/Nano silica of nano silicon
Powder.
C. prepared by polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material：
7.88g polytetrafluoroethylene (PTFE) is taken to be scattered in absolute ethyl alcohol, the polyimides that then prepared by addition 2.15g steps b/
10~60min of magnetic agitation under nano grade silica particles, normal temperature, mixture is dried at 80~100 DEG C；
The mixture of drying is obtained into polytetrafluoroethylene (PTFE)/polyamides under normal temperature, 20~40MPa pressure after 5~30min of pressurize
The blank of imines/nanometer silicon dioxide material；
By the blank of polytetrafluoroethylene (PTFE)/Polyimide/Nano earth silicon material under air atmosphere, with 3~5 DEG C/min
Heating rate, be warming up to after 100~120 DEG C 50~70min of insulation, then with 1~3 DEG C/min heating rate, be warming up to
50~70min is incubated after 310~330 DEG C, then with 1~3 DEG C/min heating rate, is warming up to after 340~380 DEG C and is incubated
100~140min, finally with 1~3 DEG C/min rate of temperature fall, is cooled to 50~70min of insulation after 310~330 DEG C, cold with stove
But to obtaining polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material after room temperature.
As a comparison, pure polytetrafluoroethylmaterial material (comparative example 1), polytetrafluoroethylene (PTFE)/polyimide material are prepared for respectively
(comparative example 2) and (contrast of polytetrafluoroethylene (PTFE)/Polyimide/Nano earth silicon material is prepared for using conventional hybrid method
Example 3).
Comparative example 1
The pure polytetrafluorethylepowder powders of 10g are taken, after being dried at 80~100 DEG C, the pressurize 5 under normal temperature, 20~40MPa pressure
The blank of pure polytetrafluoroethylmaterial material is obtained after~30min, by the blank of polytetrafluoroethylmaterial material under air atmosphere, with 3~5
DEG C/min heating rate, and 50~70min of insulation after 100~120 DEG C is warming up to, then with 1~3 DEG C/min heating rate,
50~70min of insulation after 310~330 DEG C is warming up to, then with 1~3 DEG C/min heating rate, is warming up to after 340~380 DEG C
100~140min is incubated, finally with 1~3 DEG C/min rate of temperature fall, 50~70min of insulation after 310~330 DEG C is cooled to, with
Stove, which is cooled to after room temperature, obtains pure polytetrafluoroethylmaterial material.
Comparative example 2
Take the pure polytetrafluorethylepowder powders of 8.00g to be scattered in absolute ethyl alcohol, then add the pure polyimide powders of 2.00g
10~60min of magnetic agitation under (identical with the preparation method of polyimides in embodiment 1), normal temperature, by mixture 80~100
Dried at DEG C, mixture is obtained into polytetrafluoroethylene (PTFE)/polyimides under normal temperature, 20~40MPa pressure after 5~30min of pressurize
The blank of material, by the blank of polytetrafluoroethylene (PTFE)/polyimide material with 3~5 DEG C/min heating rate, it is warming up to 100~
50~70min is incubated after 120 DEG C, then with 1~3 DEG C/min heating rate, be warming up to after 310~330 DEG C insulation 50~
70min, then with 1~3 DEG C/min heating rate, is warming up to 100~140min of insulation after 340~380 DEG C, finally with 1~3
DEG C/min rate of temperature fall, 50~70min of insulation after 310~330 DEG C is cooled to, cools to the furnace and polytetrafluoroethyl-ne is obtained after room temperature
Alkene/polyimide material.
Comparative example 3
It is sub- that this comparative example prepares polytetrafluoroethylene (PTFE)/polyamides using traditional blend method, by the component proportion of embodiment 2
Amine/nanometer silicon dioxide material.
Take 0.06g nano silicons to be put into absolute ethyl alcohol, 0.006g silane couplers (KH-560) are added dropwise, magnetic force is stirred
Rear 20~60min of sonic oscillation is mixed, is stablized and finely dispersed nano silicon dioxide dispersion；
Take the pure polytetrafluorethylepowder powders of 7.95g to add in nano silicon dioxide dispersion, then add the pure polyamides of 2.00g sub-
10~60min of magnetic agitation under amine powder (identical with the preparation method of polyimides in embodiment 1), normal temperature, mixture is existed
Dried at 80~100 DEG C, mixture is obtained under normal temperature, 20~40MPa pressure to polytetrafluoroethylene (PTFE)/poly- after 5~30min of pressurize
The blank of acid imide/nanometer silicon dioxide material；
By the blank of polytetrafluoroethylene (PTFE)/Polyimide/Nano earth silicon material with 3~5 DEG C/min heating rate, rise
Temperature is to 50~70min of insulation after 100~120 DEG C, then with 1~3 DEG C/min heating rate, is warming up to after 310~330 DEG C and protects
50~70min of temperature, then with 1~3 DEG C/min heating rate, is warming up to 100~140min of insulation after 340~380 DEG C, finally
With 1~3 DEG C/min rate of temperature fall, 50~70min of insulation after 310~330 DEG C is cooled to, cools to the furnace after room temperature and is gathered
Tetrafluoroethene/Polyimide/Nano earth silicon material.
Respectively with GCr15 steel balls (diameter 9.525mm) and the polytetrafluoroethylene (PTFE) in above-described embodiment 1-3 and comparative example 1-3
Material (load 50N, stroke 15mm, frequency 2Hz, 120min, room temperature) testing friction abrasiveness under the conditions of identical friction testing
Can, test result is shown in Table 1.
The friction and wear behavior of polytetrafluoroethylmaterial material in the embodiment 1-3 of table 1 and comparative example 1-3
Polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material that embodiment of the present invention 1-3 is provided and contrast
Polytetrafluoroethylene (PTFE)/polyimide material in pure polytetrafluoroethylmaterial material, comparative example 2 in example 1 and the polytetrafluoro in comparative example 3
Ethene/Polyimide/Nano earth silicon material (traditional blend method preparation) is compared, and coefficient of friction is relatively low, and wearability is big
Width is improved, while the uniformity of material structure is preferably, therefore practicality is stronger, available for ball, Zi Run in self-lubricating knuckle bearing
The occasions such as sliding bushing, self-lubricating machine tool guideway, self-lubricating retainer.
It is only presently preferred embodiments of the present invention that specific description of embodiments of the present invention above, not to limit this hair
Bright, all any modification and improvement made within principle of the present invention all should belong to scope of the following claims of the present invention.
Claims (6)
1. a kind of polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material, it is characterised in that：The material it is each
Component is polytetrafluoroethylene (PTFE), polyimides and nano silicon, and its mass percent is：Polyimides 19~21%, nanometer
Silica 0.01~3%, surplus is polytetrafluoroethylene (PTFE), and the distribution form of each component is：Polyimides is evenly distributed on poly- four
In PVF matrix, and nano silicon then completely and is evenly distributed in polyimides.
2. polytetrafluoroethylene (PTFE) according to claim 1/Polyimide/Nano silica self-lubricating material, its feature exists
In the polytetrafluorethylepowder powder particle diameter is 1 μm~100 μm.
3. polytetrafluoroethylene (PTFE) according to claim 1/Polyimide/Nano silica self-lubricating material, its feature exists
In, the nano silicon is spherical, 1~50nm of particle diameter, and by silane coupler modification.
4. polytetrafluoroethylene (PTFE) according to claim 1/Polyimide/Nano silica self-lubricating material, its feature exists
In the polyimides is：By 3,3 ˊ, the polyamides that 4,4 ˊ-oxydiphthalic is synthesized with 4,4 ˊ-diaminodiphenyl ether is sub-
Amine, particle diameter is 1 μm~74 μm, and contains equally distributed nano silicon in polyimides.
5. a kind of preparation of polytetrafluoroethylene (PTFE) according to claim 1/Polyimide/Nano silica self-lubricating material
Method, it is characterised in that the preparation method is as follows：
It is prepared by step (1) polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material mixture：
Take 7.7~7.999g polytetrafluorethylepowder powder to be scattered in absolute ethyl alcohol, then add the poly- of 2.001~2.3g preparations
10~60min of magnetic agitation under acid imide/nano grade silica particles, normal temperature, is well mixed, by mixture at 80~100 DEG C
Lower drying；
Step (2) polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material shaping：
The mixture that step (1) is obtained obtained under normal temperature and 20~40MPa pressure after 5~30min of pressurize polytetrafluoroethylene (PTFE)/
The blank of Polyimide/Nano silica self-lubricating material；
Step (3) polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material sintering：
The blank for the polytetrafluoroethylmaterial material that step (2) is obtained is under air atmosphere, with 3~5 DEG C/min heating rate, rises
Temperature is to 50~70min of insulation after 100~120 DEG C, then with 1~3 DEG C/min heating rate, is warming up to after 310~330 DEG C and protects
50~70min of temperature, then with 1~3 DEG C/min heating rate, is warming up to 100~140min of insulation after 340~380 DEG C, finally
With 1~3 DEG C/min rate of temperature fall, 50~70min of insulation after 310~330 DEG C is cooled to, cools to the furnace after room temperature and is gathered
Tetrafluoroethene/Polyimide/Nano silica self-lubricating material.
6. the preparation side of polytetrafluoroethylene (PTFE) according to claim 5/Polyimide/Nano silica self-lubricating material
Method, it is characterised in that the preparation method of the Polyimide/Nano SiO 2 powder is as follows：
It is prepared by step (1) nano silicon dioxide dispersion：
Take 0.01~0.3g nano silicons to be put into acetone, be added dropwise after 0.001~0.03g silane couplers, magnetic agitation
20~60min of sonic oscillation, is uniformly dispersed and stable nano silicon dioxide dispersion；
It is prepared by step (2) polyamic acid/nano grade silica particles：
6.00~6.20g 4,4 ˊ-diaminodiphenyl ether are added in the nano silicon dioxide dispersion of step (1), and 40
40~100min of magnetic agitation at~50 DEG C, then adds 9.00~9.50g 3,3 ˊ, 4,4 ˊ-oxydiphthalic, room temperature
After 3~6h of lower magnetic agitation, the mixed liquor of generation polyamic acid/nano grade silica particles and acetone；
It is prepared by step (3) Polyimide/Nano SiO 2 powder：
In the polyamic acid/nano silicon and addition triethylamine, acetic anhydride and toluene, three in acetone mixture of step (2)
The addition of kind of raw material be respectively polyamic acid/nano silicon quality 40~60%, 300~400%, 150~
250%, continue to stir 1~3h, after imidization is complete, after suction filtration, washing, product is dried, and with 1~5 DEG C/min
Heating rate, be incubated 2h after being warming up to 280 DEG C, cool to the furnace after room temperature, cross 200 mesh sieves, obtain Polyimide/Nano two
Silicon oxide powder.
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| CN107698972A (en) * | 2017-10-18 | 2018-02-16 | 徐宏伟 | A kind of joint of robot self-lubricating material and its preparation technology |
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| CN111303628A (en) * | 2020-03-16 | 2020-06-19 | 中国科学院兰州化学物理研究所 | Polyimide self-lubricating composite material and preparation method thereof |
| CN113510891A (en) * | 2021-04-23 | 2021-10-19 | 中国科学院兰州化学物理研究所 | Two-stage hole polyimide material, preparation method thereof, two-stage hole polyimide retainer and application thereof |
| CN115819788A (en) * | 2022-12-08 | 2023-03-21 | 万华化学集团股份有限公司 | Preparation method of high-adhesion high-wear-resistance lightweight nylon powder |
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| CN111303628B (en) * | 2020-03-16 | 2021-03-23 | 中国科学院兰州化学物理研究所 | Polyimide self-lubricating composite material and preparation method thereof |
| CN113510891A (en) * | 2021-04-23 | 2021-10-19 | 中国科学院兰州化学物理研究所 | Two-stage hole polyimide material, preparation method thereof, two-stage hole polyimide retainer and application thereof |
| CN113510891B (en) * | 2021-04-23 | 2022-09-27 | 中国科学院兰州化学物理研究所 | Two-stage hole polyimide material, preparation method thereof, two-stage hole polyimide retainer and application thereof |
| CN115819788A (en) * | 2022-12-08 | 2023-03-21 | 万华化学集团股份有限公司 | Preparation method of high-adhesion high-wear-resistance lightweight nylon powder |
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