CN109825012A - A kind of modified polytetrafluoroethylcomposite composite material and preparation method thereof - Google Patents
A kind of modified polytetrafluoroethylcomposite composite material and preparation method thereof Download PDFInfo
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- CN109825012A CN109825012A CN201910131763.2A CN201910131763A CN109825012A CN 109825012 A CN109825012 A CN 109825012A CN 201910131763 A CN201910131763 A CN 201910131763A CN 109825012 A CN109825012 A CN 109825012A
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Abstract
The present invention relates to technical field of composite materials, a kind of modified polytetrafluoroethylcomposite composite material is provided, includes 50~65 parts of polytetrafluoroethylene (PTFE), the modified mica of 30~45 parts of N- β-aminoethyl-γ-aminopropyltrimethoxysilanes, 1~5 part of molybdenum disulfide, 1~5 part of graphite and 1~5 part of polyether-ether-ketone.Gained modified polytetrafluoroethylcomposite composite material tensile strength >=10MPa of the invention, tensile modulus of elasticity >=2200MPa, tension fracture elongation rate >=15%, coefficient of friction :≤0.24, Volume erosion rate≤7.7 × 10‑6mm3/ N.m, has excellent performance.The present invention also provides the preparation methods of the material: suppressing after polytetrafluoroethylene (PTFE), N- β-aminoethyl-γ-aminopropyltrimethoxysilane modified mica, molybdenum disulfide, graphite and polyether-ether-ketone are mixed, obtains compacting material；Gained compacting material is sintered, modified polytetrafluoroethylcomposite composite material is obtained.
Description
Technical field
The present invention relates to technical field of composite materials more particularly to a kind of modified polytetrafluoroethylcomposite composite material and its preparations
Method.
Background technique
Sealing is the general technology of high-end equipment manufacture.Currently, high-end equipment service condition is more harsh, for a long time
Be subjected to the extreme harsh environments such as wide temperature range, high revolving speed, high/low temperature alternation, complex dielectrics, the high rebound of sealing material, low friction and
High abrasion collaborative design and key technology have become the significant technology issues for restricting high-end equipment.Polymer with light, media-resistant,
Designability waits by force excellent performances, is the desirable seal material that high-end equipment uses under bad lubrication state.But conventional polymeric
Object sealing material there are poor flexibility, it is tough be difficult to the problems such as having both, is easy to wear, stability is poor, be unable to satisfy modern high end dress
The requirement of standby high reliability and long-life.
Polytetrafluoroethylene material (PTFE), be widely used in defence and military, atomic energy, petroleum, radio, electric machinery,
The important departments such as chemical industry.Polytetrafluoroethylene (PTFE) has a series of excellent service performances: high-low temperature resistant-long-term use temperature-
200~260 DEG C；It is corrosion-resistant-to be resistant to chloroazotic acid and all organic solvents；Optimal aging life-span in weatherability-plastics；Gao Run
It is sliding-there is the smallest coefficient of friction in plastics.But pure polytetrafluoroethylene (PTFE) is due to the easy shearing slip of molecule interchain (easy-cold flow),
Occur that plastic deformation (easy creep), resilience is poor, wear no resistance, thermal conductivity is low under the effect of long-time continuous load, as close
Closure material exist wear no resistance, easy-cold flow and the problems such as poor thermal conductivity.Therefore, it is necessary to realize teflon seal by modified
Material high elastic modulus with it is anti abrasive compatible, difficult point is by selecting suitable functional stuffing and process for modifying surface to mention
The elasticity modulus and wear resistance of high polytetrafluoroethylene (PTFE).
Summary of the invention
The purpose of the present invention is to provide a kind of modified polytetrafluoroethylcomposite composite material and preparation method thereof, present invention selections
The modified mica filled polytetrafluoroethylene (PTFE) in-aminoethyl-γ-aminopropyltrimethoxysilane surface N- β, and composite filled graphite,
Molybdenum disulfide and polyether-ether-ketone improve effect using the collaboration between multicomponent, realize high rebound with it is anti abrasive compatible.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of modified polytetrafluoroethylcomposite composite material, the component comprising following mass fraction:
Preferably, the partial size of the polytetrafluoroethylene (PTFE) is 20~100 μm.
Preferably, the preparation method of the modified mica of the N- β-aminoethyl-γ-aminopropyltrimethoxysilane includes such as
Lower step:
It disperses mica in acetone, obtains dispersion liquid；
Graft modification is carried out after the dispersion liquid and N- β-aminoethyl-γ-aminopropyltrimethoxysilane are mixed, is obtained
The modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane.
Preferably, the partial size of the mica is 1~10 μm.
Preferably, the partial size of the molybdenum disulfide is 1~200 μm.
Preferably, the partial size of the graphite is 1~200 μm.
Preferably, the partial size of the polyether-ether-ketone is 20~50 μm.
The present invention also provides the preparation methods of the modified polytetrafluoroethylcomposite composite material, comprise the following steps:
(1) by the modified mica of polytetrafluoroethylene (PTFE), N- β-aminoethyl-γ-aminopropyltrimethoxysilane, molybdenum disulfide,
It is suppressed after graphite and polyether-ether-ketone mixing, obtains compacting material；
(2) gained compacting material is sintered, obtains modified polytetrafluoroethylcomposite composite material.
Preferably, the pressure of the compacting is 70~100MPa, and the time is 1~10min.
Preferably, the temperature of the sintering is 360~380 DEG C, and the time is 90~150min.
It include 50~65 parts of polytetrafluoroethylene (PTFE) the present invention provides a kind of modified polytetrafluoroethylcomposite composite material, 30~45
The modified mica of part N- β-aminoethyl-γ-aminopropyltrimethoxysilane, 1~5 part of molybdenum disulfide, 1~5 part of graphite and 1~5
Part polyether-ether-ketone.The present invention can be improved mica as modifying agent and existed using N- β-aminoethyl-γ-aminopropyltrimethoxysilane
Dispersibility in polytetrafluoroethylene (PTFE), while improving the interface cohesion between mica and polytetrafluoroethylene (PTFE) and mica.In addition, gained N-
The modified mica of β-aminoethyl-γ-aminopropyltrimethoxysilane can also be shown in conjunction with molybdenum disulfide, graphite and polyether-ether-ketone
Write the tensile property for improving polytetrafluoroethylene (PTFE) and wear-resisting property etc..By embodiment result it is found that the modified polytetrafluoro of present invention gained
Ethylene composite material tensile strength >=10MPa, tensile modulus of elasticity >=2200MPa, tension fracture elongation rate >=15%, friction system
Number :≤0.24, Volume erosion rate≤7.7 × 10-6mm3/ N.m, has excellent performance.
The present invention also provides the preparation methods of the modified polytetrafluoroethylcomposite composite material, comprise the following steps: (1) will
Polytetrafluoroethylene (PTFE), N- β-aminoethyl-γ-aminopropyltrimethoxysilane modified mica, molybdenum disulfide, graphite and polyether-ether-ketone
It is suppressed after mixing, obtains compacting material；(2) gained compacting material is sintered, obtains modified polytetrafluoroethylcomposite composite material.
The method that the present invention prepares the modified polytetrafluoroethylcomposite composite material, it is easy to operate, it is easy to implement.
Specific embodiment
The present invention provides a kind of modified polytetrafluoroethylcomposite composite material, the component comprising following mass fraction:
Modified polytetrafluoroethylcomposite composite material of the present invention include 50~65 parts of polytetrafluoroethylene (PTFE), preferably 55~60
Part.In the present invention, the commercially available polyflon that the polytetrafluoroethylene (PTFE) is well known to those skilled in the art；It is described poly-
The partial size of tetrafluoroethene is preferably 20~100 μm, and more preferably 40~60 μm.Polytetrafluoroethylene (PTFE) of the present invention has resistance to height
The features such as warm, wear-resisting and low-friction coefficient.
On the basis of the quality of polytetrafluoroethylene (PTFE), modified polytetrafluoroethylcomposite composite material of the present invention includes 30~45 parts
The modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane, preferably 35~40 parts.
In the present invention, the preparation method of the modified mica of the N- β-aminoethyl-γ-aminopropyltrimethoxysilane is excellent
Choosing comprises the following steps:
It disperses mica in acetone, obtains dispersion liquid；
Graft modification is carried out after the dispersion liquid and N- β-aminoethyl-γ-aminopropyltrimethoxysilane are mixed, is obtained
The modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane.
The present invention preferably disperses mica in acetone, obtains dispersion liquid.In the present invention, the partial size of the mica is preferred
It is 1~10 μm, more preferably 4~6 μm；The mass ratio of the mica and acetone is preferably 100:(400~600), more preferably
100:(500~550).The present invention does not have particular/special requirement to the specific embodiment of the dispersion, can uniformly be dispersed
Liquid.Mica of the present invention is constructed with continuous stratiform oxygen-octahedron, the peelable thin slice for tool elasticity, the soft bendable of matter
Song, and its radius-thickness ratio is big, and wear resistence and wearability are good, are insoluble in acid-base solution, and chemical property is stablized.
After obtaining dispersion liquid, the present invention mixes the dispersion liquid and N- β-aminoethyl-γ-aminopropyltrimethoxysilane
After carry out graft modification, obtain the modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane.
In the present invention, the mica and N- β-aminoethyl-γ-aminopropyltrimethoxysilane mass ratio are preferably
100:(1~3), further preferably 100:2.In the present invention, the mixing is preferably stirred, and the stirring uses machine
Tool stirring；The graft modification preferably carries out under agitation, and the time of the graft modification is preferably 1~3h, into
One step is preferably 2h.Graft modification of the present invention is specially by surface modifier N- β-aminoethyl-γ-aminopropyl trimethoxy
Silane Grafted is to mica surface.
The present invention preferably after the graft modification, is filtered obtained product system, dries, and obtains N- β-
The modified mica of aminoethyl-γ-aminopropyltrimethoxysilane.
The present invention first obtains mica dispersion liquid, then mixes with N- β-aminoethyl-γ-aminopropyltrimethoxysilane, can
Mica and N- β-aminoethyl-γ-aminopropyltrimethoxysilane are mixed to visibly homogeneous, guarantee N- β-aminoethyl-γ-ammonia third
Modified effect of the base trimethoxy silane to mica.In the present invention, it is commercially available it is modified micaceous be not appropriate for filling polytetrafluoroethyl-ne
Alkene, N- β-aminoethyl-γ-aminopropyltrimethoxysilane can be improved dispersion of the mica in polytetrafluoroethylene (PTFE) as modifying agent
Property, while improving the interface cohesion between mica and polytetrafluoroethylene (PTFE) and mica.In addition, gained N- β-aminoethyl-γ-aminopropyl
The modified mica of trimethoxy silane can also significantly improve polytetrafluoroethylene (PTFE) in conjunction with molybdenum disulfide, graphite and polyether-ether-ketone
Tensile property and wear-resisting property etc..
On the basis of the quality of polytetrafluoroethylene (PTFE), modified polytetrafluoroethylcomposite composite material of the present invention includes 1~5 part two
Molybdenum sulfide, preferably 2~3 parts.In the present invention, the partial size of the molybdenum disulfide is preferably 1~200 μm, more preferably 50~
150 μm, most preferably 80~120 μm.
On the basis of the quality of polytetrafluoroethylene (PTFE), modified polytetrafluoroethylcomposite composite material of the present invention includes 1~5 part of stone
Ink, preferably 2~3 parts.In the present invention, the partial size of the graphite is preferably 1~200 μm, and more preferably 50~150 μm, most
Preferably 80~120 μm.
Ultra-fine molybdenum disulfide and graphite of the present invention have excellent solid lubrication performance.
On the basis of the quality of polytetrafluoroethylene (PTFE), modified polytetrafluoroethylcomposite composite material of the present invention includes 1~5 part poly-
Ether ether ketone, preferably 2~3 parts.In the present invention, the partial size of the polyether-ether-ketone is preferably 20~50 μm, more preferably 35~
45μm.Polyether-ether-ketone resin of the present invention has good mechanical property, and the size that can be improved under polytetrafluoroethylene (PTFE) high temperature is steady
It is qualitative.
The present invention also provides the preparation methods of the modified polytetrafluoroethylcomposite composite material, comprise the following steps:
(1) by the modified mica of polytetrafluoroethylene (PTFE), N- β-aminoethyl-γ-aminopropyltrimethoxysilane, molybdenum disulfide,
It is suppressed after graphite and polyether-ether-ketone mixing, obtains compacting material；
(2) gained compacting material is sintered, obtains modified polytetrafluoroethylcomposite composite material.
The present invention is by the modified mica of polytetrafluoroethylene (PTFE), N- β-aminoethyl-γ-aminopropyltrimethoxysilane, curing
It is suppressed after molybdenum, graphite and polyether-ether-ketone mixing, obtains compacting material.In the present invention, the mixing and compacting use ability
Conventional technical means known to field technique personnel carries out.In the present invention, the pressure of the compacting be preferably 70~
100MPa, further preferably 80~90MPa；The pressure hold time of the compacting is preferably 1~10min, further preferably
For 3~5min.
After obtaining compacting material, gained compacting material is sintered by the present invention, obtains modified polytetrafluoroethylcomposite composite material.
In the present invention, the sintering carries out preferably in sintering furnace；The temperature of the sintering is preferably 360~380 DEG C,
Further preferably 365~375 DEG C, much further preferably from 370~372 DEG C；The temperature hold-time of the sintering is preferably
90~150min, more a step are preferably 100~120min.In the present invention, the rate for being warming up to the sintering temperature is preferably
80~100 DEG C/h, more preferably 90~95 DEG C/h can be specifically adjusted according to the size of blank；The sintering
It is freely down to room temperature later.
In the present invention, the compacting is that mold is added in the powder weighed up, then keeps one section under pressure
Time, by powder pressing at blank；Blank after compression moulding is specially heated to sintering temperature by the sintering, and herein
At a temperature of keep certain time, be gradually converted into polytetrafluoroethylene (PTFE) molecule by crystalline amorphous, the single polytetrafluoro of dispersion
Vinyl particle is continuous whole at one by diffusing into one another bond vitrified, then again through cooling, polytetrafluoroethylene (PTFE) molecule
Gradually switch to crystalline from amorphous again, polytetrafluoroethylene material can be obtained in cooling completion.
In the present invention, the pressure of the compacting and time directly affect final products, and pressure is too small, and powder exists
The degree being compacted in mold is small, and the shrinking percentage of product is big after sintering；Pressure is excessive, and internal stress is difficult to discharge, and produces in sintering process
There is the defects of layering, crackle in product.In the present invention, sintering is one in polytetrafluoroethylene material molding process important
Link, it will make polytetrafluoroethylproducts products performance that basic change occur, and the conditions such as temperature and time of sintering influence the heat of material
Performance, mechanical property, density, hardness and gas permeability etc..The selection of component of the present invention, the control of pressing conditions and sintered bar
Interact connection between the control of part, and it is comprehensive can finally to improve tensile property and wear-resisting property of polytetrafluoroethylene material etc.
Performance.
The present invention can complete resulting modified polytetrafluoroethylcomposite composite material to sintering and be machined out, and obtain polytetrafluoro
Ethylene seal, specific such as sealing ring, gasket and snap ring.
Technical solution provided by the invention is described in detail below with reference to embodiment, but they cannot be understood
For limiting the scope of the present invention.
Embodiment 1
65 grams of teflon resin powder are weighed, the modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane
It 45 grams, 5 grams of graphite, 5 grams of molybdenum disulfide, 5 grams of polyether-ether-ketone, is uniformly mixed in stirred type mixing machine.The powder mixed is put
Enter mold, under the pressure of 100MPa, suppresses 3 minutes, be put into sintering furnace and be sintered after demoulding, be warming up to the rate of 80 DEG C/h
150 minutes are kept the temperature after 365 DEG C, room temperature is freely cooled to after sintering, the modified Teflon composite wood that sintering is completed
Material machining, obtains teflon seal.
Each performance data of the present embodiment resulting materials is respectively as follows: tensile strength 10.5MPa, tensile modulus of elasticity
2310MPa, tension fracture elongation rate 15.5%, coefficient of friction 0.23, Volume erosion rate 7.5 × 10-6mm3/N.m。
Embodiment 2
55 grams of teflon resin powder are weighed, the modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane
It 40 grams, 2 grams of graphite, 3 grams of molybdenum disulfide, 4 grams of polyether-ether-ketone, is uniformly mixed in stirred type mixing machine.The powder mixed is put
Enter mold, under the pressure of 70MPa, suppresses 5 minutes, be put into sintering furnace and be sintered after demoulding, be warming up to the rate of 90 DEG C/h
150 minutes are kept the temperature after 365 DEG C, is freely cooled down after sintering, the modified polytetrafluoroethylcomposite composite material machine completed to sintering adds
Work obtains teflon seal.
Each performance data of the present embodiment resulting materials is respectively as follows: tensile strength 10.8MPa, tensile modulus of elasticity
2270MPa, tension fracture elongation rate 15.2%, coefficient of friction 0.22, Volume erosion rate 7.7 × 10-6mm3/N.m。
Embodiment 3
60 grams of teflon resin powder are weighed, the modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane
It 35 grams, 4 grams of graphite, 1 gram of molybdenum disulfide, 3 grams of polyether-ether-ketone, is uniformly mixed in stirred type mixing machine.The powder mixed is put
Enter mold, under the pressure of 100MPa, suppresses 5 minutes, be put into sintering furnace and be sintered after demoulding, heated up with the rate of 100 DEG C/h
90 minutes are kept the temperature after to 375 DEG C, is freely cooled down after sintering, the modified polytetrafluoroethylcomposite composite material machine completed to sintering adds
Work obtains teflon seal.
Each performance data of the present embodiment resulting materials is respectively as follows: tensile strength 11.3MPa, tensile modulus of elasticity
2210MPa, tension fracture elongation rate 18.5%, coefficient of friction 0.21, Volume erosion rate 7.1 × 10-6mm3/N.m。
Embodiment 4
60 grams of teflon resin powder are weighed, the modified mica of N- β-aminoethyl-γ-aminopropyltrimethoxysilane
It 45 grams, 2 grams of graphite, 4 grams of molybdenum disulfide, 2 grams of polyether-ether-ketone, is uniformly mixed in stirred type mixing machine.The powder mixed is put
Enter mold, under the pressure of 80MPa, suppresses 4 minutes, be put into sintering furnace and be sintered after demoulding, be warming up to the rate of 80 DEG C/h
100 minutes are kept the temperature after 368 DEG C, is freely cooled down after sintering, the modified polytetrafluoroethylcomposite composite material machine completed to sintering adds
Work obtains teflon seal.
Each performance data of the present embodiment resulting materials is respectively as follows: tensile strength 10.2MPa, tensile modulus of elasticity
2350MPa, tension fracture elongation rate 15.1%, coefficient of friction 0.24, Volume erosion rate 7.4 × 10-6mm3/N.m。
By embodiment result it is found that present invention gained modified polytetrafluoroethylcomposite composite material tensile strength >=10MPa, stretches
Elasticity modulus >=2200MPa, tension fracture elongation rate >=15%, coefficient of friction :≤0.24, Volume erosion rate≤7.7 × 10- 6mm3/ N.m, has excellent performance.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of modified polytetrafluoroethylcomposite composite material, which is characterized in that the component comprising following mass fraction:
2. modified polytetrafluoroethylcomposite composite material according to claim 1, which is characterized in that the grain of the polytetrafluoroethylene (PTFE)
Diameter is 20~100 μm.
3. modified polytetrafluoroethylcomposite composite material according to claim 1, which is characterized in that the N- β-aminoethyl-γ-
The preparation method of the modified mica of aminopropyl trimethoxysilane comprises the following steps:
It disperses mica in acetone, obtains dispersion liquid；
Graft modification is carried out after the dispersion liquid and N- β-aminoethyl-γ-aminopropyltrimethoxysilane are mixed, obtains N- β-
The modified mica of aminoethyl-γ-aminopropyltrimethoxysilane.
4. modified polytetrafluoroethylcomposite composite material according to claim 3, which is characterized in that the partial size of the mica is 1
~10 μm.
5. modified polytetrafluoroethylcomposite composite material according to claim 1, which is characterized in that the partial size of the molybdenum disulfide
It is 1~200 μm.
6. modified polytetrafluoroethylcomposite composite material according to claim 1, which is characterized in that the partial size of the graphite is 1
~200 μm.
7. modified polytetrafluoroethylcomposite composite material according to claim 1, which is characterized in that the partial size of the polyether-ether-ketone
It is 20~50 μm.
8. the preparation method of modified polytetrafluoroethylcomposite composite material described in claim 1~7 any one, which is characterized in that
It comprises the following steps:
(1) by the modified mica of polytetrafluoroethylene (PTFE), N- β-aminoethyl-γ-aminopropyltrimethoxysilane, molybdenum disulfide, graphite
It is suppressed with after polyether-ether-ketone mixing, obtains compacting material；
(2) gained compacting material is sintered, obtains modified polytetrafluoroethylcomposite composite material.
9. preparation method according to claim 8, which is characterized in that the pressure of the compacting is 70~100MPa, time
For 1~10min.
10. preparation method according to claim 8 or claim 9, which is characterized in that the temperature of the sintering is 360~380 DEG C,
Time is 90~150min.
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| CN201910131763.2A CN109825012B (en) | 2019-02-22 | 2019-02-22 | Modified polytetrafluoroethylene composite material and preparation method thereof |
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| CN113462106A (en) * | 2021-08-03 | 2021-10-01 | 温州东一机械制造有限公司 | Wear-resistant sealing ring and preparation method thereof |
| CN114456525A (en) * | 2022-02-15 | 2022-05-10 | 江门市格雷亚特流体密封技术有限公司 | Polytetrafluoroethylene sealing element for oil cylinder and preparation method thereof |
| CN117089117A (en) * | 2023-10-17 | 2023-11-21 | 季华实验室 | Graphite hybrid microcapsule and preparation method thereof, fluorine-based material and preparation method thereof |
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| CN113462106B (en) * | 2021-08-03 | 2022-01-21 | 温州东一机械制造有限公司 | Wear-resistant sealing ring and preparation method thereof |
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| CN117089117A (en) * | 2023-10-17 | 2023-11-21 | 季华实验室 | Graphite hybrid microcapsule and preparation method thereof, fluorine-based material and preparation method thereof |
| CN117089117B (en) * | 2023-10-17 | 2024-02-13 | 季华实验室 | Graphite hybrid microcapsule and preparation method thereof, fluorine-based material and preparation method thereof |
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