CN102924854A - Teflon composite material and preparation method thereof - Google Patents
Teflon composite material and preparation method thereof Download PDFInfo
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- CN102924854A CN102924854A CN201210437295XA CN201210437295A CN102924854A CN 102924854 A CN102924854 A CN 102924854A CN 201210437295X A CN201210437295X A CN 201210437295XA CN 201210437295 A CN201210437295 A CN 201210437295A CN 102924854 A CN102924854 A CN 102924854A
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Abstract
The invention discloses a Teflon composite material and a preparation method thereof. The composite material contains 65%-85% by weight of Teflon and 15%-35% by weight of high stereospecific polyacrylonitrile, wherein the content of an isotactic three-unit group (mm) of the high stereospecific polyacrylonitrile is 45%-78%. The preparation method comprises the steps of mixing Teflon powder, acrylonitrile and urea, then performing low temperature refrigeration at the temperature from -75 to -50 DEG C for more than 120 hours, dispersing a frozen mixture in liquid nitrogen to perform gamma ray irradiation, performing acrylonitrile polymerization in the environment of -70 DEG C+/-5 DEG C for 3-10 hours after irradiation, using water to repetitively clean and remove the urea and an unreacted acrylonitrile monomer, and performing filtering, drying, compression forming and high-temperature sintering. Compared with unmodified Teflon, the abrasive resistance of the composite material is improved by 100-150 times, the heat resistance and the high-temperature mechanical property are further improved, and the Teflon composite material has wide application in industrial departments of machinery, chemical engineering, aerospace and the like.
Description
Technical field
The invention belongs to the filamentary material preparation field, be specifically related to ptfe composite of a kind of high-wearing feature and preparation method thereof.
Background technology
Tetrafluoroethylene is widely used in various fields because of its excellent chemical stability, high thermal resistance, anti-ultraviolet radiation and low frictional coefficient, yet it wears no resistance and has but limited its use range.In order to improve the wear resisting property of polytetrafluoroethylmaterial material, technology in the past is the preparation such as filler metal and glass fibre, carbon fiber ptfe composite in tetrafluoroethylene mainly.Above-mentioned packing material can improve the wear resisting property of ptfe composite to a certain extent, but the improvement of performance is not ideal.
China Science ﹠ Technology University adopts polytetrafluorethylepowder powder and polyacrylonitrile powder to be mixed with ptfe composite in the CN100582158C patent, add in addition metal and metal oxide etc., it has improved the wear resistance of tetrafluoroethylene to a certain extent, but wherein polyacrylonitrile powder addition is larger, and metallics and tetrafluoroethylene lack consistency, generation is separated easily, reduces its mechanical property.
Summary of the invention
The purpose of embodiment of the present invention provides a kind of ptfe composite and preparation method thereof, this ptfe composite wear resisting property is good, consistency is high, sintering temperature is low when preparing, can solve present polytetrafluoroethylmaterial material and wear no resistance, the low bad technical problem of mechanism performance that causes of consistency.
The objective of the invention is to be achieved through the following technical solutions:
Embodiment of the present invention provides a kind of ptfe composite, this matrix material contains the tetrafluoroethylene of 65wt%～85wt% and the vertical structure polyacrylonitrile of height of 15wt%～35wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 45%～78%.
Embodiment of the present invention also provides a kind of preparation method of ptfe composite, comprising:
Step 1, each component is the percentage composition meter by weight, and the tetrafluoroethylene with 30%～60%, 15%～25% vinyl cyanide and 30%～50% urea mix the formation mixture,
Step 2, with described mixture-75 ℃～-50 ℃ cryogenic freezings more than 120 hours;
Step 3 is dispersed in the described mixture after freezing in the liquid nitrogen, carries out Co
60Gamma-ray irradiation, radiation dose are 3～30kGy;
Step 4 makes vinyl cyanide in the described mixture carry out polyase 13～10 hour in-70 ℃ ± 5 ℃ environment behind the irradiation;
Step 5 after the polyreaction, is removed urea and unreacting propylene nitrile monomer, filtration, drying with the described mixture of water repetitive scrubbing, in coldmoulding under the 40MPa pressure and kept under 40MPa pressure 5～10 minutes;
Step 6 is inserted the sample of compression moulding in the high temperature sintering furnace, is heated to 330 ℃～380 ℃ with 30 ℃～100 ℃/hour temperature rise rates, heat preservation sintering 2 hours;
Step 7 naturally cools to room temperature, namely obtains ptfe composite.
Can be found out by the above-mentioned technical scheme that provides, the ptfe composite that embodiment of the present invention provides, at the synthetic high vertical structure polyacrylonitrile of polytetrafluorethylepowder powder situ, its isotactic triad (mm) content is 45%～78%, high vertical structure polyacrylonitrile is present in the polytetrafluoroethylmaterial material in the mode of grafting and blend, content only is 15wt%～35wt%, so that the consistency of this material is good.Cyclization can occur in high vertical structure polyacrylonitrile in high-temperature sintering process, form ladder structure, and the friction transfer that has strengthened matrix material is rubbed at the sticking power to the face surface of rubbing, thereby greatly improves its wear resistance.Actual measurement shows, under identical friction testing condition, the abrasion loss that contains high vertical structure polyacrylonitrile high-wearing polytetrafluoroethylcomposite composite material is 1/150～1/100 of unmodified tetrafluoroethylene, contains simultaneously high vertical structure polyacrylonitrile high-wearing polytetrafluoroethylcomposite composite material heatproof and can reach more than 300 ℃.
Embodiment
The below is clearly and completely described the technical scheme in the embodiment of the invention, and obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills belong to protection scope of the present invention not making the every other embodiment that obtains under the creative work prerequisite.
The embodiment of the invention provides a kind of ptfe composite, this matrix material contains the tetrafluoroethylene of 65wt%～85wt% and the vertical structure polyacrylonitrile of height of 15wt%～35wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 45%～78%.
The preparation method of above-mentioned ptfe composite may further comprise the steps:
Step 1, each component is the percentage composition meter by weight, and the tetrafluoroethylene with 30%～60%, 15%～25% vinyl cyanide and 30%～50% urea mix the formation mixture,
Step 2, with described mixture-75 ℃～-50 ℃ cryogenic freezings more than 120 hours;
Step 3 is dispersed in the described mixture after freezing in the liquid nitrogen, carries out Co
60Gamma-ray irradiation, radiation dose are 3～30kGy;
Step 4 makes vinyl cyanide in the described mixture carry out polyase 13～10 hour in-70 ℃ ± 5 ℃ environment behind the irradiation;
Step 5 after the polyreaction, is removed urea and unreacting propylene nitrile monomer, filtration, drying with the described mixture of water repetitive scrubbing, in coldmoulding under the 40MPa pressure and kept under 40MPa pressure 5～10 minutes;
Step 6 is inserted the sample of compression moulding in the high temperature sintering furnace, is heated to 330 ℃～380 ℃ with 30 ℃～100 ℃/hour temperature rise rates, heat preservation sintering 2 hours;
Step 7 naturally cools to room temperature, namely obtains ptfe composite.
The granularity of above-mentioned urea is less than 400 μ m.
It is the polytetrafluorethylepowder powder of 30 μ m～200 μ m that above-mentioned tetrafluoroethylene adopts granularity.
The below describes the present invention in detail and provides several embodiment, and the friction and wear behavior test is carried out at MM2200 type ring-block abrasion tester, and test is undertaken by GB 3960-83 " plastics sliding frictional wear test method ".
Embodiment 1:
Present embodiment provides a kind of ptfe composite, and this matrix material contains the tetrafluoroethylene of 79wt% and the vertical structure polyacrylonitrile of height of 21wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 63% through the carbon-13 nmr spectra test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material is the percentage composition meter by weight, polytetrafluorethylepowder powder with 50% (granularity is 50 μ m), 15% vinyl cyanide and 35% urea (granularity is 100 μ m) mix and form mixture and add in the reaction flask,-50 ℃ of lower cryogenic freezings 120 hours, in reaction flask, add afterwards liquid nitrogen, carry out Co
60Gamma-ray irradiation, irradiation dose is 15kGy, in the environment with-70 ℃ ± 5 ℃ of reaction flask immigrations behind the irradiation, carry out polymerization after 10 hours, remove urea and unreacting propylene nitrile monomer, filtration, drying with the water repetitive scrubbing, kept 8 minutes in coldmoulding under the 40MPa pressure and under 40MPa pressure, be heated to 375 ℃ with 50 ℃/hour temperature rise rate again, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained the ptfe composite finished product.The friction and wear behavior test-results sees Table 1.
Embodiment 2:
Present embodiment provides a kind of ptfe composite, and this matrix material contains the tetrafluoroethylene of 67wt% and the vertical structure polyacrylonitrile of height of 33wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 52% through the nucleus magnetic resonance test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material is the percentage composition meter by weight, polytetrafluorethylepowder powder with 40% (granularity is 50 μ m), 20% vinyl cyanide and 40% urea (granularity 100 μ m) mix and form mixture and add in the reaction flask,-70 ℃ of lower cryogenic freezings 170 hours, in reaction flask, add afterwards liquid nitrogen, carry out Co
60Gamma-ray irradiation, irradiation dose is 25kGy, in the environment with-70 ℃ ± 5 ℃ of reaction flask immigrations behind the irradiation, carry out polymerization after 8 hours, remove urea and unreacting propylene nitrile monomer, filtration, drying with the water repetitive scrubbing, kept 10 minutes in coldmoulding under the 40MPa pressure and under 40MPa pressure, be heated to 350 ℃ with 80 ℃/hour temperature rise rate again, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained the ptfe composite finished product.The friction and wear behavior test-results sees Table 1.
Embodiment 3:
Present embodiment provides a kind of ptfe composite, and this matrix material contains the tetrafluoroethylene of 83wt% and the vertical structure polyacrylonitrile of height of 17wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 71% through the carbon-13 nmr spectra test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material is the percentage composition meter by weight, polytetrafluorethylepowder powder with 55% (granularity is 150 μ m), 15% vinyl cyanide and 30% urea (granularity is 200 μ m) mix and form mixture and add in the reaction flask,-70 ℃ of lower cryogenic freezings 170 hours, in reaction flask, add afterwards liquid nitrogen, carry out Co
60Gamma-ray irradiation, irradiation dose is 8kGy, in the environment with-70 ℃ ± 5 ℃ of reaction flask immigrations behind the irradiation, after carrying out polyase 13 hour, remove urea and unreacting propylene nitrile monomer, filtration, drying with the water repetitive scrubbing, kept 5 minutes in coldmoulding under the 40MPa pressure and under 40MPa pressure, be heated to 330 ℃ with 100 ℃/hour temperature rise rate again, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained the ptfe composite finished product.The friction and wear behavior test-results sees Table 1.
Embodiment 4:
Present embodiment provides a kind of ptfe composite, and this matrix material contains the tetrafluoroethylene of 72wt% and the vertical structure polyacrylonitrile of height of 28wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 58% through the carbon-13 nmr spectra test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material is the percentage composition meter by weight, polytetrafluorethylepowder powder with 50% (granularity is 50 μ m), 20% vinyl cyanide and 30% urea (granularity is 100 μ m) mix and form mixture and add in the reaction flask,-60 ℃ of lower cryogenic freezings 150 hours, in reaction flask, add afterwards liquid nitrogen, carry out Co
60Gamma-ray irradiation, irradiation dose is 20kGy, in the environment with-70 ℃ ± 5 ℃ of reaction flask immigrations behind the irradiation, carry out polymerization after 8 hours, remove urea and unreacting propylene nitrile monomer, filtration, drying with the water repetitive scrubbing, kept 5 minutes in coldmoulding under the 40MPa pressure and under 40MPa pressure, be heated to 360 ℃ with 30 ℃/hour temperature rise rate again, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained the ptfe composite finished product.The friction and wear behavior test-results sees Table 1.
Friction and wear behavior test-results such as the table 1 of above embodiment 1～4 prepared ptfe composite are compared with unmodified polytetrafluoroethylmaterial material, and its wear resistance has improved 100～150 times.
Table 1
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (7)
1. a ptfe composite is characterized in that, this matrix material contains the tetrafluoroethylene of 65wt%～85wt% and the vertical structure polyacrylonitrile of height of 15wt%～35wt%, and isotactic triad (mm) content of the vertical structure polyacrylonitrile of described height is 45%～78%.
2. matrix material according to claim 1 is characterized in that, described matrix material prepares by the following method, comprising:
Each component is the percentage composition meter by weight, and the tetrafluoroethylene with 30%～60%, 15%～25% vinyl cyanide and 30%～50% urea mix the formation mixture,
With described mixture-75 ℃～-50 ℃ cryogenic freezings more than 120 hours;
Described mixture after freezing is dispersed in the liquid nitrogen, carries out Co
60Gamma-ray irradiation, radiation dose are 3～30kGy;
In-70 ℃ ± 5 ℃ environment, make vinyl cyanide in the described mixture carry out polyase 13～10 hour behind the irradiation;
After the polyreaction, remove urea and unreacting propylene nitrile monomer, filtration, drying with the described mixture of water repetitive scrubbing, in coldmoulding under the 40MPa pressure and under 40MPa pressure, kept 5～10 minutes;
The sample of compression moulding is inserted in the high temperature sintering furnace, be heated to 330 ℃～380 ℃ with 30 ℃～100 ℃/hour temperature rise rates, heat preservation sintering 2 hours;
Naturally cool to room temperature, namely obtain ptfe composite.
3. matrix material according to claim 2 is characterized in that, the granularity of described urea is less than 400 μ m.
4. matrix material according to claim 1 and 2 is characterized in that, it is the polytetrafluorethylepowder powder of 30 μ m～200 μ m that described tetrafluoroethylene adopts granularity.
5. the preparation method of a ptfe composite is characterized in that, comprising:
Step 1, each component is the percentage composition meter by weight, and the tetrafluoroethylene with 30%～60%, 15%～25% vinyl cyanide and 30%～50% urea mix the formation mixture,
Step 2, with described mixture-75 ℃～-50 ℃ cryogenic freezings more than 120 hours;
Step 3 is dispersed in the described mixture after freezing in the liquid nitrogen, carries out Co
60Gamma-ray irradiation, radiation dose are 3～30kGy;
Step 4 makes vinyl cyanide in the described mixture carry out polyase 13～10 hour in-70 ℃ ± 5 ℃ environment behind the irradiation;
Step 5 after the polyreaction, is removed urea and unreacting propylene nitrile monomer, filtration, drying with the described mixture of water repetitive scrubbing, in coldmoulding under the 40MPa pressure and kept under 40MPa pressure 5～10 minutes;
Step 6 is inserted the sample of compression moulding in the high temperature sintering furnace, is heated to 330 ℃～380 ℃ with 30 ℃～100 ℃/hour temperature rise rates, heat preservation sintering 2 hours;
Step 7 naturally cools to room temperature, namely obtains ptfe composite.
6. method according to claim 5 is characterized in that, the granularity of described urea is less than 400 μ m.
7. according to claim 5 or 6 described methods, it is characterized in that it is the polytetrafluorethylepowder powder of 30 μ m～200 μ m that described tetrafluoroethylene adopts granularity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014161112A1 (en) * | 2013-04-03 | 2014-10-09 | 太仓金凯特种线缆有限公司 | METHOD FOR PREPARING PTFE SUPERFINE POWDER BY COMBINING γ RAYS WITH OZONE AND CARBON TETRACHLORIDE |
| WO2014161113A1 (en) * | 2013-04-03 | 2014-10-09 | 太仓金凯特种线缆有限公司 | Method for preparing ptfe superfine powder by combining ultraviolet rays with ozone and hydrogen peroxide |
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| EP0226922A2 (en) * | 1985-12-21 | 1987-07-01 | Bayer Ag | Process for preparing thermoplastic molding compositions with flame-retarding properties |
| CN1786070A (en) * | 2005-11-24 | 2006-06-14 | 中国科学技术大学 | High abrasive resistance poly tetra fluoro ethylene composite material and its preparation method |
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2012
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| EP0226922A2 (en) * | 1985-12-21 | 1987-07-01 | Bayer Ag | Process for preparing thermoplastic molding compositions with flame-retarding properties |
| CN1786070A (en) * | 2005-11-24 | 2006-06-14 | 中国科学技术大学 | High abrasive resistance poly tetra fluoro ethylene composite material and its preparation method |
Non-Patent Citations (2)
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| 肖高军等: ""以聚四氟乙烯乳胶粒子为种子的丙烯腈/苯乙烯乳液共聚合"", 《化学反应工程与工艺》, vol. 26, no. 01, 28 February 2010 (2010-02-28), pages 64 - 68 * |
| 葛学武，张志成: ""辐射引发丙烯腈聚合研究进展"", 《辐射研究与辐射工艺学报》, vol. 13, no. 04, 10 November 1995 (1995-11-10) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014161112A1 (en) * | 2013-04-03 | 2014-10-09 | 太仓金凯特种线缆有限公司 | METHOD FOR PREPARING PTFE SUPERFINE POWDER BY COMBINING γ RAYS WITH OZONE AND CARBON TETRACHLORIDE |
| WO2014161113A1 (en) * | 2013-04-03 | 2014-10-09 | 太仓金凯特种线缆有限公司 | Method for preparing ptfe superfine powder by combining ultraviolet rays with ozone and hydrogen peroxide |
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Denomination of invention: Polytetrafluoroethylene composite material and its preparation method Effective date of registration: 20230816 Granted publication date: 20150114 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: GESHAN CONSTRUCTION GROUP Co.,Ltd. Registration number: Y2023980052356 |