CN102924854B - Teflon composite material and preparation method thereof - Google Patents
Teflon composite material and preparation method thereof Download PDFInfo
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- CN102924854B CN102924854B CN201210437295.XA CN201210437295A CN102924854B CN 102924854 B CN102924854 B CN 102924854B CN 201210437295 A CN201210437295 A CN 201210437295A CN 102924854 B CN102924854 B CN 102924854B
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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 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 the chemical stability of its excellence, high thermal resistance, anti-ultraviolet radiation and low frictional coefficient, but it wears no resistance and but limits its use range.In order to improve the wear resisting property of polytetrafluoroethylmaterial material, technology in the past mainly in tetrafluoroethylene filler metal and glass fibre, carbon fiber etc. prepare ptfe composite.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 CN100582158C patent, add metal and metal oxide etc. in addition, it improves the wear resistance of tetrafluoroethylene to a certain extent, but wherein polyacrylonitrile powder addition is larger, and metallics and tetrafluoroethylene lack consistency, easy generation is separated, and reduces its mechanical property.
Summary of the invention
The object of embodiment of the present invention is to provide a kind of ptfe composite and preparation method thereof, this ptfe composite wear resisting property is good, consistency is high, preparation time sintering temperature low, current polytetrafluoroethylmaterial material can be solved wear no resistance, the low technical problem causing mechanism performance bad of consistency.
The object of the invention is to be achieved through the following technical solutions:
Embodiment of the present invention provides a kind of ptfe composite, the height of tetrafluoroethylene and 15wt% ~ 35wt% that this matrix material contains 65wt% ~ 85wt% founds structure polyacrylonitrile, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 45% ~ 78%.
Embodiment of the present invention also provides a kind of preparation method of ptfe composite, comprising:
Step 1, each component weight percentage, by the tetrafluoroethylene of 30% ~ 60%, the vinyl cyanide of 15% ~ 25% and 30% ~ 50% urea mix formation mixture,
Step 2, by described mixture-75 DEG C ~-50 DEG C cryogenic freezings more than 120 hours;
Step 3, is dispersed in liquid nitrogen by the described mixture after freezing, carries out Co
60gamma-ray irradiation, radiation dose is 3 ~ 30kGy;
Step 4, makes the vinyl cyanide in described mixture carry out polyase 13 ~ 10 hour in the environment of-70 DEG C ± 5 DEG C after irradiation;
Step 5, after polyreaction, with mixture removing urea described in water repetitive scrubbing and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 5 ~ 10 minutes under 40MPa pressure;
Step 6, inserts in high temperature sintering furnace by the sample of compression moulding, is heated to 330 DEG C ~ 380 DEG C with the temperature rise rate of 30 DEG C ~ 100 DEG C/h, heat preservation sintering 2 hours;
Step 7, naturally cools to room temperature, namely obtains ptfe composite.
As can be seen from the above-mentioned technical scheme provided, the ptfe composite that embodiment of the present invention provides, at the high vertical structure polyacrylonitrile of polytetrafluorethylepowder powder situ synthesis, its isotactic triad (mm) content is 45% ~ 78%, high vertical structure polyacrylonitrile is present in polytetrafluoroethylmaterial material with grafting and blended mode, content is only 15wt% ~ 35wt%, makes the consistency of this material good.Can there is cyclization in high vertical structure polyacrylonitrile, form ladder structure, the friction transfer enhancing matrix material is rubbed at the sticking power to surface, face of rubbing, thus greatly improves its wear resistance in high-temperature sintering process.Actual measurement shows, under identical friction testing condition, abrasion loss containing high vertical structure polyacrylonitrile high-wearing polytetrafluoroethylcomposite composite material is 1/150 ~ 1/100 of unmodified tetrafluoroethylene, can reach more than 300 DEG C containing high vertical structure polyacrylonitrile high-wearing polytetrafluoroethylcomposite composite material heatproof simultaneously.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
The embodiment of the present invention provides a kind of ptfe composite, the height of tetrafluoroethylene and 15wt% ~ 35wt% that this matrix material contains 65wt% ~ 85wt% founds structure polyacrylonitrile, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 45% ~ 78%.
The preparation method of above-mentioned ptfe composite, comprises the following steps:
Step 1, each component weight percentage, by the tetrafluoroethylene of 30% ~ 60%, the vinyl cyanide of 15% ~ 25% and 30% ~ 50% urea mix formation mixture,
Step 2, by described mixture-75 DEG C ~-50 DEG C cryogenic freezings more than 120 hours;
Step 3, is dispersed in liquid nitrogen by the described mixture after freezing, carries out Co
60gamma-ray irradiation, radiation dose is 3 ~ 30kGy;
Step 4, makes the vinyl cyanide in described mixture carry out polyase 13 ~ 10 hour in the environment of-70 DEG C ± 5 DEG C after irradiation;
Step 5, after polyreaction, with mixture removing urea described in water repetitive scrubbing and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 5 ~ 10 minutes under 40MPa pressure;
Step 6, inserts in high temperature sintering furnace by the sample of compression moulding, is heated to 330 DEG C ~ 380 DEG C with the temperature rise rate of 30 DEG C ~ 100 DEG C/h, 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 μm.
Above-mentioned tetrafluoroethylene employing granularity is the polytetrafluorethylepowder powder of 30 μm ~ 200 μm.
Provide several embodiment the following detailed description of the present invention, friction and wear behavior test is carried out on MM2200 type ring-block abrasion tester, and test is undertaken by GB 3960-83 " plastic slide friction wear test method ".
Embodiment 1:
The present embodiment provides a kind of ptfe composite, and the height of tetrafluoroethylene and 21wt% that this matrix material contains 79wt% founds structure polyacrylonitrile, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 63% through carbon-13 nmr spectra test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material weight percentage, polytetrafluorethylepowder powder (granularity is 50 μm) by 50%, the vinyl cyanide of 15% and 35% urea (granularity is 100 μm) mix formed mixture add in reaction flask, cryogenic freezing 120 hours at-50 DEG C, in reaction flask, add liquid nitrogen afterwards, carry out Co
60gamma-ray irradiation, irradiation dose is 15kGy, reaction flask is moved in the environment of-70 DEG C ± 5 DEG C after irradiation, carry out polymerization after 10 hours, with water repetitive scrubbing removing urea and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 8 minutes under 40MPa pressure, then is heated to 375 DEG C with the temperature rise rate of 50 DEG C/h, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained ptfe composite finished product.Friction and wear behavior test-results is in table 1.
Embodiment 2:
The present embodiment provides a kind of ptfe composite, and the height of tetrafluoroethylene and 33wt% that this matrix material contains 67wt% founds structure polyacrylonitrile, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 52% through nucleus magnetic resonance test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material weight percentage, polytetrafluorethylepowder powder (granularity is 50 μm) by 40%, the vinyl cyanide of 20% and 40% urea (granularity 100 μm) mix formed mixture add in reaction flask, cryogenic freezing 170 hours at-70 DEG C, in reaction flask, add liquid nitrogen afterwards, carry out Co
60gamma-ray irradiation, irradiation dose is 25kGy, reaction flask is moved in the environment of-70 DEG C ± 5 DEG C after irradiation, carry out polymerization after 8 hours, with water repetitive scrubbing removing urea and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 10 minutes under 40MPa pressure, then is heated to 350 DEG C with the temperature rise rate of 80 DEG C/h, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained ptfe composite finished product.Friction and wear behavior test-results is in table 1.
Embodiment 3:
The present embodiment provides a kind of ptfe composite, and the height of tetrafluoroethylene and 17wt% that this matrix material contains 83wt% founds structure polyacrylonitrile, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 71% through carbon-13 nmr spectra test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material weight percentage, polytetrafluorethylepowder powder (granularity is 150 μm) by 55%, the vinyl cyanide of 15% and 30% urea (granularity is 200 μm) mix formed mixture add in reaction flask, cryogenic freezing 170 hours at-70 DEG C, in reaction flask, add liquid nitrogen afterwards, carry out Co
60gamma-ray irradiation, irradiation dose is 8kGy, reaction flask is moved in the environment of-70 DEG C ± 5 DEG C after irradiation, after carrying out polyase 13 hour, with water repetitive scrubbing removing urea and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 5 minutes under 40MPa pressure, then is heated to 330 DEG C with the temperature rise rate of 100 DEG C/h, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained ptfe composite finished product.Friction and wear behavior test-results is in table 1.
Embodiment 4:
The present embodiment provides a kind of ptfe composite, and the height of tetrafluoroethylene and 28wt% that this matrix material contains 72wt% founds structure polyacrylonitrile, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 58% through carbon-13 nmr spectra test.
The preparation method of above-mentioned ptfe composite is as follows:
Each raw material weight percentage, polytetrafluorethylepowder powder (granularity is 50 μm) by 50%, the vinyl cyanide of 20% and 30% urea (granularity is 100 μm) mix formed mixture add in reaction flask, cryogenic freezing 150 hours at-60 DEG C, in reaction flask, add liquid nitrogen afterwards, carry out Co
60gamma-ray irradiation, irradiation dose is 20kGy, reaction flask is moved in the environment of-70 DEG C ± 5 DEG C after irradiation, carry out polymerization after 8 hours, with water repetitive scrubbing removing urea and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 5 minutes under 40MPa pressure, then is heated to 360 DEG C with the temperature rise rate of 30 DEG C/h, heat preservation sintering naturally cooled to room temperature after 2 hours, namely obtained ptfe composite finished product.Friction and wear behavior test-results is in table 1.
The friction and wear behavior test-results of the ptfe composite obtained by above embodiment 1 ~ 4 is as table 1, and compared with unmodified polytetrafluoroethylmaterial material, its wear resistance improves 100 ~ 150 times.
Table 1
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change 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 (6)
1. a ptfe composite, it is characterized in that, this matrix material founds structure polyacrylonitrile by the tetrafluoroethylene of 72wt% ~ 85wt% and the height of 15wt% ~ 28wt% and forms, and isotactic triad (mm) content that described height founds structure polyacrylonitrile is 45% ~ 78%;
Described matrix material is prepared by the following method, comprising:
Each component weight percentage, by the tetrafluoroethylene of 30% ~ 60%, the vinyl cyanide of 15% ~ 25% and 30% ~ 50% urea mix formation mixture,
By described mixture-75 DEG C ~-50 DEG C cryogenic freezings more than 120 hours;
Described mixture after freezing is dispersed in liquid nitrogen, carries out C
o 60gamma-ray irradiation, radiation dose is 3 ~ 30kGy;
In the environment of-70 DEG C ± 5 DEG C, make the vinyl cyanide in described mixture carry out polyase 13 ~ 10 hour after irradiation;
After polyreaction, with mixture removing urea described in water repetitive scrubbing and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 5 ~ 10 minutes under 40MPa pressure;
The sample of compression moulding is inserted in high temperature sintering furnace, is heated to 330 DEG C ~ 380 DEG C with the temperature rise rate of 30 DEG C ~ 100 DEG C/h, heat preservation sintering 2 hours;
Naturally cool to room temperature, namely obtain ptfe composite.
2. matrix material according to claim 1, is characterized in that, the granularity of described urea is less than 400 μm.
3. matrix material according to claim 1, is characterized in that, described tetrafluoroethylene employing granularity is the polytetrafluorethylepowder powder of 30 μm ~ 200 μm.
4. a preparation method for ptfe composite as claimed in claim 1, is characterized in that, comprising:
Step 1, each component weight percentage, by the tetrafluoroethylene of 30% ~ 60%, the vinyl cyanide of 15% ~ 25% and 30% ~ 50% urea mix formation mixture;
Step 2, by described mixture-75 DEG C ~-50 DEG C cryogenic freezings more than 120 hours;
Step 3, is dispersed in liquid nitrogen by the described mixture after freezing, carries out Co
60gamma-ray irradiation, radiation dose is 3 ~ 30kGy;
Step 4, makes the vinyl cyanide in described mixture carry out polyase 13 ~ 10 hour in the environment of-70 DEG C ± 5 DEG C after irradiation;
Step 5, after polyreaction, with mixture removing urea described in water repetitive scrubbing and unreacting propylene nitrile monomer, filtration, drying, coldmoulding under 40MPa pressure also keeps 5 ~ 10 minutes under 40MPa pressure;
Step 6, inserts in high temperature sintering furnace by the sample of compression moulding, is heated to 330 DEG C ~ 380 DEG C with the temperature rise rate of 30 DEG C ~ 100 DEG C/h, heat preservation sintering 2 hours;
Step 7, naturally cools to room temperature, namely obtains ptfe composite.
5. method according to claim 4, is characterized in that, the granularity of described urea is less than 400 μm.
6. the method according to claim 4 or 5, is characterized in that, described tetrafluoroethylene employing granularity is the polytetrafluorethylepowder powder of 30 μm ~ 200 μm.
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| CN103191818B (en) * | 2013-04-03 | 2016-02-24 | 太仓金凯特种线缆有限公司 | Gamma-rays combined with ozone and carbon tetrachloride prepare the method for ultrafine PTFE powder |
| CN103170400B (en) * | 2013-04-03 | 2016-02-24 | 太仓金凯特种线缆有限公司 | The method of ultrafine PTFE powder prepared by ultraviolet combined 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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)
| Title |
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| "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";肖高军等;《化学反应工程与工艺》;20100228;第26卷(第01期);第64-68页 * |
| 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》.1995,第13卷(第04期),第197页第3.2节. * |
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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 |