CN101440163B - Preparation of polytetrafluorethylene nano-microsphere - Google Patents
Preparation of polytetrafluorethylene nano-microsphere Download PDFInfo
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- CN101440163B CN101440163B CN2007101885799A CN200710188579A CN101440163B CN 101440163 B CN101440163 B CN 101440163B CN 2007101885799 A CN2007101885799 A CN 2007101885799A CN 200710188579 A CN200710188579 A CN 200710188579A CN 101440163 B CN101440163 B CN 101440163B
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Abstract
The invention discloses a method for preparing polyfluortetraethylene nano-microspheres. The method comprises the following steps of preparing fluorination carbon nano-tubes from hydroxylation carbon nano-tubes and then mixing the fluorination carbon nano-tubes with tetrafluoroethylene powder so as to prepare the polyfluortetraethylene nano-microspheres. Through an SEM photograph with the amplification factor of twenty thousands times, the polyfluortetraethylene nano-microspheres prepared by the method have spherical appearance and have the average particle size between 90 and 120 nanometers.
Description
Technical field
The present invention relates to a kind of preparation method of polytetrafluorethylenano nano-microsphere.
Background technology
Nanometer polytetrafluoroethylcomposite is a kind of good solid lubricant, and its streamlined structure and extremely low molcohesion make the intermolecular relatively sliding that is easy to, thereby demonstrate extremely low frictional coefficient.Under high temperature or high pressure, nanometer polytetrafluoroethylcomposite particle and the metallic surface generation metal fluoride that reacts, therefore on friction surface, form and contain nanometer polytetrafluoroethylcomposite particle and the deposited film of metallic surface, thereby reduced wearing and tearing because of the generation compound that friction chemical reaction generated.The nanometer polytetrafluoroethylcomposite particle plays the antifriction function except generating deposited film, can also make filling and leading up pit and being absorbed in the matrix effect and being strengthened of conventional particle.In addition, because nanometer polytetrafluoroethylcomposite particulate hardness, toughness and Young's modulus increase to some extent than its conventional granulates, on contact surface, can play the effect of similar bearing, thereby reduce the friction and wear between friction pair.
Nanometer polytetrafluoroethylcomposite is the preparation method mainly contain: 1) use emulsion synthesis method synthetic PTFE particle size in 50～150nm scope, average particle diameter is 100nm (E.Fern ' andez Rico, I.Minondo, D.Garc ' ia Cuervo, The effectiveness of PTFE nanoparticle powder as an EP additive tomineral base oils, Wear 262 (2007) 1399-1406); 2) use microemulsion synthesis method synthetic nanometer polytetrafluoroethylcomposite particle dia generally between 10～80nm, the appropriate change reaction conditions can obtain particle (the Bladel.AqueousDispersion of Fluoropolymers Its Preparationand Usefor Coating.US Patent:5576381 of 10～60nm, 1996211219), and main nanometer polytetrafluoroethylcomposite preparation method only limits to a few countries (Wu S.Microemulsion of PolytetrafluoroethyleneParticles.US Patent:5616648 at present, 19962225.Giannetti E, Visca M.Process for thePolymerization in A2 queous Dispersion of Fluorinated Monomers.US Patent:4864006,198721023.), and synthetic method is comparatively complicated, therefore can not be by widespread usage.And for the preparation method of polytetrafluorethylenano nano-microsphere, rare at present report.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polytetrafluorethylenano nano-microsphere, it is simpler that this method has production technique, and the control of the dissemination by carbon nanotube nano particle is the spheric characteristics.
A kind of preparation method of polytetrafluorethylenano nano-microsphere is characterized in that this method may further comprise the steps successively:
A, hydroxylation carbon nanotube and Perfluorocaprylic Acid are mixed to join N, among the N '-dimethyl formamide (DMF), behind the ultra-sonic dispersion, in stirring, drip sulphuric acid soln, carry out the heated and stirred reaction; After finishing reaction, through water filtration, vacuum-drying obtains carbon fluoride nano-tube;
B, carbon fluoride nano-tube and tetrafluoroethylene powder mixes join in the dispersion solvent chloroform, ultra-sonic dispersion, and volatilization removes and desolvates, and drying obtains polytetrafluorethylenano nano-microsphere.
In steps A, the mass ratio of hydroxylation carbon nanotube and Perfluorocaprylic Acid is 0.1: 1～2.
In steps A, the temperature of heated and stirred reaction is 80～85 ℃.
In step B, the mass ratio of carbon fluoride nano-tube and tetrafluoroethylene powder is 1: 2～3.
The invention has the advantages that: add carbon fluoride nano-tube in the preparation process and can strengthen its dissemination in chloroform, to reach the purpose of control ball shaped nano coating of particles and particle diameter.This method is comparatively simple, and the product pattern is spherical, and granularity is comparatively even.
According to the polytetrafluorethylenano nano-microsphere of the present invention's preparation, by 20,000 times of magnification SEM photos, pattern is spherical, and median size is at 90～120nm.
Embodiment
Embodiment 1:
0.5 gram hydroxylation carbon nanotube and 5 gram Perfluorocaprylic Acids are mixed to join N by mass ratio, among the N '-dimethyl formamide (DMF), behind the ultra-sonic dispersion 30min, the sulphuric acid soln with 10mL 20% in stirring is added drop-wise in the above-mentioned dispersion system, and heated and stirred; After reaction finished, through water filtration, vacuum-drying obtained carbon fluoride nano-tube.Then gained carbon fluoride nano-tube and 1.5 gram tetrafluoroethylene powder are mixed to join in the dispersion solvent chloroform with mass ratio, and ultra-sonic dispersion 1 hour, drying obtains polytetrafluorethylenano nano-microsphere, and particle diameter is at 90～110nm.
Embodiment 2:
0.5 gram hydroxylation carbon nanotube and 5 gram Perfluorocaprylic Acids are mixed to join N by mass ratio, among the N '-dimethyl formamide (DMF), behind the ultra-sonic dispersion 30min, the sulphuric acid soln with 10mL 20% in stirring is added drop-wise in the above-mentioned dispersion system, and heated and stirred; After reaction finished, through water filtration, vacuum-drying obtained carbon fluoride nano-tube.Then gained carbon fluoride nano-tube and 1.0 gram tetrafluoroethylene powder are mixed to join in the dispersion solvent chloroform with mass ratio, and ultra-sonic dispersion 1 hour, drying obtains polytetrafluorethylenano nano-microsphere, and particle diameter is at 110～120nm.
Embodiment 3:
0.5 gram hydroxylation carbon nanotube and 8 gram Perfluorocaprylic Acids are mixed to join N by mass ratio, among the N '-dimethyl formamide (DMF), behind the ultra-sonic dispersion 30min, the sulphuric acid soln with 10mL 20% in stirring is added drop-wise in the above-mentioned dispersion system, and heated and stirred; After reaction finished, through water filtration, vacuum-drying obtained carbon fluoride nano-tube.Then gained carbon fluoride nano-tube and 0.5 gram tetrafluoroethylene powder are mixed to join in the dispersion solvent chloroform with mass ratio, and ultra-sonic dispersion 1 hour, drying obtains polytetrafluorethylenano nano-microsphere, and particle diameter is at 90～100nm.
Claims (3)
1. the preparation method of a polytetrafluorethylenano nano-microsphere is characterized in that this method may further comprise the steps successively:
A, hydroxylation carbon nanotube and Perfluorocaprylic Acid are mixed to join N, in N '-dimethyl formamide, behind the ultra-sonic dispersion, in stirring, drip sulphuric acid soln, carry out the heated and stirred reaction; After finishing reaction, through water filtration, vacuum-drying obtains carbon fluoride nano-tube; Wherein the mass ratio of hydroxylation carbon nanotube and Perfluorocaprylic Acid is 0.1: 1～2.
B, carbon fluoride nano-tube and tetrafluoroethylene powder mixes join in the dispersion solvent chloroform, ultra-sonic dispersion, and volatilization removes and desolvates, and drying obtains polytetrafluorethylenano nano-microsphere.
2. the method for claim 1 is characterized in that in steps A, and the temperature of heated and stirred reaction is 80～85 ℃.
3. the method for claim 1 is characterized in that in step B, and the mass ratio of carbon fluoride nano-tube and tetrafluoroethylene powder is 1: 2～3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101885799A CN101440163B (en) | 2007-11-22 | 2007-11-22 | Preparation of polytetrafluorethylene nano-microsphere |
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| CN2007101885799A CN101440163B (en) | 2007-11-22 | 2007-11-22 | Preparation of polytetrafluorethylene nano-microsphere |
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| CN101440163A CN101440163A (en) | 2009-05-27 |
| CN101440163B true CN101440163B (en) | 2011-04-27 |
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| CN2007101885799A Expired - Fee Related CN101440163B (en) | 2007-11-22 | 2007-11-22 | Preparation of polytetrafluorethylene nano-microsphere |
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| CN105820412A (en) * | 2016-04-20 | 2016-08-03 | 安徽中宏线缆有限公司 | Anti-static nano magnesium oxide doped polyethylene DC (direct current) cable composite material and preparation method thereof |
| CN105860197A (en) * | 2016-04-20 | 2016-08-17 | 安徽中宏线缆有限公司 | High-toughness nano magnesium oxide doped polyethylene DC (Direct Current) cable composite material and preparation method thereof |
| CN105778233A (en) * | 2016-04-20 | 2016-07-20 | 安徽中宏线缆有限公司 | High-strength nanometer magnesia doped polyethylene direct-current cable composite material and preparing method thereof |
| CN105860250A (en) * | 2016-04-20 | 2016-08-17 | 安徽中宏线缆有限公司 | Pollution-proof nano magnesium oxide doped polyethylene direct-current cable composite material and preparation method thereof |
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