CN105175991A - Preparation method of high strength polyether ether ketone composite material - Google Patents
Preparation method of high strength polyether ether ketone composite material Download PDFInfo
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- CN105175991A CN105175991A CN201410262746.XA CN201410262746A CN105175991A CN 105175991 A CN105175991 A CN 105175991A CN 201410262746 A CN201410262746 A CN 201410262746A CN 105175991 A CN105175991 A CN 105175991A
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Abstract
The invention relates to a preparation method of a high strength PEEK composite material. An inorganic filler and remodified carbon fibers are blended with PEEK through a melt extrusion technology to form the high strength PEEK composite material with a high performance utilization rate.
Description
Technical field
The invention belongs to PEEK special engineering plastics field, relate to a kind of preparation method utilizing special coupling agent treatment carbon fiber and inorganic filler to strengthen PEEK.
Background technology
Polyether-ether-ketone (PEEK) is a kind of thermoplastic engineering plastic of all aromatic hemicrystalline, due to the phenyl ring containing rigidity on macromolecular chain, submissive ehter bond and the carbonyl improving Intermolecular Forces, compound with regular structure, thus has the over-all properties that high heat resistance, high strength, high-modulus, high-fracture toughness etc. are excellent.Also there is the features such as insulation, hydrolysis, capability of resistance to radiation be strong, be with a wide range of applications at many engineering fields.But nowadays scientific and technological develop rapidly, the performance requriements of material is also being improved constantly, especially aerospace field, the while of requiring lightweight, also require high strength and modulus, a lot of fields require very high heat-drawn wire, and these to be all pure PEEK resin be beyond one's reach, so must carry out enhancement process to it.
The Main way that wherein fiber reinforcement PEEK matrix material, especially fibre reinforced PEEK matrix material will be following PEEK modification.But the surface due to carbon fibre is wetting ability, and resin-based consistency is bad.Although traditional silane coupling agent etc. can the consistency of the obvious fine and resin of carbon modified, its temperature classification is low, in structure and PEEK difference comparatively greatly, cannot play compatibilization, so cause the problem of fibre reinforced utilization ratio deficiency, namely reinforced effects is undesirable.Therefore we carry out primary treatment by plasma modification method to carbon fiber, strengthen its surfactivity, ensure the consistency of carbon fiber and resin by preparing resistant to elevated temperatures silane coupling agent simultaneously, and both characteristics are utilized efficiently.Simultaneously in order to meet some specific demands, add inorganic filler wherein, with the rigidity of reinforced composite.
Summary of the invention
The object of the present invention is to provide a kind of preparation method utilizing special coupling agent treatment fibre reinforced PEEK, by utilizing special high temperature resistant silane coupling agent, twice-modified process is carried out to the carbon fiber carrying out plasma modification, strengthen surfactivity, undertaken blended by extrusion by melting and the PEEK that with the addition of inorganic filler, form the enhancing PEEK matrix material of carbon fiber high utilization rate, wherein inorganic fillings is made up of by weight 2:1:1 glass fibre, talcum powder, calcium carbonate superfine powder.Concrete steps are as follows:
One, the pre-treatment of carbon fiber
First atmospheric plasma fluidics is adopted to carry out surface treatment to carbon fiber, with the mixed gas of helium and oxygen as generation gas, helium is as inert carrier gas, oxygen is as the reactive gas added, helium gas flow is 20L/min, oxygen flow is 0.4L/min, the helium used and oxygen for purity be the high-pure gas of 99.99%, the power setting of equipment is 100W.
Then titanic acid ester, biphenyl dianhydride, allyl amine and triethoxyl silane is selected to be that coupling agent prepared by raw material, pass through imidization reaction, and obtain special high temperature resistant silane coupling agent with the physical mixed of titanic acid ester, carry out twice-modified by gas-liquid economic benefits and social benefits method to the carbon fiber carrying out plasma modification.
Three, carbon fiber and PEEK resin is blended
By PEEK, inorganic filler, special coupling agent and treated short carbon fibre of cutting add first, second, third Weightlessness balance respectively, PEEK, inorganic filler and special coupling agent is added from main spout, carbon fibre is added from the second side spout, by each component concentration in Weightlessness balance fine adjustment formula, processing temperature is from 320 DEG C to 380 DEG C.
Namely the material strip extruded is obtained the fine reinforced polyether ether ketone matrix material of high strength carbon of the present invention through travelling belt transmission, air cold cut, pelletizing.
Embodiment
As no specific instructions, various raw material of the present invention all can be obtained by commercially available; Or prepare according to the ordinary method of this area.Unless otherwise defined or described herein, all specialties used herein and scientific words and those skilled in the art the same meaning be familiar with.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
Below in conjunction with specific embodiment, set forth the present invention further.These embodiments are only not used in for illustration of the present invention and limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or carry out according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all numbers are weight part, and all per-cent is weight percentage, and described polymericular weight is number-average molecular weight.
Step 1,
The surface treatment of carbon fiber used in following examples, treatment step is as follows: the Atmoflo-250 atmospheric plasma equipment adopting SurfxTechnologies company of the U.S. to produce processes PAN base carbon fibre.Under normal pressure open environment, use the mixed gas of helium and oxygen as generation gas, the power setting of equipment is 100W, and temperature is 60 degree, to reach a modification of carbon fiber.Carbon fiber after process is undertaken twice-modified with special high temperature resistant silane coupling agent by gas-liquid economic benefits and social benefits method.Wherein coupling agent preparation selects titanic acid ester, biphenyl dianhydride, allyl amine and triethoxyl silane to be raw material, by imidization reaction, and obtains special high temperature resistant coupling agent with the physical mixed of titanic acid ester.
Step 2,
The each process section temperature of setting twin screw extruder is 320 DEG C, 340 DEG C, 355 DEG C, 355 DEG C, 355 DEG C, 355 DEG C, 355 DEG C, 355 DEG C, 350 DEG C, 340 DEG C, after temperature reaches set(ting)value, first the first Weightlessness balance is opened, PEEK powder is added from main spout with the rate of feeding of 20Kg/h, wherein PEEK melting means is 219/10min, after die extrusion PEEK, open the second Weightlessness balance, inorganic filler and special coupling agent is added with the speed of 0.45Kg/h, after machine to be extruded operates steadily, open side feeding and the 3rd Weightlessness balance, add with the speed of 2.27Kg/h and shortly cut carbon fibre, controlling twin screw rotating speed is 300-500Rad/min, moment of torsion is no more than 80%, head melt temperature is no more than 400 DEG C, obtain PEEK content 88%, inorganic fill agent content 5%, the matrix material of the fine content 10% of carbon.Adjustment feeding parameter, obtain different formulas, formula is in table 1, and each performance formula is in table 2.
The content of each component of table 1 different ingredients
| Formula 1 | Formula 2 | Formula 3 | Formula 4 | Formula 5 | |
| Raw material | Consumption (part) | Consumption (part) | Consumption (part) | Consumption (part) | Consumption (part) |
| PEEK | 78 | 63 | 48 | 60 | 55 |
| Carbon is fine | 10 | 20 | 30 | 15 | 25 |
| Coupling agent | 2 | 2 | 2 | 5 | 5 |
| Weighting agent | 10 | 15 | 20 | 20 | 15 |
Table 2 different ingredients Performance comparision
| Formula 1 | Formula 2 | Formula 3 | Formula 4 | Formula 5 | |
| Tensile modulus (GPa) | 5.8 | 7.9 | 12.4 | 6.5 | 8.9 |
| Tensile strength (MPa) | 135 | 167 | 213 | 144 | 183 |
| Modulus in flexure (MPa) | 6.1 | 8.4 | 13.7 | 7.7 | 9.8 |
| Flexural strength (MPa) | 191 | 233 | 289 | 207 | 252 |
| Heat-drawn wire (DEG C) | 229 | 258 | 291 | 238 | 278 |
As can be seen from table, fine and the inorganic filler of high strength carbon add the intensity and thermotolerance that can significantly improve PEEK, and along with the increase of the fine content of carbon, the intensity of material and thermotolerance are all in improve, the increase of inorganic fill agent content, can Drawing abillity be improved, improve the dispersiveness of carbon fibre, thus material property is increased.
Below be only embody rule example of the present invention, protection scope of the present invention is not constituted any limitation.The technical scheme that all employing equivalents or equivalence are replaced and formed, all drops within rights protection scope of the present invention.
Claims (4)
1. a preparation method for sharp high strength polyether-ether-ketone composite material, utilizes mineral filler and through twice-modified carbon fiber, is undertaken blended by extrusion by melting and PEEK, forms the high strength PEEK matrix material that material property utilization ratio is high.
2. mineral filler is made up of glass fibre, talcum powder, calcium carbonate superfine powder according to claim 1, and each component concentration is 2:1:1 by weight.
3. according to claim 1 in twice-modified carbon fiber, carbon fiber cuts carbon fibre by the high strength of western Cree Inc. of Germany production is short, length is 6mm, a modification carries out modification by plasma method to it, then carries out twice-modified by special high temperature resistant coupling agent to it.
4. according to claim 3 by special high temperature resistant coupling agent to its carry out twice-modified in, coupling agent preparation selects titanic acid ester, biphenyl dianhydride, allyl amine and triethoxyl silane to be raw material, pass through imidization reaction, and obtain special high temperature resistant silane coupling agent with the physical mixed of titanic acid ester, carry out twice-modified by gas-liquid economic benefits and social benefits method to the carbon fiber carrying out plasma modification.
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| CN201410262746.XA CN105175991A (en) | 2014-06-13 | 2014-06-13 | Preparation method of high strength polyether ether ketone composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778407A (en) * | 2016-04-25 | 2016-07-20 | 苏州亚科塑胶有限公司 | Polyether-ether-ketone heat conduction composite material and preparation method thereof |
| CN107333401A (en) * | 2017-06-29 | 2017-11-07 | 广东美的制冷设备有限公司 | Reflow soldering tool and its production and use |
| CN109851729A (en) * | 2018-12-29 | 2019-06-07 | 福建师范大学 | Preparation method of the one kind containing ferrocene/DOPO base and crosslinking alkenyl polyether ether ketone resin |
| CN109851730A (en) * | 2018-12-29 | 2019-06-07 | 福建师范大学 | One kind containing DOPO side group Polyether-ether-ketocable cable material and preparation method thereof |
| CN111979781A (en) * | 2020-08-11 | 2020-11-24 | 金华拓达休闲用品有限公司 | Preparation method of anti-aging PU coating polyester fabric furniture cover |
| CN114479345A (en) * | 2022-01-18 | 2022-05-13 | 中国科学院兰州化学物理研究所 | Sealing material for fireproof plate hot press and preparation method thereof |
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2014
- 2014-06-13 CN CN201410262746.XA patent/CN105175991A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778407A (en) * | 2016-04-25 | 2016-07-20 | 苏州亚科塑胶有限公司 | Polyether-ether-ketone heat conduction composite material and preparation method thereof |
| CN107333401A (en) * | 2017-06-29 | 2017-11-07 | 广东美的制冷设备有限公司 | Reflow soldering tool and its production and use |
| CN107333401B (en) * | 2017-06-29 | 2019-11-26 | 广东美的制冷设备有限公司 | Reflow soldering jig and its preparation method and application |
| CN109851729A (en) * | 2018-12-29 | 2019-06-07 | 福建师范大学 | Preparation method of the one kind containing ferrocene/DOPO base and crosslinking alkenyl polyether ether ketone resin |
| CN109851730A (en) * | 2018-12-29 | 2019-06-07 | 福建师范大学 | One kind containing DOPO side group Polyether-ether-ketocable cable material and preparation method thereof |
| CN111979781A (en) * | 2020-08-11 | 2020-11-24 | 金华拓达休闲用品有限公司 | Preparation method of anti-aging PU coating polyester fabric furniture cover |
| CN111979781B (en) * | 2020-08-11 | 2022-10-11 | 金华拓达休闲用品有限公司 | Preparation method of anti-aging PU coating polyester fabric furniture cover |
| CN114479345A (en) * | 2022-01-18 | 2022-05-13 | 中国科学院兰州化学物理研究所 | Sealing material for fireproof plate hot press and preparation method thereof |
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Application publication date: 20151223 |