CN103146175A - Polyether ether ketone (PEEK) composite material modified from polyhedral oligomeric silsesquioxane (POSS) - Google Patents
Polyether ether ketone (PEEK) composite material modified from polyhedral oligomeric silsesquioxane (POSS) Download PDFInfo
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- CN103146175A CN103146175A CN2012105724246A CN201210572424A CN103146175A CN 103146175 A CN103146175 A CN 103146175A CN 2012105724246 A CN2012105724246 A CN 2012105724246A CN 201210572424 A CN201210572424 A CN 201210572424A CN 103146175 A CN103146175 A CN 103146175A
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Abstract
The invention belongs to the technical field of materials, and relates to high polymer material technology, in particular to an engineering plastic composite material, namely a polyether ether ketone (PEEK) composite material modified from polyhedral oligomeric silsesquioxane (POSS). According to the PEEK composite material modified from the POSS, high heat resistance and a nanometer characteristic of the POSS are utilized, the POSS is used as high-temperature resistant lubricant and dispersing agent, fibers are used as reinforcing materials to modify PEEK engineering plastics, screw rod extruding method is adopted for preparation, the processing process is improved, and the performance of the composite material is improved at the same time. The PEEK composite material modified from the POSS at least comprises 20-50 wt% of reinforced fibers, the mass ratio between the PEEK and the POSS is in a range of (3.5-69)/1, the melt index of the PEEK composite material modified from the POSS is obviously lowered, the PEEK composite material modified from the POSS is good in process, low in energy consumption, high in production efficiency, strong in designability of a material system, suitable for processing of fiber content composite products, and particularly suitable for processing special-shaped thin-wall products, and meanwhile the skin-friction coefficient of the products can be lowered.
Description
Technical field
The invention belongs to the material technology field, relate to high polymer material technology, particularly engineering plastic composite material.
Background technology
The PEEK special engineering plastics has special high temperature resistant, high strength, high abrasion, high-dimensional stability and good corrosion resistance nature, has general-purpose plastics and the direct labor engineering plastics performance advantage that is beyond one's reach, along with the reduction of technical progress and production cost, obtain to use more and more widely in Aeronautics and Astronautics, national defence and civilian industry at present.The PEEK melt viscosity is large, processing fluidity is bad, the melt viscosity of the PEEK matrix material that the organic or inorganic high-intensity fiber strengthens is higher, processing characteristics is more bad, need mobility well to process occasion at some like this, as injection moulding large thin-wall product, extruded product and it seems at present the Application Areass such as thermoplastic composite with good application prospect, because fiber reinforcement PEEK composite processing mobility is bad, cause goods pore, unreal, fiber non-wetting, surface irregularity occur and reveal the defectives such as fine.Adding lubricant is the method for improving the polymer processing performance of commonly using, lubricant divides external lubricant and internal lubricant, internal lubricant is by reducing the frictional force between polymer molecule, reduce the year of polymer melt, improve mobility, external lubricant by reducing the friction resistance between polymer melt and mould, improves fluidity of molten.Because traditional stearic acid, paraffin class and the decomposition temperature of mineral oils lubricant own are low, be difficult to be applied to the high temperature process condition (up to 400 ℃) of PEEK matrix material.A kind of silicone processing modified adjuvant is arranged in the market, although can reach the requirement of the high temperature process condition of PEEK matrix material, due to its chain-like structure, usually when improving mobility, can reduce the mechanical property of PEEK matrix material, this is also the inherent characteristics of common lubricant.
Polyhedral oligomeric silsesquioxane (POSS) is a kind of organic-inorganic materials, to be the inorganic nano core that is made of silicone atom consist of with peripheral organic group for it, POSS class nano material has many special character, as high temperature resistant, rub resistance, fire-retardant, high structural stability, low dielectric, high strength.In addition, the specific hybrid inorganic-organic structure of POSS makes it and organic polymer material have natural good consistency.POSS had both had the common resistant to elevated temperatures characteristics of silicone material as the polymer processing lubricant, had again the characteristics of nanometer strengthener.Patent WO2008/054418 mentions, and POSS can improve dispersiveness and the surface bonding power of mineral-type filler in polymkeric substance as surface-modifying agent; Patent WO/0172885A1 mentions, and POSS plays softening agent and toughener simultaneously as the properties-correcting agent of polymkeric substance in polymeric matrix, improves the performances such as thermotolerance, modulus, compressive strength, hardness and wear resistance of polymer materials.
Summary of the invention
The object of the present invention is to provide the good fiber reinforcement PEEK matrix material of a kind of processing characteristics.
The object of the present invention is achieved like this, utilizes high heat resistance and the nano-meter characteristic of POSS, as fire-resistant lubricants and dispersion agent, take fiber as strongthener modified PE EK engineering plastics, when improving processing technology, improves composite property with POSS.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to comprises fortifying fibre 20～50wt% at least, and the mass ratio of PEEK and POSS is between 3.5～69: between 1;
POSS is selected from ［ (RSiO
1.5)
8 ∑ 8, ［ (RSiO
1.5)
7(R
1SiO
1.5)
1 ∑ 8Or ［ (RSiO
1.5)
4(R (OH) SiO
1.0)
3 ∑ 7POSS in a kind of, wherein: R is selected from a kind of in alkyl, phenyl, siloxy; R
1Be selected from a kind of in alkyl, phenyl, aminoalkyl group, epoxy group(ing) alkyl, fluorocarbon radicals, siloxy; ∑ # represents the Siliciumatom number in the POSS molecule, and # 8 represents that the POSS molecule is complete cagelike structure, and # 7 represents that the POSS molecule is the imperfect cagelike structure of unfilled corner.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, the mass ratio of PEEK and POSS is between 4～15: between 1.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, the mass ratio of PEEK and POSS is between 6～12: between 1.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, reinforced fiber content is between 25～45wt%.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, reinforced fiber content is between 30～40wt%.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, described fortifying fibre are selected from a kind of in glass fibre, carbon fiber, aramid fiber or their mixed system.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, its course of processing is: modified additive POSS and PEEK mix in high-speed mixer; Mix with the twin screw extruder melting, the side spout is introduced fortifying fibre, extrudes tie rod and granulated and dried, the POSS modified PE EK matrix material that obtains the present invention relates to.
The working method of the polyhedral oligomeric silsesquioxane modified PE EK matrix material that the present invention relates to, in the course of processing, extruder temperature is: 330 ℃～400 ℃, 220～300 rev/mins of screw speeds.
The polyhedral oligomeric silsesquioxane modified PE EK matrix material melting index that the present invention relates to is significantly fallen, good manufacturability is low, energy consumption is low, production efficiency improves, the material system designability is strong, be applicable to high fibre content composite product processing, be specially adapted to the processing of special-shaped thin wall goods, can reduce the product surface frictional coefficient simultaneously.
Embodiment
Below in conjunction with specific embodiment, the scheme that the present invention proposes is further illustrated, but not as the restriction to technical scheme.
Embodiment 1
With VICTREX PEEK 450P and [(isobutyl--SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 69:1, adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, the side feeding is introduced 3 bundle glass fibre (988A, diameter 13 μ, 2400Tex), screw rod 10 district's Temperature Settings are: 330,340,350,370,375,380,385,385,390,380,250 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 30.1wt%, melting index is: 4.6g/10min; Tensile strength is: 190.5MPa; Tensile modulus is: 11.9GPa; Skin friction coefficient is: 0.14.
Embodiment 2
With VICTREX PEEK 450P and [(isobutyl--SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 13:1, and side feeding introducing 3 bundle glass fibre (910, diameter 13 μ, 2400Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,350,350,370,370,380,380,385,385,370,250 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 30.5wt%, melting index is: 5g/10min; Tensile strength is: 195MPa; Tensile modulus is: 12.0GPa; Skin friction coefficient is: 0.12.
Embodiment 3
With VICTREX PEEK 450P and [(iso-octyl-SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 9:1, the side feeding is introduced 3 bundle glass fibre (988A, diameter 13 μ, 2400Tex), adopt the processing of CTE-35 equidirectional parallel double-screw extruder, screw rod 6 district's Temperature Settings are: 330,350,370,380,390,380,220 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 21.1wt%, melting index is: 7g/10min; Tensile strength is: 185MPa; Tensile modulus is: 11.0GPa; Skin friction coefficient is: 0.10.
Embodiment 4
With VICTREX PEEK 450P and [(phenyl-SiO
1.5)
8 ∑ 8Mix by 15:1, and side feeding introducing 4 bundle glass fibre (910, diameter 13 μ, 2000Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,350,370,370,380,380,385,390,390,370,260 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 40.1wt%, melting index is: 5.9g/10min; Tensile strength is: 199MPa; Tensile modulus is: 14.5GPa; Skin friction coefficient is: 0.11.
Embodiment 5
With VICTREX PEEK 450P and [(isobutyl--SiO
1.5)
7(1,1,1-trifluoro propyl-SiO
1.5)
1 ∑ 8Mix by 25:1, and side feeding introducing 4 bundle glass fibre (910, diameter 13 μ, 2000Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,350,370,370,380,380,385,390,390,370,260 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 40.1wt%, melting index is: 6.9g/10min; Tensile strength is: 209MPa; Tensile modulus is: 13.5GPa; Skin friction coefficient is: 0.10.
Embodiment 6
With VICTREX PEEK 450P and ［ (isobutyl--SiO
1.5)
7(1,1,1-trifluoro propyl-SiO
1.5)
1 ∑ 8Mix by 6:1, the side feeding is introduced 2 bundle glass fibre (988A, diameter 13 μ, 2400Tex) and 2 bundle carbon fibers (T300-1000), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,340,345,360,370,385,385,385,385,370,250 rev/mins of screw speeds, obtaining fibre content is the assorted fibre enhancing PEEK matrix material of 30.9wt%, melting index is: 9.6g/10min; Tensile strength is: 210MPa; Tensile modulus is: 12.5GPa; Skin friction coefficient is:.0.05。
Embodiment 7
With VICTREX PEEK 450P and ［ (isobutyl--SiO
1.5)
7(1,1,1-trifluoro propyl-SiO
1.5)
1 ∑ 8Mix by 5:1, add to account for VICTREX PEEK 450P and ［ (isobutyl--SiO
1.5)
7(1,1,1-trifluoro propyl-SiO
1.5)
1 ∑ 8The carbonarius of total content 1wt% female (UN2014), and side feeding introducing 4 bundle glass fibre (910, diameter 13 μ, 2000Tex), adopt the processing of CTE-35 equidirectional parallel double-screw extruder, screw rod 6 district's Temperature Settings are: 330,350,370,385,390,380,250 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 40.9wt%, melting index is: 8.5g/10min; Tensile strength is: 215MPa; Tensile modulus is: 16.5GPa; Skin friction coefficient is: 0.06.
Embodiment 8
With VICTREX PEEK 450P and [(isobutyl--SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 50:1, the side feeding is introduced 8 bundle carbon fibers (T300-1000), adopts the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,350,360,380,380,390,395,400,390,380,300 rev/mins of screw speeds, obtaining carbon fiber content is the carbon fiber enhancing PEEK matrix material of 44.5wt%, melting index is: 4.3g/10min; Tensile strength is: 270MPa; Tensile modulus is: 26.4GPa; Skin friction coefficient is: 0.045.
Embodiment 9
With VICTREX PEEK 450P and [(isobutyl--SiO
1.5)
7(1,1,1-trifluoro propyl-SiO
1.5)
1 ∑ 8Mix by 35:1, the side feeding is introduced 8 bundle carbon fibers (T300-1000), adopts the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,350,360,380,380,390,395,400,390,380,300 rev/mins of screw speeds, obtaining carbon fiber content is the carbon fiber enhancing PEEK matrix material of 45.5wt%, melting index is: 5.7g/10min; Tensile strength is: 278MPa; Tensile modulus is: 25.4GPa; Skin friction coefficient is: 0.041.
Embodiment 10
With Kodel PEEK E-100 and ［ (phenyl-SiO
1.5)
4(SiO
1.0OH)
3 ∑ 7Mix by 3.5:1, the side feeding is introduced 3 bundle glass fibre (988A, diameter 13 μ, 2400Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,340,350,370,375,380,385,385,390,380,290 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 45.8wt%, melting index is: 6.4g/10min; Tensile strength is: 230MPa; Tensile modulus is: 18.5GPa; Skin friction coefficient is: 0.08.
Embodiment 11
With Kodel PEEK E-1000 and ［ (isobutyl--SiO
1.5)
4(SiO
1.0OH)
3 ∑ 7Mix by 4:1, the side feeding is introduced 4 bundle glass fibre (988A, diameter 13 μ, 2400Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are 330,350,360,370,375,380,390,390,390,380,300 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 50.8wt%, melting index is: 7.4g/10min; Tensile strength is: 225MPa; Tensile modulus is: 19.2GPa; Skin friction coefficient is: 0.09.
Embodiment 12
With Kodel PEEK E-1000 and [(isobutyl--SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 12:1, the side feeding is introduced chopped aramid fiber (Twaron1488,3mm), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,340,350,370,385,385,390,395,395,385, screw speed 26O rev/min, obtaining aramid fiber content is the aramid fiber enhancing PEEK matrix material of 35.3wt%, and melting index is: 5.1g/10min; Tensile strength is: 220MPa; Tensile modulus is: 15.5GPa; Skin friction coefficient is: 0.04.
Embodiment 13
With Kodel PEEK E-1000 and [(isobutyl--SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 40:1, the side feeding is introduced chopped aramid fiber (Twaron1488,3mm), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,345,360,375,385,385,390,395,395,385, screw speed 26O rev/min, obtaining aramid fiber content is the aramid fiber enhancing PEEK matrix material of 34.5wt%, and melting index is: 4.4g/10min; Tensile strength is: 215MPa; Tensile modulus is: 15.2GPa; Skin friction coefficient is: 0.05.
Embodiment 14
With VICTREX PEEK 450G and ［ (iso-octyl-SiO
1.5)
7(1-epoxypropoxy-SiO
1.5)
1 ∑ 8Mix by 6.5:1, the side feeding is introduced chopped aramid fiber (Twaron1488,3mm), adopt the processing of CTE-35 equidirectional parallel double-screw extruder, screw rod 6 district's Temperature Settings are: 330,350,375,380,390,380,230 rev/mins of screw speeds, obtaining aramid fiber content is the glass fibre enhancing PEEK matrix material of 24.9wt%, and melting index is: 8.36g/10min; Tensile strength is: 210MPa; Tensile modulus is: 13.8GPa; Skin friction coefficient is: 0.05.
Embodiment 15
With VICTREX PEEK 450P and [(isobutyl--SiO
1.5)
7(1-aminopropyl-SiO
1.5)
1 ∑ 8Mix by 6:1, the side feeding is introduced 3 bundle glass fibre (988A, diameter 13 μ, 2400Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,340,350,370,375,380,385,385,390,380,270 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 40.1wt%, melting index is: 7.2g/10min; Tensile strength is: 218MPa; Tensile modulus is: 16.1GPa; Skin friction coefficient is: 0.05.
Comparative Examples
With VICTREX PEEK 450P screw extrusion press extruding pelletization, the side feeding is introduced 3 bundle glass fibre (988A, diameter 13 μ, 2400Tex), adopt the processing of ZSE-27 equidirectional parallel double-screw extruder, screw rod 10 district's Temperature Settings are: 330,340,350,370,375,380,385,385,390,380,250 rev/mins of screw speeds, obtaining content of glass fiber is the glass fibre enhancing PEEK matrix material of 30.5wt%, melting index is: 3.9g/10min; Tensile strength is: 190MPa; Tensile modulus is: 11.7GPa; Skin friction coefficient is: 0.15.
Claims (6)
1. a polyhedral oligomeric silsesquioxane modified PE EK matrix material, comprise fortifying fibre 20～50wt% at least, and the mass ratio of PEEK and POSS is between 3.5～69: between 1; POSS is selected from ［ (RSiO
1.5)
8 ∑ 8, ［ (RSiO
1.5)
7(R
1SiO
1.5)
1 ∑ 8Or ［ (RSiO
1.5)
4(R (OH) SiO
1.0)
3 ∑ 7POSS in a kind of, wherein: R is selected from a kind of in alkyl, phenyl, siloxy; R
1Be selected from a kind of in alkyl, phenyl, aminoalkyl group, epoxy group(ing) alkyl, fluorocarbon radicals, siloxy.
2. polyhedral oligomeric silsesquioxane modified PE EK matrix material according to claim 1, the mass ratio of PEEK and POSS is between 4～15: between 1.
3. polyhedral oligomeric silsesquioxane modified PE EK matrix material according to claim 1, the mass ratio of PEEK and POSS is between 6～12: between 1.
4. according to claim 1,2 or 3 described arbitrary polyhedral oligomeric silsesquioxane modified PE EK matrix materials, reinforced fiber content is between 25～45wt%.
5. according to claim 1,2 or 3 described arbitrary polyhedral oligomeric silsesquioxane modified PE EK matrix materials, reinforced fiber content is between 30～40wt%.
6. according to claim 1,2 or 3 described arbitrary polyhedral oligomeric silsesquioxane modified PE EK matrix materials, described fortifying fibre are selected from a kind of in glass fibre, carbon fiber, aramid fiber or their mixed system.
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| CN105086740A (en) * | 2015-07-01 | 2015-11-25 | 宁波格莱美厨具有限公司 | Graphene polyether-ether-ketone composite coating and preparation method thereof |
| CN107022094A (en) * | 2017-04-20 | 2017-08-08 | 哈尔滨工业大学 | A kind of preparation method of the transparent flexible film of POSS enhancings aramid nano-fiber |
| CN107043518A (en) * | 2016-12-26 | 2017-08-15 | 沈阳化工大学 | Isomerism containing L POSS crosslinking agents, which is modified, reclaims PEEK and preparation method thereof |
| CN108641281A (en) * | 2018-04-11 | 2018-10-12 | 启东海大聚龙新材料科技有限公司 | A kind of poly(aryl ether ketone) wear-resistant material and preparation method thereof |
| CN109181213A (en) * | 2018-07-23 | 2019-01-11 | 宁波七诺新材料科技有限公司 | A kind of modified PE EK composite material and preparation method |
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| CN107043518A (en) * | 2016-12-26 | 2017-08-15 | 沈阳化工大学 | Isomerism containing L POSS crosslinking agents, which is modified, reclaims PEEK and preparation method thereof |
| CN107043518B (en) * | 2016-12-26 | 2018-10-26 | 沈阳化工大学 | Isomerism containing L-POSS crosslinking agents is modified recycling PEEK and preparation method thereof |
| US10968340B1 (en) | 2017-01-31 | 2021-04-06 | Eaton Intelligent Power Limited | Electrically conductive, high strength, high temperature polymer composite for additive manufacturing |
| CN107022094A (en) * | 2017-04-20 | 2017-08-08 | 哈尔滨工业大学 | A kind of preparation method of the transparent flexible film of POSS enhancings aramid nano-fiber |
| CN107022094B (en) * | 2017-04-20 | 2022-10-04 | 哈尔滨工业大学 | Preparation method of transparent flexible film of POSS (polyhedral oligomeric silsesquioxane) reinforced aramid nanofiber |
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| CN109181213B (en) * | 2018-07-23 | 2021-03-23 | 宁波七诺新材料科技有限公司 | Modified PEEK composite material and preparation method thereof |
| CN109181213A (en) * | 2018-07-23 | 2019-01-11 | 宁波七诺新材料科技有限公司 | A kind of modified PE EK composite material and preparation method |
| CN110028756B (en) * | 2019-04-01 | 2020-07-31 | 吉林大学 | Polyether-ether-ketone-based synergistic flame-retardant nano composite material and preparation method thereof |
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| CN110591329A (en) * | 2019-08-02 | 2019-12-20 | 苏州聚泰新材料有限公司 | Polyaryletherketone composition with high-uniform resistivity for static dissipative sheet material and preparation method thereof |
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| CN114351465A (en) * | 2021-12-28 | 2022-04-15 | 南通新帝克单丝科技股份有限公司 | Method for coating aramid 1414 fibers with PEEK |
| CN117462763A (en) * | 2023-12-27 | 2024-01-30 | 中国科学院空间应用工程与技术中心 | Silicon nitride fiber reinforced polyether-ether-ketone composite material, preparation method and application |
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