CN102333910A - Pekk复合纤维、其制备方法及其用途 - Google Patents
Pekk复合纤维、其制备方法及其用途 Download PDFInfo
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- CN102333910A CN102333910A CN2009801575287A CN200980157528A CN102333910A CN 102333910 A CN102333910 A CN 102333910A CN 2009801575287 A CN2009801575287 A CN 2009801575287A CN 200980157528 A CN200980157528 A CN 200980157528A CN 102333910 A CN102333910 A CN 102333910A
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- composite fibre
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- pekk
- walls nanotube
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- 229920001652 poly(etherketoneketone) Polymers 0.000 claims abstract description 34
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- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 6
- 239000002071 nanotube Substances 0.000 claims description 54
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 229920006260 polyaryletherketone Polymers 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
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- 239000004744 fabric Substances 0.000 claims description 7
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- 229910052710 silicon Inorganic materials 0.000 claims description 3
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052580 B4C Inorganic materials 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
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- PPWPWBNSKBDSPK-UHFFFAOYSA-N [B].[C] Chemical compound [B].[C] PPWPWBNSKBDSPK-UHFFFAOYSA-N 0.000 claims description 2
- FFBGYFUYJVKRNV-UHFFFAOYSA-N boranylidynephosphane Chemical compound P#B FFBGYFUYJVKRNV-UHFFFAOYSA-N 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
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- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910019093 NaOCl Inorganic materials 0.000 description 2
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- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/02—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising combinations of reinforcements, e.g. non-specified reinforcements, fibrous reinforcing inserts and fillers, e.g. particulate fillers, incorporated in matrix material, forming one or more layers and with or without non-reinforced or non-filled layers
- B29C70/021—Combinations of fibrous reinforcement and non-fibrous material
- B29C70/025—Combinations of fibrous reinforcement and non-fibrous material with particular filler
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
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- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/66—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyethers
- D01F6/665—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyethers from polyetherketones, e.g. PEEK
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
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- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
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- D10B2331/06—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyethers
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- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明涉及复合纤维,包含包括聚醚酮酮(PEKK)的热塑性聚合物基体,其中分散有多壁纳米管、特别是碳多壁纳米管。本发明还涉及所述复合纤维的制备方法及其用途。
Description
本发明涉及复合纤维,尤其是导电纤维,由其中分散有多壁纳米管特别是碳纳米管的包括聚醚酮酮(PEKK)的热塑性聚合物基体组成。本发明还涉及所述复合纤维的制备方法和其用途。
能够允许电流流过并通过焦耳效应产生热的导电纤维用于制备加热的织物例如衣服、覆盖物、汽车座椅或保护衬里(用于例如保护燃料箱不受寒冷)。
导电纤维还用于不需要热效应的应用,例如由于其抗静电性能特别地用于制备航空或汽车部件或者用于电子设备的电磁屏蔽,例如以消除摩擦产生的电荷,特别是在流体流过热塑性管时感生的那些。
现有技术已知的的导电纤维包括:
-金属线,其缺点是重且易于氧化;
-本征导电聚合物的纤维,其不是非常耐洗的且在它们对于氧化以及由焦耳效应释放的热敏感的情况下不是非常稳定的,在超过一定温度后所述热可使聚合物化学退化(例如交联)和/或损害其机械性能;
-聚合物纤维,通过在其表面上沉积导电颗粒使其导电,例如镀银纤维,其中涂层易于通过摩擦和磨损而退化;和
-填充有基于碳或金属的导电颗粒的聚合物纤维。
在导电纤维的后者类别中,可提及由碳纳米管增强的聚合物基体,例如申请人的专利US-6331265中描述的那些。该专利由此公开了各种聚合物基体,特别是基于聚醚醚酮(或PEEK)的那些,但优选基于聚烯烃,其根据用于优化纤维的机械性能的方法通过碳纳米管增强,没有特别追求导电性能。
现在,申请人想到基于另一类型的聚醚酮即聚醚酮酮(或PEKK)和多壁纳米管特别是碳纳米管的一些复合材料不仅具有良好的机械性能(特别是杨氏模量和断裂强度),而且具有很好的导电性能以及非常好的热稳定性,使得它们能够通过高的电流密度而没有由焦耳效应释放的热化学地损害它们使得实质上损害它们的外观和/或它们的机械性能。这些复合材料还具有良好的熔体纺丝能力。所述性能的该组合使得它们非常适于制备导电纤维,以制造加热的织物或其它导电材料,例如上面描述的那些,特别是经受高的热和/或机械应力的抗静电材料。这些复合材料还显示出生物相容性,使得可设想将它们用于生物医学应用,特别是用于缝线的制备。
诚然,由专利申请WO 2005/081781已知制备基于聚合物如PEEK或PEKK和碳纳米管的复合材料。这些复合材料用于制备用于封装电子部件或用于制备电化学电池的双极板的模塑制品。然而,上述申请没有想到由它们制备纤维。
同样地,Oxford Performance Materials Inc.公司以商标销售各种级别的热稳定PEKK,其中一些(-IG知-MG级230C和240C)是通过玻璃纤维或碳纤维增强的。然而,这些复合材料在发明的范围中不能转变成纤维。这是因为,由于碳纤维的直径(约5-10μm),它们难以均匀地分散在复合纤维中且可因此产生易于堵塞用于形成复合纤维的喷丝头的过滤料或孔的缺陷。
因此,本发明的一个主题是复合纤维,特别是导电纤维,其由包括聚醚酮酮(PEKK)的热塑性聚合物基体组成,其中分散有多壁纳米管,特别是基于碳的纳米管。
在本发明的范围中,术语“复合纤维”理解为是指由直径为100nm-300μm、优选1-100μm和还更好地2-50μm的绳股(线,strand)构成的纤维。
在本说明书的范围中,术语“PEKK”理解为是指包含如下且优选由如下组成的聚合物:满足如下通式(A)的单体:
其中Ph表示1,4-亚苯基(在该情况下-CO-Ph-CO-单元表示对苯二甲酰(T)基),和/或其中Ph表示1,3-亚苯基(在该情况下-CO-Ph-CO-单元表示间苯二甲酰(I)基)的式的单体(I)。所述苯基可任选被C1-C8烷基取代。
根据本发明的一个优选实施方案,所述聚合物包含上述单体的组合,且有利地由该组合组成。在该情况下,(T)/(I)的摩尔比可为80/20-20/80,优选60/40-50/50,包括端值。
根据本发明可使用的PEKK可为结晶的、半结晶的或者非晶的。然而,优选使用非晶的PEKK,使得可获得聚合物链沿由PEKK形成的复合纤维的轴的更有利取向,且由此获得这些复合纤维的更好的机械性能。还优选PEKK具有150-170℃(包括端值)的玻璃化转变温度(Tg)。当存在熔点时,其熔点可为例如280-400℃,优选300-370℃,包括端值。
本发明的另一主题是复合纤维,其包括主要包含聚芳基醚酮(PAEK)特别是非晶PAEK的聚合物基体,其中分散有至少一种元素周期表的IIIa、IVa或Va族化学元素的多壁纳米管。
除了PEKK或PAEK之外,根据本发明使用的聚合物基体还可包含至少一种添加剂,所述添加剂特别地选自增塑剂、抗氧化剂、光稳定剂、颜料或染料、抗冲改性剂、抗静电剂、阻燃剂、润滑剂及其混合物,条件是这些添加剂不损害导电纤维的制备。作为变型或另外,所述聚合物基体可包含至少一种其它热塑性聚合物,其与PEKK相容或者被使得与PEKK相容。
根据本发明的复合纤维的第二要素是多壁纳米管的分散,这些有利地由至少一种选自周期表的IIIa、IVa或Va族元素的化学元素组成。所述纳米管因此可基于硼、碳、氮、磷、硅或钨。它们可例如包含以下物质,或由以下物质组成:碳、氮化碳、氮化硼、碳化硼、磷化硼、氮化磷或硼氮化碳、或者硅或钨。
使用多壁纳米管的优点在于以下事实:当它们经受表面处理特别地以使它们的加工更容易或使它们与基体相容时,它们保持它们的导电性能,不像单壁纳米管随它们表面的改变而改变。
根据本发明的一个优选实施方案,使用多壁碳纳米管(或CNT)。这些是中空的石墨碳纤丝,其各自包括若干沿纤丝轴取向的石墨管壁。具有多重壁的多壁纳米管可使用CVD(化学气相沉积)法制备。多壁纳米管可例如包含3-15片和更优选3-10片。
本发明可应用的多壁纳米管的平均直径为3-100nm,更优选4-50nm,和还更好地为4-30nm,且有利地长度为0.1-10μm。它们的长度/直径比优选大于10,且通常大于100或甚至大于1000。因此,多壁纳米管不同于碳纤维,所述纤维通常更长且直径更大,因此与多壁纳米管相比较不适于常规的热塑性挤出技术。
在多壁纳米管的情况下,它们的比表面积为例如100-500m2/g(包括端值),通常100-300m2/g。它们的堆密度可特别地为0.05-0.5g/cm3(包括端值)和更优选0.1-0.2g/cm3(包括端值)。
粗(未加工,raw)多壁的多壁碳纳米管的一个实例特别地可由ArkemaFrance公司以商标C100获得。
在这些多壁纳米管在根据本发明的方法中处理之前,可对它们进行纯化和/或处理(例如氧化)和/或研磨和/或官能化。
多壁纳米管的研磨可特别地使用已知的加工技术在设备例如球磨机、锤磨机、磨碎机、切碎机、气体射流冲击研磨机或任何其它能够减小多壁纳米管的缠绕网络的尺寸的研磨系统中冷或热地进行。优选该研磨步骤使用气体射流冲击研磨技术进行,特别地在空气射流冲击研磨机中。
所述粗或研磨的多壁纳米管可通过用硫酸溶液洗涤来纯化,以从它们除去任何残留的来自它们的制备工艺的矿物和金属杂质。多壁纳米管/硫酸的重量比可特别地为1/2-1/3(包括端值)。纯化操作还可在90-120℃的温度下进行例如5-10小时的时间。该操作可有利地后面有用水漂洗纯化的多壁纳米管和将它们干燥的步骤。
多壁纳米管的氧化有利地通过使它们与次氯酸钠溶液接触进行,所述溶液包含0.5-15重量%的NaOCl和优选1-10重量%的NaOCl,例如在1/0.1-1/1的多壁纳米管/次氯酸钠的重量比下。有利地,所述氧化在低于60℃的温度下且优选在室温下进行几分钟-24小时的时间。该氧化操作可有利地后面有过滤和/或离心分离、洗涤和干燥所述氧化的多壁纳米管的步骤。
多壁纳米管的官能化可通过将反应性实体如乙烯基单体接枝到多壁纳米管的表面上进行。在已经历用于消除在其表面上的含氧基团的在无水和无氧的介质中在高于900℃下的热处理之后,所述多壁纳米管的组成材料用作自由基聚合引发剂。
为了消除金属催化剂残留物,还可使多壁纳米管经历在至少1000℃、例如1200℃的温度下的热处理。
在本发明中,特别地使用任选研磨的粗多壁纳米管,即没有有意地氧化、纯化、官能化且没有经历其它化学处理的多壁纳米管。
多壁纳米管是否经历处理(化学或退火处理)取决于纤维增强热塑性塑料的最终用途。
相对于根据本发明的复合纤维的重量,多壁纳米管可占0.1-15重量%且优选1-10重量%。
本发明的主题还为上述基于PEKK的复合纤维的制备方法,包括在于如下的相继步骤:
(a)将多壁纳米管(任选地以在聚合物基体的一部分中的母料形式)分散到聚合物基体的全部或其它部分中以获得复合共混物;和
(b)将所述复合共混物转变为纤维。
在于将多壁纳米管共混到PEKK中的步骤(a)可在任何装置中进行。优选,多壁纳米管和热塑性聚合物通过使用标准装置如双螺杆挤出机或共捏合机配混来进行共混。它们可同时或在沿挤出机的不同点处引入。在该方法中,聚合物颗粒或粉末典型地与多壁纳米管熔融共混。
作为变型,所述多壁纳米管可通过任何合适的方式分散在溶于溶剂的热塑性聚合物中。在这种情况下,根据本发明的一个有利实施方案,可通过使用分散系统(例如超声或转子/定子系统)或者借助特定的分散剂改善该分散。
所述分散剂可特别地选自增塑剂,特别地环化的聚对苯二甲酸丁二醇酯和混合物如Cyclics Corporation销售的树脂100。作为变型,所述分散剂可为包含至少一种阴离子亲水单体和至少一种包含至少一个芳环的单体的共聚物,例如文献FR-2766106中所描述的共聚物,分散剂/多壁纳米管的重量比优选为0.6/1-1.9/1。在又一实施方案中,分散剂可为乙烯基吡咯烷酮均聚物或共聚物,在该情况下多壁纳米管/分散剂的重量比优选为0.1-小于2。通常,分散剂也可选自具有两亲特性的合成或天然的分子或大分子,例如表面活性剂,对分散介质和多壁纳米管两者具有亲和力。
在本发明的优选实施方案中,在步骤(a)中使用的多壁纳米管是与聚合物基体的一部分的母料的形式,并在步骤(a)中用剩余的聚合物基体和增塑剂例如Cyclics Corporation销售的树脂100稀释,其浓度取决于多壁纳米管的含量。在该实施方案中,相对于母料的重量,多壁纳米管可占3-30重量%,优选5-20重量%。在该优选实施方案中,基体的选择优选为粉末形式的非晶PEKK,且有利地使用L/D比为11-15的BUSS共捏合机进行共混。
在本发明的第二优选实施方案中,由非晶PEKK、多壁纳米管和增塑剂组成的母料用于基于任选地包含纤维(碳或玻璃纤维)或甚至其它矿物填料的PEKK、PEEK或任何其它结晶PAEK的配料。
由步骤(a)得到的复合共混物然后在步骤(b)中转变成纤维。这些纤维可有利地使用熔体纺丝方法、优选地通过使它们通过具有小直径模头的挤出机而形成。在惰性气氛中进行该步骤以保持多壁纳米管的结构可为有利的。根据另一实施方案,所述纤维可使用基于溶剂的方法获得。
根据本发明的方法还可包括另外的步骤(c),在于将得到的纤维在高于PEKK的玻璃化转变温度(Tg)且优选低于其熔点(如果存在)的温度下拉伸。这样的步骤描述在专利US-6331265中,该文献在此引入作为参考,该步骤使得可对多壁纳米管和聚合物基体基本上在相同的方向上沿纤维轴进行取向且因此改善纤维的机械性能,特别是其拉伸模量(杨氏模量)和其韧度(断裂强度)。定义为拉伸后的纤维长度与拉伸前的纤维长度之比的拉伸比可为1-20,优选1-10,包括端值。拉伸可进行仅一次,或进行若干次,在各拉伸操作之间使纤维稍微松弛。该拉伸步骤优选通过使纤维通过一系列以不同速度旋转的辊进行,放出纤维的那些辊以比卷起纤维的那些辊低的速度旋转。为了实现所需的拉伸温度,可使纤维通过置于辊之间的烘箱,或使用加热的辊,或将这两种技术组合。通过使用非晶PEKK使拉伸步骤容易。
该拉伸步骤使得可强化纤维和获得高的断裂强度。
此外,尽管根据该方法得到的复合纤维是本征导电的,即它们在室温下具有可低于105ohm.cm的电阻率,但是它们的电导率可通过热处理进一步改善。
最后,这些复合纤维能够经受高电流密度而基本上不损害它们的机械性能或它们的外观,一方面因为PEKK的良好的热稳定性且另一方面因为多壁纳米管散热的能力。
本发明的主题还为复合纤维的制备方法,包括下列步骤:
(a)将至少一种来自元素周期表的IIIa、IVa或Va族的化学元素的多壁纳米管分散到主要包含聚芳基醚酮(PAEK)的热塑性基体中;
(b)将得到的共混物转化以形成纤维;和
(c)任选地拉伸得到的纤维。
由于以上所述的有利性能,根据本发明的复合纤维可用于制备:火箭或航空器的头锥体、机翼或机身;海上柔性管道增强材料;汽车车身或发动机底盘部件;抗静电包装和纺织品,特别是用于筒仓的保护;电磁屏蔽器件,特别是用于电子部件的保护;加热的织物;导电电缆;传感器,特别是机械应变或应力传感器;或生物医学器件,例如缝线或导管。
本发明的另一主题特别地为结构复合部件,其包含如上所述的复合纤维(基于PEKK或PAEK)。
这些复合部件的制备可使用各种方法进行,通常包括用聚合物基体浸渍纤维的步骤。该浸渍步骤本身可使用各种技术进行,特别地取决于使用的基体的物理形式(粉末或相对液体的形式)。纤维可优选使用流化床浸渍方法浸渍,其中聚合物基体为粉末态。纤维本身可原样或在将它们编织成由纤维的双向网络构成的织物的步骤之后浸渍。
根据本发明的纤维可引入到热塑性塑料、弹性体或热固性塑料中。
这些半成品然后用于制备所需的复合部件。相同或不同组成的各种预浸料织物可堆叠以形成片或层叠物,或者作为变型,经受热成型工艺。在所有的情形中,最终部件的制备包括强化聚合物基体的步骤,其例如局部加热以产生其中纤维相互扣紧的区域。
作为变型,可由浸渍基体制备膜,特别地通过挤出或压延方法,所述膜具有例如约100μm的厚度,然后该膜置于两个纤维垫之间,然后热压该组件以浸渍所述纤维并制造复合物。
在这些方法中,浸渍基体可包括热塑性、弹性体性或热固性聚合物、或者这些的共混物。所述聚合物基体本身可包含一种或多种填料或纤维。
而且,根据本发明的复合纤维可单独或与其它纤维一起编织或编结,或者可单独或与其它纤维组合用于制备毡或无纺材料。组成这些其它纤维的材料的实例包括,非穷举:
-拉伸聚合物纤维,特别地基于以下:聚酰胺,例如尼龙-6(PA-6)、尼龙-11(PA-11)、尼龙-12(PA-12)、尼龙-6,6(PA-6,6)、尼龙-4,6(PA-4,6)、尼龙-6,10(PA-6,10)或尼龙-6,12(PA-6,12);聚酰胺/聚醚嵌段共聚物高密度聚乙烯;聚丙烯;或聚酯如聚羟基链烷酸酯和由Du Pont以商标销售的聚酯;
-碳纤维;
-玻璃纤维,特别是E-玻璃、R-玻璃或S2玻璃纤维;
-硼纤维;
-硅石纤维;
-天然纤维,例如亚麻、大麻、剑麻、棉或羊毛纤维;和
-其混合物,例如玻璃纤维、碳和芳族聚酰胺纤维的混合物。
实施例1:
实施例2:
将在实施例1中获得的颗粒引入加热至390℃且配有具有0.5mm孔的模头的单螺杆挤出机(L/D=16)中。在拉伸设备上以最终直径稳定在100μm的方式拉伸得到的纤维,这些在空气中冷却,然后使用合适的装置在卷轴上卷起。
Claims (12)
1.复合纤维,特别是导电纤维,由其中分散有多壁纳米管的包括聚醚酮酮(PEKK)的热塑性聚合物基体组成。
2.根据权利要求1的复合纤维,特征在于所述多壁纳米管包含以下、特别地由以下组成:碳、氮化碳、氮化硼、碳化硼、磷化硼、氮化磷、硼氮化碳、硅或钨。
3.根据权利要求2的复合纤维,特征在于所述多壁纳米管是多壁碳纳米管。
4.根据权利要求1-3中任一项的复合纤维,特征在于相对于所述纤维的重量,所述多壁纳米管占0.1-50重量%,且优选1-10重量%。
5.根据权利要求1-4中任一项的复合纤维,特征在于所述PEKK是非晶的。
6.根据权利要求1-5中任一项的复合纤维,特征在于所述PEKK具有150-170℃(包括端值)的玻璃化转变温度(Tg)。
7.根据权利要求1-6中任一项的复合纤维的在制备如下中的用途:火箭或航空器的头锥体、机翼或机身;海上柔性管道增强材料;汽车车身或发动机底盘部件;抗静电包装和纺织品;电磁屏蔽器件,特别是用于电子部件的保护;加热的织物;导电电缆;传感器,特别是机械应变或应力传感器;或生物医学器件,例如缝线或导管。
8.根据权利要求1-6中任一项的复合纤维的制备方法,包括在于如下的相继步骤:
(a)将任选地在聚合物基体的一部分中的母料形式的多壁纳米管分散到聚合物基体的全部或其它部分中以获得复合共混物;和
(b)将所述复合共混物转变成纤维,优选使用熔体纺丝方法。
9.根据权利要求8的方法,特征在于其包括另外的步骤(c),在于将得到的纤维在高于PEKK的玻璃化转变温度且优选低于其熔点的温度下拉伸。
10.复合纤维,其包括主要包含聚芳基醚酮(PAEK)、特别是非晶PAEK的聚合物基体,其中分散有至少一种元素周期表的IIIa、IVa或Va族的化学元素的多壁纳米管。
11.复合纤维的制备方法,包括下列步骤:
(a)将至少一种元素周期表的IIIa、IVa或Va族的化学元素的多壁纳米管分散到主要包含聚芳基醚酮(PAEK)的热塑性基体中;
(b)将得到的共混物转变以形成纤维;和
(c)任选地拉伸得到的纤维。
12.结构复合物部件,其包含根据权利要求1-10中任一项的复合纤维。
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FR0859090A FR2940659B1 (fr) | 2008-12-26 | 2008-12-26 | Fibre composite a base de pekk, son procede de fabrication et ses utilisations |
FR0859090 | 2008-12-26 | ||
PCT/FR2009/052665 WO2010072975A1 (fr) | 2008-12-26 | 2009-12-22 | Fibre composite a base de pekk, son procede de fabrication et ses utilisations |
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CN102333910A true CN102333910A (zh) | 2012-01-25 |
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US (1) | US20110311811A1 (zh) |
EP (1) | EP2370619B1 (zh) |
JP (1) | JP5485293B2 (zh) |
KR (1) | KR20110089441A (zh) |
CN (1) | CN102333910A (zh) |
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KR102093565B1 (ko) * | 2018-11-01 | 2020-03-25 | 김경웅 | 제전성을 극대화 한 수지조성물 |
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JP5485293B2 (ja) | 2014-05-07 |
KR20110089441A (ko) | 2011-08-08 |
US20110311811A1 (en) | 2011-12-22 |
FR2940659B1 (fr) | 2011-03-25 |
FR2940659A1 (fr) | 2010-07-02 |
EP2370619A1 (fr) | 2011-10-05 |
WO2010072975A1 (fr) | 2010-07-01 |
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