CN102660103B - Antistatic polyether-ether-ketone composite material and preparation method thereof - Google Patents

Antistatic polyether-ether-ketone composite material and preparation method thereof Download PDF

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CN102660103B
CN102660103B CN201210064019.3A CN201210064019A CN102660103B CN 102660103 B CN102660103 B CN 102660103B CN 201210064019 A CN201210064019 A CN 201210064019A CN 102660103 B CN102660103 B CN 102660103B
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ether
polyether
coupling agent
ketone
composite material
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CN102660103A (en
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吴立豪
万长宇
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Dalian Luyang Science & Technology Development Co Ltd
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Dalian Luyang Science & Technology Development Co Ltd
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Abstract

The invention relates to an antistatic polyether-ether-ketone composite material and a preparation method thereof, and belongs to the fields of high polymer materials and the preparation thereof. The composite material of the invention is prepared by selecting polyether-ether-ketone, PAN carbon fiber, acetylene carbon black, and a coupling agent as raw materials, and the composite material is molded by adopting the method of compression molding. According to the invention, the preparation method is simple, the parameters are easy to control, the consistency is good, the stability is high, and no special device is needed. The composite material can be applied to vacuum suction cups and wafer trays used in semiconductor manufacturing industry, electronic components used in hostile environments such as high temperature and high pressure in oil field industry, and sealing-connecting electronic components used in electronic and electrical industries, and the like.

Description

A kind of antistatic Peek Composite Material and Preparation Method
Technical field
The invention belongs to macromolecular material and preparation field thereof, particularly a kind of matrix material taking polyether-ether-ketone as main raw material and preparation method thereof.
Background technology
Polyether-ether-ketone has multiple good characteristic as high thermal resistance, wear resistance, chemical resistance, hydrolytic resistance, insulativity, excellent intensity and toughness, stability, fire prevention and the performance such as nontoxic.
Semi-conductor industry requires very high to the antistatic property of material, in the packaging of electronic product and transportation, easily produce static, can be caused very large harm to electronic product if static does not lead away.Current anlistatig method adopts the method for spraying static inhibitor on some workpiece to realize more.This method is short work-ing life, generally quantity-produced enterprise monthly all will spray more than 2 times, make whole workshop all with a kind of niff, workman cannot be worked, or work under rugged environment, now also there is the use of a lot of common anti-electrostatic sheet materials such as PP, ABS, PE, PC, but common antistatic material cannot meet under 200 DEG C of environment of electronic manufacturing industry high temperature and uses, the equipment of especially present electronic manufacturing industry and frock, not only require anti-electrostatic, and require high temperature resistant.Common like this antistatic material just has no idea to meet, and needs a kind of novel material, has high temperature resistantly, and purity is high, wear resistance, the features such as chemical stability.
Summary of the invention
Object of the present invention is for existing antistatic material deficiency, provide a kind of taking polyether-ether-ketone as base-material, add carbon conductive filler and realize anlistatig matrix material and preparation method thereof, there is the carbon series conductive of interpolation material few, resistivity is easily controlled, and stability is high, meet the advantages such as ROHS environment friendly non-halogen.
Technical scheme of the present invention is as follows:
The each composition of antistatic polyether-ether-ketone composite material and weight proportion thereof are: polyether-ether-ketone 80-95 part, PAN carbon fibre 8-15 part, Shawinigan black 4-10 part, silane coupling agent 0.5-2.5 part, titanate coupling agent 0.5-1 part.PAN carbon fibre need be treated to modification PAN carbon fibre through silane coupling agent, and Shawinigan black need be treated to modification Shawinigan black through titanate coupling agent.
Preparation method's following (the each composition of raw material is in weight proportion) of antistatic polyether-ether-ketone composite material:
(1) polyether-ether-ketone 80-95 part is dried before use, at 130-150 DEG C, dry and put 2-4 hour;
(2) PAN carbon fibre 8-15 part is placed in to high mixer, then in dehydrated alcohol, add silane coupling agent 0.5-2.5 part, make coupling agent solution, inject carbon black with syringe again, premix 10-15 minute at 60 DEG C, then by solution filter extracting, finally modification PAN carbon fibre is dried at 120 DEG C except residual solvent;
(3) Shawinigan black 4-10 part is placed in to high mixer, then in dehydrated alcohol, adds titanate coupling agent 0.5-1 part, be sprayed on equably on Shawinigan black with syringe, high-speed stirring 4-8 minute, dry 4-8 hour at 100-110 DEG C;
(4) by polyether-ether-ketone after treatment in step (1), (2), (3), carbon fibre, Shawinigan black, is placed in high-speed mixer and mixing even, and mixing time 30 minutes, is mixing raw material;
(5) mixing raw material is put into mould coldmoulding, pressure is 5Mpa, pressurize 1-3 minute;
(6) mould is put into baking box and heat, Heating temperature 380-400 DEG C, heating 2-3 hour;
(7) fast fetching goes out mould and is placed on press, after cooling 5-10 minute, is pressurized to 5-10Mpa, pressurize 15-30 minute, the demoulding.
Silane coupling agent model be commercially available kind as KH-590, KH-602, KH-570 or KH-792 etc., titanate coupling agent model be commercially available kind as NDZ-102, NDZ-201 or JTW-102 etc.
Antistatic polyether-ether-ketone composite material provided by the invention is widely used, can be used for high requirement Reflow Soldering, Wave soldering fixture in electron and electrician industry, high temperature resistant end turn set collar, the protection of thermometric hot resistance and other bonding under hot operation condition are antistatic; In wiring board manufacturing, can be used for Electronic Protection and paste, be specially adapted to the electronic devices and components of the high temperature resistant and moisture protection of the various need such as the protection of SMT heatproof, electronic switch, the protection of pcb board golden finger, electronic transformer, rly.; Also applicable to Metal Materials At High Temperature spray paint, sandblast application covers surface protection etc.The present invention has high temperature resistant, and tensile strength is high, and chemical resistant properties is good, meets the advantages such as ROHS environment friendly non-halogen.
Specific embodiment
embodiment 1
(1) take 81 parts of polyether-ether-ketones, 12 parts of PAN carbon fibres, 4 parts of Shawinigan blacks, 2.5 parts of silane coupling agent KH590,1.5 parts of titanate coupling agent NDZ-102;
(2) polyether-ether-ketone is placed in to 150 DEG C of baking ovens dry 3 hours;
(3) PAN carbon fibre is placed in to high mixer, then in dehydrated alcohol, add silane coupling agent KH590, make coupling agent solution, inject carbon black with syringe again, premix 15 minutes at 60 DEG C, then by solution filter extracting, finally modifying carbon fiber is dried at 120 DEG C except residual solvent;
(4) Shawinigan black is placed in to high mixer, then in dehydrated alcohol, adds titanate coupling agent NDZ-102, be sprayed on equably on Shawinigan black with syringe, high-speed stirring 5 minutes, at 105 DEG C dry 6 hours;
(5) by polyether-ether-ketone after treatment, modifying carbon fiber, modification Shawinigan black, is placed in high-speed mixer and mixing even, and mixing time 30 minutes, is mixing raw material;
(6) mixing raw material is put into mould coldmoulding, pressure is 5Mpa, pressurize 1 minute;
(7) mould is put into baking box and heat, 380 DEG C of Heating temperatures, heat 2 hours;
(8) fast fetching goes out mould and is placed on press, after cooling 5 minutes, is pressurized to 5Mpa, pressurize 15 minutes, the demoulding.
embodiment 2
(1) take 88 parts of polyether-ether-ketones, 8 parts of PAN carbon fibres, 10 parts of Shawinigan blacks, 0.5 part of silane coupling agent KH602,0.5 part of titanate coupling agent NDZ-201;
(2) polyether-ether-ketone is placed in to 130 DEG C of baking ovens dry 4 hours;
(3) PAN carbon fibre is placed in to high mixer, then in dehydrated alcohol, add silane coupling agent KH602, make coupling agent solution, inject carbon black with syringe again, premix 10 minutes at 60 DEG C, then by solution filter extracting, finally modifying carbon fiber is dried at 120 DEG C except residual solvent;
(4) Shawinigan black is placed in to high mixer, then in dehydrated alcohol, adds titanate coupling agent NDZ-201, be sprayed on equably on Shawinigan black with syringe, high-speed stirring 4 minutes, at 110 DEG C dry 4 hours;
(5) by polyether-ether-ketone after treatment, modifying carbon fiber, modification Shawinigan black, is placed in high-speed mixer and mixing even, and mixing time 30 minutes, is mixing raw material;
(6) mixing raw material is put into mould coldmoulding, pressure is 5Mpa, pressurize 3 minutes;
(7) mould is put into baking box and heat, 390 DEG C of Heating temperatures, heat 2 hours;
(8) fast fetching goes out mould and is placed on press, after cooling 8 minutes, is pressurized to 8Mpa, pressurize 25 minutes, the demoulding.
embodiment 3
(1) take 95 parts of polyether-ether-ketones, 10 parts of PAN carbon fibres, 6 parts of Shawinigan blacks, 1.5 parts of silane coupling agent KH792,1 part of titanate coupling agent JTW-102;
(2) polyether-ether-ketone is placed in to 140 DEG C of baking ovens dry 2 hours;
(3) PAN carbon fibre is placed in to high mixer, then in dehydrated alcohol, add silane coupling agent KH792, make coupling agent solution, inject carbon black with syringe again, premix 13 minutes at 60 DEG C, then by solution filter extracting, finally modifying carbon fiber is dried at 120 DEG C except residual solvent;
(4) Shawinigan black is placed in to high mixer, then in dehydrated alcohol, adds titanate coupling agent JTW-102, be sprayed on equably on Shawinigan black with syringe, high-speed stirring 8 minutes, at 100 DEG C dry 8 hours;
(5) by polyether-ether-ketone after treatment, modifying carbon fiber, modification Shawinigan black, is placed in high-speed mixer and mixing even, and mixing time 30 minutes, is mixing raw material;
(6) mixing raw material is put into mould coldmoulding, pressure is 5Mpa, pressurize 2 minutes;
(7) mould is put into baking box and heat, 400 DEG C of Heating temperatures, heat 2 hours;
(8) fast fetching goes out mould and is placed on press, after cooling 5 minutes, is pressurized to 10Mpa, pressurize 30 minutes, the demoulding.
embodiment 4
Performance test as an example of silane coupling agent KH590 and titanate coupling agent NDZ-102 example:
Surface resistivity test is tested by standard GB/T/T 1401-2006.Sample is diameter 83mm, the circular specimen that thickness is 5mm:
Composition (%) Sample 1 Sample 2 Sample 3
PEEK 81 88 95
Carbon fibre 8 15 10
Shawinigan black 10 5 6
Silane coupling agent KH590 1 2 1.5
Titanate coupling agent NDZ-102 0.5 0.9 1.1
Surface resistivity:
As can be seen from the above table, the antistatic polyether-ether-ketone composite material surface resistivity that prepared by employing the present invention is 10 6~ 10 10between, realize anlistatig needs, and easily regulated, the antistatic polyether-ether-ketone composite material that has added carbon fibre and Shawinigan black, not only has antistatic property, and has improved intensity and the wear resisting property of material, moulding process is simple, and equipment and technical requirements are low.

Claims (1)

1. a preparation method for antistatic polyether-ether-ketone composite material, is characterized in that: the each composition of raw material is in weight proportion,
(1) polyether-ether-ketone 80-95 part is dried before use, at 130-150 DEG C, dry and put 2-4 hour;
(2) PAN carbon fibre 8-15 part is placed in to high mixer, then in dehydrated alcohol, add silane coupling agent 0.5-2 part, make coupling agent solution, inject PAN carbon fibre with syringe again, premix 10 minutes at 60 DEG C, then by solution filter extracting, finally modification PAN carbon fibre is dried at 120 DEG C except residual solvent;
(3) Shawinigan black 4-10 part is placed in to high mixer, then in dehydrated alcohol, adds titanate coupling agent 0.5-1 part, be sprayed on equably on Shawinigan black with syringe, high-speed stirring 4-8 minute, dry 4-8 hour at 100-110 DEG C;
(4) by polyether-ether-ketone after treatment in step (1), (2), (3), carbon fibre, Shawinigan black, is placed in high-speed mixer and mixing even, and mixing time 30 minutes, is mixing raw material;
(5) mixing raw material is put into mould coldmoulding, pressure is 5MPa, pressurize 1-3 minute;
(6) mould is put into baking box and heat, Heating temperature 380-400 DEG C, heating 2-3 hour;
(7) fast fetching goes out mould and is placed on press, and cooling 5-10 minute, is pressurized to 5-10MPa, pressurize 15-30 minute, the demoulding.
CN201210064019.3A 2012-03-13 2012-03-13 Antistatic polyether-ether-ketone composite material and preparation method thereof Active CN102660103B (en)

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CN103146175B (en) * 2012-12-26 2015-02-04 余姚中国塑料城塑料研究院有限公司 Polyether ether ketone (PEEK) composite material modified from polyhedral oligomeric silsesquioxane (POSS)
CN103275458B (en) * 2013-06-20 2016-07-06 衡阳恒飞电缆有限责任公司 A kind of Polyether-ether-ketocable cable material and preparation method thereof
CN103554950B (en) * 2013-10-25 2017-01-11 东北林业大学 Flame-retardant antistatic wood powder/polypropylene wood-plastic composite material with silane modified conductive carbon black, and preparation method of composite material
CN103740088A (en) * 2013-12-24 2014-04-23 苏州华东橡胶工业有限公司 Formula for modifying polyether-ether-ketone plastics
CN104277414B (en) * 2014-11-02 2016-05-04 吉林大学 Polyetheretherketonepolymer polymer carbon fibre composite that contains phenylacetylene side group and preparation method thereof
CN107915955A (en) * 2017-11-08 2018-04-17 大连路阳科技开发有限公司 Antistatic polyether-ether-ketone composite material and preparation method

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CN101875774A (en) * 2009-12-21 2010-11-03 扬州大学 Polyarylether/nano expanded graphite/carbon fiber high-strength conducting composite material and preparation method thereof
CN102321338A (en) * 2011-07-15 2012-01-18 吉林大学 Polyetheretherketone-base composite electromagnetic shielding material and preparation method thereof

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US6372829B1 (en) * 1999-10-06 2002-04-16 3M Innovative Properties Company Antistatic composition

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101875774A (en) * 2009-12-21 2010-11-03 扬州大学 Polyarylether/nano expanded graphite/carbon fiber high-strength conducting composite material and preparation method thereof
CN102321338A (en) * 2011-07-15 2012-01-18 吉林大学 Polyetheretherketone-base composite electromagnetic shielding material and preparation method thereof

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