CN102250446B - High-dimension-stability and friction-resistant polyether-ether-ketone composite material and preparation method thereof - Google Patents
High-dimension-stability and friction-resistant polyether-ether-ketone composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of high-performance polymer, and relates to a high-dimension-stability and friction-resistant polyether-ether-ketone composite material and a preparation method thereof. The composite material comprises the following components in terms 100 percent by weight: 60-90 percent of polyether-ether-ketone resin, 0.05-0.12 percent of high-temperature-resistant coupling agent, 5-20 percent of wollastonite and 0-30 percent of glass fiber. The preparation method comprises the following steps of: dissolving the high-temperature-resistant coupling agent into an organic solvent under the protection of N2; adding the wollastonite; stirring; heating to a reflow temperature; adding water and continuously heating to reflow for 1-4 hours; performing extraction filtration to obtain modified wollastonite; washing the modified wollastonite, drying and mixing with polyether-ether-ketone powder; extruding through a double-screw extruder; and granulating to obtain the polyether-ether-ketone composite material. The composite material prepared by the invention has extremely low linear expansion coefficient and forming shrinkage rate, also has self-lubrication property and high mechanical performance and is applied to preparation of bearings, gears, valve plates and the like.
Description
Technical field
The invention belongs to the high-performance polymer field, be specifically related to the wear-resisting wiping Peek Composite Material and Preparation Method of a kind of high-dimensional stability.
Background technology
PEEK is a kind of typical thermoplasticity high-performance polymer; Have performances such as high temperature resistant, anti-solvent, ageing-resistant, hydrolysis and high specific tenacity, specific modulus; Particularly in hot and humid severe environment, still can keep good comprehensive performances; Therefore, to material performance requirement increasingly high today, the importance of PEEK and matrix material thereof highlights day by day.In recent years, along with the raising that macromolecular material use temperature, carrying capacity and wear resistance are required, traditional high molecular abrasion-proof is wiped material, and for example nylon, tetrafluoroethylene etc. more and more are difficult to satisfy request for utilization.Polyetheretherketone has self lubricity, is a kind of good scratch-resistant material, yet still exists heat-drawn wire low; Problems such as frictional coefficient is higher, the accumulation of frictional heat can cause the polyether-ether-ketone resin deliquescing, plastic deformation takes place and causes bigger wear rate; Therefore; Lot of domestic and international researchist adopts the method for Wear-resistant fillers such as adding spun glass, silit, graphite that it is carried out modification, but its limitation is all arranged, and effect is not very good.For example solid lubricant can obviously reduce wear rate, but often need be than higher loading level, and high filler loading capacity can bring other performance, the particularly rapid decline of mechanical property.Inorganic particulate and fiber-like filler often can reduce abrasion loss, but limited to reducing the frictional coefficient effect, and price comparison is high.Except wear resisting property itself, dimensional stability also has very important meaning to the processing and manufacturing of component, and the processing of precision parts just requires material to have very high dimensional stability.Polyetheretherketone itself has lower linear expansivity and molding shrinkage, but for the plurality of applications field, the dimensional stability of polyetheretherketone still needs further to improve.
Wollastonite is a kind of emerging inorganic mineral filler; Have that cheap, reserves are abundant, wear-resisting wiping, dimensional stability is good, product surface is smooth; Plurality of advantages such as glossiness is good are filler with the wollastonite, not only can give better scratch-resistant performance of polyetheretherketone and dimensional stability; Also can reduce cost greatly, solve the restriction that fancy price is used PEEK to a certain extent.Therefore; We combine the characteristics and the market requirement of PEEK and wollastonite itself; With wollastonite and spun glass is filler; Be used the high temperature resistant coupling agent of self-control, designing and preparing a series of matrix materials, this material has excellent mechanical property, good dimensional stability (lower molding shrinkage and linear expansivity) and good scratch-resistant performance; Its outstanding performance will have certain competitive edge with relative lower cost in the world market, be expected to be applied to wear-resisting wiping parts such as precise part such as electric connector and gear, valve block.
The background technology relevant with the present invention is the compound method technology (Chinese patent " preparation method of polyether ethersulfone and polyetheretherketoneterpolymer terpolymer " of polyether-ether-ketone resin; Application number 200610016723.6; Not only can prepare polyether ethersulfone but also can prepare polyether-ether-ketone resin and their multipolymer) and article (Preparation and Properties of Poly (Ether Ether Ketone) the Composites Reinforced by Modified Wollastonite Grafting with Different Oligomers that delivered of the inventor; High Performance Polymers; 2011,23 (2) 160-169).Further; Utilize above-mentioned patent synthetic polyether-ether-ketone resin add wollastonite and spun glass and different content like synthetic coupling agent in the article; Prepared a series of matrix materials through melt extruding process for granulating, can be applied in the precision parts manufacturing that requires to have under the unlubricated dose of condition scratch-resistant performance with high-dimensional stability and scratch-resistant performance.
Summary of the invention
The objective of the invention is to prepare a kind of polyether-ether-ketone composite material, to be applied to the manufacturing of wear-resisting wiping precision parts with high-dimensional stability and scratch-resistant performance.
At present a lot of component (like bearing, gear, valve block etc.) are very high to the dimension precision requirement of goods; Promptly require to have very little linear expansivity and molding shrinkage; Require to have self lubricity simultaneously, promptly under nothing adds the condition of lubricant, keep lower frictional coefficient and wear rate.The present invention adopts polyetheretherketone, wollastonite, spun glass and high temperature resistant coupling agent etc., through different proportionings, has prepared a series of matrix materials, when satisfying above-mentioned requirements, also has higher mechanical property.
The wear-resisting wiping polyether-ether-ketone composite material of high-dimensional stability of the present invention; It is characterized in that: each component and press 100wt% and calculate; The polyether-ether-ketone resin that contains 60～90wt%, the high temperature resistant coupling agent of 0.05～0.12wt%, the wollastonite of 5～20wt% and the spun glass of 0～30wt%.
Used polyether-ether-ketone resin melting index is 12～90g/10min, and grinding to form particle diameter is to use behind 200～400 purpose powder.
Further preferred embodiment comprises the matrix material of following two kinds of prescriptions,
Prescription a:
PEEK resin 90wt%
Wollastonite 9.88wt%～9.95wt%
High temperature resistant coupling agent 0.05～0.12wt%
Prescription b:
PEEK resin 60～75wt%
Wollastonite 5～20wt%
Spun glass 15～30wt%
Polyetheretherketone (PEEK) structural formula is shown in (I), and n is >=1 integer, the expression polymerization degree.
High temperature resistant coupling agent is the self-control of this seminar, powdered soluble property solid.Coupling agent can form an interfacial layer between strongthener and resin matrix, effectively transmit stress, thereby improves performance of composites.And commercially available coupling agent commonly used is difficult to bear the processing temperature of polyetheretherketone up to 360 ℃, and structure also differs greatly with polyetheretherketone, therefore is difficult to be applied in the polyetheretherketone industry.For this reason, we design the high temperature resistant coupling agent of polyarylether oligopolymer (High Performance Polymers, 2011 of having synthesized several kinds of different structures; 23 (2); 160-169), similar on the structure with polyetheretherketone, and have higher temperature classification; Be polyetheretherketonematerials materials ideal interface reinforcing aids, this part work is delivered.The structure of several kinds of coupling agents is as follows, and three kinds of coupling agents are designated as g-R, g-A, g-S respectively;
One of preparation method of polyether-ether-ketone composite material of the present invention is:
At N
2Protection down; Ratio in 1g: 20～60mL is dissolved in high temperature resistant coupling agent in the organic solvent (DMF, DMAc or chloroform), adds wollastonite then, stirs; Be heated to reflux temperature; In the volume ratio of organic solvent and water is that 50: 1～80: 1 ratio adds entry, continues reflux 1～4 hour, obtains modified grammite behind the suction filtration; With modified lime stone with organic solvent washing after in vacuum drying oven under 80～120 ℃ of temperature oven dry remove organic solvent; With the modified grammite after the oven dry and the powder of polyetheretherketone; Premix is even in impeller; Join twin screw extruder through feed hopper, through twin screw extruder extrude, granulation, obtain containing the polyether-ether-ketone composite material of PEEK resin, wollastonite, high temperature resistant coupling agent; Through thermal gravimetric analyzer (TGA) test, each component and press 100wt% calculating contains the PEEK resin of 90wt%, the wollastonite of 9.88wt%～9.95wt%, the high temperature resistant coupling agent of 0.05～0.12wt%.
The preparing method's of polyether-ether-ketone composite material of the present invention two is:
(1) with the powder of wollastonite and polyetheretherketone, premix is even in impeller again, joins twin screw extruder through feed hopper, through twin screw extruder extrude, granulation, obtain containing the polyether-ether-ketone composite material pellet of PEEK resin and wollastonite;
(2) the polyetheretherketone powder is joined twin screw extruder through feed hopper; First exhaust ports of spun glass from twin screw extruder imported; Through twin screw extruder extrude, granulation, obtain containing the polyether-ether-ketone composite material pellet of PEEK resin and spun glass;
(3) powder with polyetheretherketone joins twin screw extruder through feed hopper, through twin screw extruder extrude, granulation, obtain pure polyetheretherketone pellet;
(4) after the pellet that step (1), (2), (3) is obtained mixes by a certain percentage, join twin screw extruder, extrude, obtain polyether-ether-ketone composite material of the present invention after the granulation through the twin screw extruder secondary through feed hopper; Through thermal gravimetric analyzer (TGA) test, each component and press 100wt% calculating contains the PEEK resin of 60～75wt%, the wollastonite of 5～20wt%, the spun glass of 15～30wt%.
Description of drawings
The frictional coefficient curve of Fig. 1: embodiment 1 said matrix material;
The friction ratio Changing Pattern figure of Fig. 2: embodiment 1 said matrix material;
The frictional coefficient curve of Fig. 3: embodiment 3, embodiment 6, embodiment 7 and embodiment 8 said matrix materials;
The frictional coefficient curve of Fig. 4: embodiment 2, embodiment 3, embodiment 4 and embodiment 5 said matrix materials;
The friction ratio Changing Pattern figure of Fig. 5: embodiment 3, embodiment 6, embodiment 7 and embodiment 8 said matrix materials;
The molding shrinkage Changing Pattern figure of Fig. 6: embodiment 3, embodiment 5 and embodiment 8 said matrix materials;
Fig. 1, Fig. 3, Fig. 4 have provided the Changing Pattern of the friction coefficient of composite material of three kinds of prescriptions respectively.By finding out that the adding of wollastonite and spun glass can reduce the frictional coefficient of material significantly among the figure.Among Fig. 1, through the wollastonite after the surface graft modification processing, because the interface keying action of filler and resin increases; The reinforced effects of wollastonite is more obvious; The ability that the hard thing of opposing dual face thrusts increases, and than unmodified wollastonite, wollastonite and matrix bond after the grafting are tight; The particle of protrusion is more wear-resisting; Be difficult for from matrix, deviating to form abrasive particle, so the grammite composite material frictional coefficient after the modification will be significantly less than unmodified wollastonite and virgin resin, the stable state frictional coefficient has descended about 50%.Can find out that from Fig. 3 and Fig. 4 the frictional coefficient of matrix material is all less than virgin resin, this is because the wollastonite and the wear-resisting property of spun glass of composite material surface protrusion are good, has reduced the real contact area of dual face, thereby has reduced frictional coefficient; Simultaneously wollastonite can improve the surface property of matrix material, alleviates the surface irregularity that the adding of spun glass causes and the frictional coefficient that causes raises.Yet along with the increase of amount of filler, the frictional coefficient of material is in rising trend.This is because the PEEK resin matrix is limited to the crystallized ability of filler, when amount of filler than higher the time, constantly have filler to come off, form abrasive particle, caused the rising of frictional coefficient.
Fig. 2, Fig. 5 have provided the Changing Pattern of the worn composite rate of two kinds of prescriptions respectively.Among Fig. 2, the adding of wollastonite has significantly reduced the wear rate of material, has reduced about 40%; And through after the grafting processing, the wear rate of material has shown different variation tendencies, and the wear rate of W-R packing material is basic the same with W; There is not significant difference, and the material that W-S and W-A fill, wear rate has all had further decline; Wherein W-A enhanced bill of material has revealed best wear resistance, and wear rate has descended 70%.The wearing and tearing of material all are several kinds of coefficient results of mechanism usually; The existence of wollastonite has limited the plastic deformation of PEEK; Thereby make the adhesive wear degree reduce, the wollastonite particle of protrusion has reduced the real contact area of frictional interface, and the hardness of wollastonite itself and wear resistance are very high; Not easy to wear, thus the degree of material abrasive wear is also descended to some extent.Wollastonite after handling through surface grafting, because better interface interaction, wollastonite particle difficult drop-off also increases the limitation capability of matrix plastic deformation, so shown better wear resistance.As can be seen from Figure 5, along with the increase of amount of filler, rise after the wearing and tearing of matrix material take the lead in descending, this is because rigid filled adding has reduced the real contact area of dual face, thereby makes the wearing and tearing of resin reduce; But resin matrix has its limit to the crystallized ability of filler, and when amount of filler was too high, filler constantly came off from matrix, forms abrasive particle, has aggravated abrasive wear, and rise in the back so wearing and tearing take the lead in descending.But in general, the introducing of wollastonite and spun glass can reduce the wear rate of material greatly, the highest one magnitude that descends.
Fig. 6 has provided the Changing Pattern of molding shrinkage.After adding wollastonite and spun glass, the radial shrinkage ratio of material descends obvious, is merely 50% of virgin resin, and does not change with the variation of amount of filler.This be since one add wollastonite and spun glass after, the linear expansivity of material descends, so the reduction of thermal contraction degree; Two come the introducing of wollastonite and spun glass to reduce the crystal property of material, make crystallization shrink and also weakened that so comprehensive, the introducing of spun glass and wollastonite has significantly reduced the molding shrinkage of material, has improved the dimensional stability of material.
Embodiment
Embodiment 1:
At N
2Protection is dissolved in three kinds of high temperature resistant coupling agent g-R, g-A, each 6g of g-S among the 300ml organic solvent DMF respectively down, adds the 100g wollastonite then; Stir, be heated to 152 ℃ of reflux temperatures after, in system, add 5ml water; Continued reflux 1 hour; Suction filtration, with DMF washing 3 times, organic solvent is removed in 80 ℃ of oven dry in vacuum drying oven with the modified grammite that obtains.The powder 900g of modified grammite 100g that obtains and polyetheretherketone is mixed, and premix is even in impeller, then through the twin screw extruder granulation, promptly obtains polyether-ether-ketone composite material of the present invention.
The linear expansivity of each component material is as shown in table 1; Because wollastonite itself has lower linear expansivity; The good interface effect that high temperature resistant coupling agent provided has simultaneously limited the motion of PEEK molecule segment greatly, so matrix material of the present invention has lower linear expansivity than pure PEEK resin; The influence that the size of material is expanded with heat and contract with cold by environment is littler, more favourable preparation high-dimensional stability component.
Table 1: high temperature resistant coupling agent is to the influence of matrix material linear expansivity (ppm/K)
Annotate: PEEK is a virgin resin, and PEEK/W is the matrix material that unmodified wollastonite is filled preparation, and PEEK/W-R, PEEK/W-S, PEEK/W-A are respectively and use coupling agent g-R, g-A, and g-S carries out the matrix material that surface modification treatment obtains to wollastonite.
Embodiment 2:
The PEEK powder of unmodified wollastonite 400g and 600g is mixed on high-speed mixer, add the feed hopper of twin screw extruder, use then that twin screw extruder is extruded, granulation, obtain the pellet 1 that 1000g wollastonite content is 40wt%;
The REEK powder of 600g is added the feed hopper of twin screw extruder, the continuous glass fibre of 400g is imported from twin screw first exhaust ports, use then that twin screw extruder is extruded, granulation, obtaining the 1000g content of glass fiber is the pellet 2 of 40wt%; Spun glass used in the present invention is the alkali free glass fibre that Hangzhou Qiantangjiang Special Glass Techn Co., Ltd. produces;
The REEK powder of 1000g is added the feed hopper of twin screw extruder, use then that twin screw extruder is extruded, granulation, obtain the pure PEEK pellet 3 of 1000g;
Get 125g pellet 1; 500g pellet 2; 375g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that the twin screw extruder secondary is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 5wt% wollastonite, 20wt% spun glass, be designated as PEEK/5wt%W/20wt%GF.
Embodiment 3:
Get the 250g pellet 1 of embodiment 2 preparations; 500g pellet 2; 250g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that twin screw extruder is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 10wt% wollastonite, 20wt% spun glass, be designated as PEEK/10wt%W/20wt%GF.
Embodiment 4:
Get the 375g pellet 1 of embodiment 2 preparations; 500g pellet 2; 125g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that twin screw extruder is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 15wt% wollastonite, 20wt% spun glass, be designated as PEEK/15wt%W/20wt%GF.
Embodiment 5:
Get the 500g pellet 1 of embodiment 2 preparations; 500g pellet 2; 0g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that twin screw extruder is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 20wt% wollastonite, 20wt% spun glass, be designated as PEEK/20wt%W/20wt%GF.
Embodiment 6:
Get the 250g pellet 1 of embodiment 2 preparations; 375g pellet 2; 375g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that twin screw extruder is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 10wt% wollastonite, 15wt% spun glass, be designated as PEEK/10wt%W/15wt%GF.
Embodiment 7:
Get the 250g pellet 1 of embodiment 2 preparations; 625g pellet 2; 125g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that twin screw extruder is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 10wt% wollastonite, 25wt% spun glass, be designated as PEEK/10wt%W/25wt%GF.
Embodiment 8:
Get the 250g pellet 1 of embodiment 2 preparations; 750g pellet 2; 0g pellet 3 mixes on high-speed mixer, adds the feed hopper of twin screw extruder, uses then that twin screw extruder is extruded, granulation; Obtain containing the polyether-ether-ketone composite material of 10wt% wollastonite, 30wt% spun glass, be designated as PEEK/10wt%W/30wt%GF.
The linear expansivity of embodiment 3, embodiment 6, embodiment 7 and embodiment 8 said matrix materials is as shown in table 2; Because wollastonite and spun glass all have lower linear expansivity; Has the motion that has limited the PEEK molecule segment than the spun glass of high length-diameter ratio greatly simultaneously, so matrix material of the present invention has lower linear expansivity than pure PEEK resin; The influence that the size of material is expanded with heat and contract with cold by environment is littler, more favourable preparation high-dimensional stability component.
Table 2: wollastonite and spun glass ratio are to the influence of matrix material linear expansivity (ppm/K)
Claims (2)
1. wear-resisting wiping polyether-ether-ketone composite material of high-dimensional stability is characterized in that: each component and press 100wt% and calculate contains polyether-ether-ketone resin, the wollastonite of 5～20wt% and the spun glass of 15～30wt% of 60～75wt%.
2. the preparation method of the wear-resisting wiping polyether-ether-ketone composite material of the described a kind of high-dimensional stability of claim 1 the steps include:
(1) with the powder of wollastonite and polyetheretherketone; Premix is even in impeller again; Join twin screw extruder through feed hopper, through twin screw extruder extrude, granulation, obtain containing the polyether-ether-ketone composite material pellet of polyether-ether-ketone resin and wollastonite;
(2) the polyetheretherketone powder is joined twin screw extruder through feed hopper; First exhaust ports of spun glass from twin screw extruder imported; Through twin screw extruder extrude, granulation, obtain containing the polyether-ether-ketone composite material pellet of polyether-ether-ketone resin and spun glass;
(3) powder with polyetheretherketone joins twin screw extruder through feed hopper, through twin screw extruder extrude, granulation, obtain pure polyetheretherketone pellet;
(4) after the pellet that step (1), (2) and (3) is obtained mixes by a certain percentage; Join twin screw extruder through feed hopper; Extrude, obtain polyether-ether-ketone composite material after the granulation through the twin screw extruder secondary; Each component and press 100wt% and calculate contains polyether-ether-ketone resin, the wollastonite of 5～20wt% and the spun glass of 15～30wt% of 60～75wt%.
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| CN103146134A (en) * | 2011-12-06 | 2013-06-12 | 黑龙江鑫达企业集团有限公司 | High strength and high heat-resistant glass fiber reinforced polyether ether ketone composite material and preparation method thereof |
| CN102653584B (en) * | 2012-04-25 | 2014-06-25 | 金发科技股份有限公司 | Polyether-ether-ketone resin as well as preparation method and application thereof |
| CN102827455B (en) * | 2012-09-09 | 2014-04-23 | 吉林大学 | Poly(ether-ether-ketone)-based dental special material with high bonding strength and preparation method thereof |
| TWI464472B (en) * | 2013-03-15 | 2014-12-11 | Protai Photonic Co Ltd | Back post for optical fiber connector |
| CN103613905B (en) * | 2013-11-25 | 2015-09-09 | 大连路阳科技开发有限公司 | With the petroleum prospecting of fiberglass reinforced polyether-ether-ketone pressure break ball and manufacture method thereof |
| CN104844775A (en) * | 2015-05-30 | 2015-08-19 | 吉林大学 | Expanded graphite flake/polyether-ether-ketone wear-resistant composite material and preparation method thereof |
| US11352480B2 (en) | 2016-03-18 | 2022-06-07 | Ticona Llc | Polyaryletherketone composition |
| CN106147424A (en) * | 2016-08-12 | 2016-11-23 | 安庆市七仙女电器制造有限公司 | A kind of electric iron high-temperature resistant coating and preparation method thereof |
| CN107090158A (en) * | 2017-05-09 | 2017-08-25 | 常州德毅新材料科技有限公司 | A kind of wear-resisting polyetheretherketonematerials materials and preparation method thereof |
| US11118053B2 (en) | 2018-03-09 | 2021-09-14 | Ticona Llc | Polyaryletherketone/polyarylene sulfide composition |
| CN109735051A (en) * | 2019-01-03 | 2019-05-10 | 漳州优普激光科技有限公司 | A kind of high-strength abrasion-proof ceramic plastic gear and preparation method thereof |
| CN113024993B (en) * | 2021-03-24 | 2023-01-31 | 广州机械科学研究院有限公司 | Polyether-ether-ketone composite material and preparation method and application thereof |
| CN114262433B (en) * | 2021-11-15 | 2024-04-26 | 吉林省中研高分子材料股份有限公司 | Coupling agent and polyaryletherketone composite material prepared from coupling agent |
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