CN101220196A - Poly(ether-ether-ketone) composite material, production method and application of sealing member - Google Patents
Poly(ether-ether-ketone) composite material, production method and application of sealing member Download PDFInfo
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- CN101220196A CN101220196A CNA2008100187243A CN200810018724A CN101220196A CN 101220196 A CN101220196 A CN 101220196A CN A2008100187243 A CNA2008100187243 A CN A2008100187243A CN 200810018724 A CN200810018724 A CN 200810018724A CN 101220196 A CN101220196 A CN 101220196A
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Abstract
The invention relates to a polyether-ether-ketone composite material which consists of polyether-ether-ketone, nanoparticles, filling materials and addition agent materials. The composite material comprises 75 to 95 portions of polyether-ether-ketone powders, 5 to 10 portions of the nanoparticles, 10 to 20 portions of the filling materials and 2 to 5 portions of the additive agents by weight. The filling materials are glass fiber, carbon fiber, quartz powder and MoS2 or toner. A method of compression moulding forming adopted is that: materials is prepared according to the formula; materials are mixed: the materials prepared according to designed requirements poured into an automatic material mixing machine for evenly mixing, the mixing time is between 0.5 minute and 3 minutes, then compressing process is carried out, and the blended mixture is sent to a mould cavity for moulding. The material can be used for sealing materials products. Various valve sealing elements produced by the invention has properties of creep resisting, corrosion resistance, heat resistance and pressurization, etc.; the ability of pressurization and wear resistance of the material are improved, and at the same time the cost is lowered by 10 to 20 percent or even higher, thus being beneficial to using and promotion of the materials.
Description
Technical field
The present invention relates to a kind of polyether-ether-ketone composite material, sealing member application and preparation method, especially nano material enhancing modified polyether-ether-ketone sealing member (KT-PEEK) and preparation method, belong to sealing material goods field.
Background technology
Polyether-ether-ketone (PEEK) resin is a kind of special engineering plastics of excellent performance, compare with other special engineering plastics and to have many significant advantages, characteristics as: high temperature resistant, mechanical property is excellent, self lubricity good, fire-retardant, the anti-separability of chemicals-resistant burn into, radioresistance, insulativity stable, hydrolysis and easily processing etc., in field widespread uses such as aerospace, automobile making, electric, medical treatment and food-processings.
The excellent performance of polyether-ether-ketone (PEEK) resin is used extensively, and the PEEK resin obtains to use as far back as aerospace field, and substitution of Al and other metallic substance are made various airplane components.Have good crocking resistance and mechanical property owing to the PEEK resin in the automotive industry, as the starting material of making the engine inner cover, in transmission, brake and the air-conditioning system of automobile, be widely adopted with various component such as the bearing of its manufacturing, pad, sealing member, clutch coupling ring gears.The PEEK resin is the ideal electrical insulator, under abominable working conditions such as high temperature, high pressure and high humidity, still can keep the excellent electric insulating energy, therefore electronic information field becomes the second largest Application Areas of PEEK resin gradually, can make pipeline, valve and the pump of carrying ultrapure water in chemical machinery field; In semi-conductor industry, be commonly used to make wafer carrying device, electronic isolation diaphragm and various connecting device.As a kind of hemicrystalline engineering plastics, PEEK is insoluble to the outer nearly all solvent of the vitriol oil, thereby is commonly used to make compressor valve plate, piston ring, sealing member and various chemical pump body, valve part.
In order further to satisfy the requirement of making high precision, heat-resisting, wear-resistant, antifatigue and shock resistance component, PEEK is carried out enhancing modified such as blend, filling, fiber composite and handle, can obtain the excellent more PEEK matrix material of performance.Matrix material after PEEK and the polyethers blend when having excellent mechanical performances, makes flame retardant properties be improved again; In PEEK, add the material that special-purpose resol is made, have special friction resistant performance; PEEK and the polytetrafluoroethylblended blended matrix material of making in the high strength that keeps PEEK, high rigidity, also have outstanding wear resistance, can be used for making components of machine such as sliding surface bearing, wear ring; Carry out modification with multiple fibers such as carbon fiber and glass fibre and strengthen, can be made into high performance fibre-reinforced PEEK matrix material, have excellent creep resistance, moisture-proof heat, ageing-resistant and shock resistance, also can increase substantially the stretching and the flexural strength of material; In PEEK, add crystal whisker materials, can improve hardness, rigidity and the dimensional stability of material, be used to make hydrogen gas compressor and the ring-type of petroleum gas compressor, netted valve block etc. on the large-scale petrochemical production line.
Valve and pipeline are very important in industry transports, its sealing problem significant, otherwise run, drip, leak wastes resource can be very serious, along with countries in the world are also more and more higher to environmental requirement, saves the energy, improves that to transport efficient, put and end to waste be necessary requirement.In the prior art, the most of materials such as tetrafluoroethylene, nylon, graphite, carbon fibers/fiberglass filled polytetrafluoroethylene matrix material, stainless steel that adopt of sealing members such as the seat material of valve.Its relative merits are all clearly: the polytetrafluoroethylmaterial material good corrosion resistance, and frictional coefficient is little, and is also little to the moment of torsion of valve, but heatproof is poor, life-time service temperature≤200 ℃, and also easily creep causes leaking; Graphite material is high temperature resistant, light specific gravity, but not withstand voltage, easily fragmentation causes leaking; Nylon material resistance to compression, hardness are good, and price is relatively cheap, but the corrosion-resistant tetrafluoroethylene that can not show a candle to, heatproof also is lower than tetrafluoroethylene relatively; Carbon fibers/fiberglass filled polytetrafluoroethylene matrix material is more withstand voltage, wear-resistant than pure polytetrafluoroethylmaterial material, heatproof increases, but because the resin base material of this material remains fluoro-resin for 70 parts, its temperature can only be≤250 ℃ of work, life-time service temperature≤200 ℃, and hydrolytic resistance is poor; Metallic substance, for example stainless steel, heatproof, withstand voltage, erosion resistance is better, but frictional coefficient is big, than great, can not recover elasticity, sealing effectiveness is bad.
The performance of polyether-ether-ketone is good, but its cost height, therefore must keep under the prerequisite of corrosion-resistant, heatproof, withstand voltage polyether-ether-ketone excellent properties, also must further improve mechanical property, improve withstand voltage and anti abrasive intensity, the system mouth and the preparation technology of the matrix material of the polyether-ether-ketone that reduces cost simultaneously also are not suggested.
Summary of the invention
The objective of the invention is, proposing a kind of polyether-ether-ketone composite material, preparation method and sealing member uses, keep original corrosion-resistant, the heatproof of polyether-ether-ketone, withstand voltage excellent properties, further improve mechanical property again, especially improve withstand voltage and anti abrasive intensity, reduce cost simultaneously, more help the use and the popularization of this material.
The object of the invention also is: the sealing members such as valve seat that adopt metal reinforced polyether ether ketone matrix material to be made during sealing member is used solve the Controlling System sealing in the fluid engineering.The present invention also aims to: provide a kind of both withstand voltage, high temperature resistant, 260 ℃ of life-time service temperature, hydrolytic resistance is good, simultaneously corrosion-resistant, creep resistance.Can satisfy the demand of current international and domestic various valve valve base seals fully.
Technical solution of the present invention is: polyether-ether-ketone composite material, form by polyether-ether-ketone, nanoparticle, packing material, promoter material, calculate by weight, it is composed as follows: 75～95 parts in polyether-ether-ketone powder, 5～10 parts of nanoparticles, 10～20 parts of packing materials, 2～5 parts of auxiliary agents.
Described packing material is: glass fibre, carbon fiber, silica powder, molybdenumdisulphide or carbon dust, glass fibre or carbon fiber can add silica powder, molybdenumdisulphide or carbon dust a kind of, two kinds or two kinds, described ratio is weight ratio.Glass fibre or carbon fiber also can mix filling.
The present invention can add auxiliary agent in addition: perfluoroethylene-propylene or polyphenylene sulfide or interpolation fluoroplastics (as tetrafluoroethylene or vinylidene material) 2～10 parts.Described nano material is a nano inoganic particle, and the employing natural clay is a raw material, and major ingredient is SiO
2, Al
2O
3, MgO, through purification, emulsification, ion-exchange, absorption and grafting etc. for several times chemical reactions handle, prepare the crystal type with one dimension Nano structure, the powder of enhancement type.The preparation method of nano material enhancing modified polyether-ether-ketone sealing member may further comprise the steps (seeing Table 1) successively, also can adopt pure nanometer SiO
2, Al
2O
3Or MgO.
The preparation method of polyether-ether-ketone composite material: the method that adopts compression molding: by above-mentioned prescription batching; Batch mixing is poured automatic mixer into by the material that design requirements will prepare, and carries out batch mixing and mixing, and mixing time was at 0.5～3 minute, and the mixer rotating speed is 2000 ± 1000 rev/mins; Compacting adds the former powder behind the mixing in the mold cavity, under the room temperature or the condition of slightly heating, (generally with 20MPa/min speed pressurization), gauge pressure reaches 10～50MPa/cm
2, beginning is venting progressively, and pressurize is 6 ± 4 minutes then, the prefabrication moulding; With the prefabrication that suppresses, put into special sintering furnace, carry out sintering by following sintering process parameter: slowly evenly be warming up to 390 ± 25C ° with 6 ± 1 hours; And be incubated 4 ± 1 hours; And slowly evenly reduced to room temperature from 390 ± 25C ° in 6 ± 1 hours.
The improvement of technology of the present invention also comprises: handle through second annealing, in order to eliminate material stress distortion, 200 ℃ ± 20 ℃ of temperature, 2 ± 1 hours time again.
The preparation method of polyether-ether-ketone composite material: adopt injection moulding, its step is as follows: drying, the polyether-ether-ketone feed particulate material is carried out drying, and go in the air circulating oven 150 ℃ ± 5 ℃ bakings 2～3 hours; The charging opening temperature of injection moulding machine should remain between 70 ℃～100 ℃; The temperature of sprue bush is controlled at more than 340 ℃.
Polyether-ether-ketone composite material of the present invention is made various valve sealing elements.The application of polyether-ether-ketone composite material sealing member: the skeleton of sealing member adopts metalwork, wraps up in matrix material 1-3mm of the present invention outward.
Polyether-ether-ketone composite material of the present invention is made various valve sealing elements and is possessed creep resistance, corrosion-resistant, heatproof, characteristics such as withstand voltage, further improved mechanical property, especially improve withstand voltage and anti abrasive intensity, reduce cost 10～20% simultaneously, more help the use and the popularization of this material.Especially fully satisfy the requirement that valve and pipeline do not leak, important effect is played in reliability, the security of complete machine.Invent the valve base seal that is made with metal reinforced polyether ether ketone matrix material, mainly solve the Controlling System sealing in the fluid engineering.260 ℃ of life-time service temperature of the present invention, hydrolytic resistance is good, simultaneously corrosion-resistant, creep resistance.Can satisfy the demand of current international and domestic valve valve base seal fully.
Four, description of drawings
Fig. 1 is a technological process block diagram of the present invention
Fig. 2 is a sintering heating curve of the present invention
Fig. 3 is another sintering heating curve of the present invention
Fig. 4 is the cross section structure synoptic diagram of sealing member of the present invention
Five, embodiment
1,1. prepare burden: at normal temperatures plurality of raw materials elder generation drying is handled, carried out automatic weighing by the prescription requirement, the batching end changes batch mixing after the assay was approved over to.2. batch mixing: the material that will prepare is poured high speed mixer into and is carried out batch mixing, mixing time 1～2 minute, and about 2000 rev/mins of rotating speeds, must batch mixing even.3. compacting: former powder behind the mixing is poured in the die cavity of mould, at normal temperatures, and with the speed extrusion forming of 20MPa/min, dwell pressure 30MPa/min, 3～10 minutes dwell times.4. sintering: prefabrication is put into the sintering oven sintering, and the sintering parametric line sees Table one, allows goods reach crystalline state, after sintering finishes, takes out goods.
Fig. 1 is seen in technical process of the present invention
The salient features (table 1) of nano material enhancing modified polyether-ether-ketone sealing member material of the present invention
Table 1:
| Characteristic | State | Testing method | Unit | Index |
| Density | Crystallization | ISO1183 | g/cm 3 | 1.51 |
| Water-absorbent | 24H 23℃ | ISO62 | Part | 0.009 |
| Thermal expansivity | ASTM D696 | 10-5℃ -1 | 2.2 | |
| Continuous use temperature | Machinery | UL746B | ℃ | 250 |
| Compressive strength | 23 ℃ of parallel directions | ASTM D695 | MPa | 210 |
| Rockwell hardness | The M level | ASTM D785 | 102 |
Embodiment 1: make 30 of sealing member 195/ Φ 145 * 17 size products, total amount 10kg.
1, composition of raw materials:
Polyether-ether-ketone powder 7.5kg
Nanoparticle 1kg
Perfluoroethylene-propylene or polyphenylene sulfide 0.5kg
Glass fibre 1kg (Fibre diameter 6～12um, length-to-diameter ratio was at 3: 1～11: 1)
2, mix: adopt high speed mixer to mix 2000 rev/mins of mixing velocities, mixing time 2 minutes.
3, as above-mentioned condition compression moulding, with gas heat-carrying sintering process sintering, 380 ± 10 ℃ of sintering top temperatures are incubated 3 hours, 50～80 ℃/H of warming and cooling rate.
4, second annealing is handled, and eliminates the material stress distortion, 200 ℃ ± 20 ℃ of temperature, 2 hours time.
5, detect the laggard capable machining of size.
Embodiment 2: adopt the charcoal fiber to be added into 2kg and can make goods fully, and meet and exceed the performance of the foregoing description.
Embodiment 3: sealing member adopts the metallic framework material better, can save matrix material of the present invention.Reduce cost.
Method embodiment, (one) compression molding:
1, batching, 65～90 parts of polyether-ether-ketones, 10～30 parts in glass fibre, 2～10 parts of tetrafluoroethylene, 5～10 parts of molybdenumdisulphide, 10～30 parts on carbon fiber.Above ratio is a weight ratio.
2, batch mixing is poured automatic mixer into by the material that design requirements will prepare, and carries out batch mixing and mixing, and mixing time was at 0.5～1 minute, and the mixer rotating speed is 2000 rev/mins.
3, compacting adds the former powder behind the mixing in the mold cavity, and under 20 ± 5 ℃ of conditions of room temperature, with the speed pressurization of 20MPa/min, gauge pressure reaches 50MPa/cm
2, beginning is venting progressively, and pressurize is 6 minutes then, the prefabrication moulding.
4, with the prefabrication that suppresses, put into special sintering furnace, press Fig. 1 sintering process parameter and carry out sintering.
5, with preform sintering finished after, initial survey is qualified again by being machined to required size, final inspection is qualified to dispatch from the factory.
(2) injection moulding:
1, drying is carried out drying with the polyether-ether-ketone feed particulate material, because should can absorb 0.5 part by material
w/ W atmospheric water causes the injection moulding pore, and in order to obtain best effect, moisture is less than 0.02wt%.Method: material is put into 150 ℃ ± 5 ℃ bakings of air circulating oven 2～3 hours.
2, barrel temperature: the column well heater that the barrel of injection moulding machine links to each other must reach 400 ℃, and reinforced for finishing correct hopper, the charging opening temperature should remain between 70 ℃～100 ℃.
3, nozzle and block sytem
In normal operating process, the nozzle and the sprue bush of barrel all can be in contact with one another in the most of the time in full cycle cycle.The temperature of sprue bush is starkly lower than melts and nozzle.If temperature drops to below 340 ℃, expect very fast curing, therefore need enough big well heater is installed in the nozzle place, to prevent cooling and to produce " cold slug ".
4, injection and clamp force
Goods and the runner shadow area on joint face has determined to penetrate under the pressure in maximum, prevents the clamp force that opening of mould is required.Representative value 65～140MPa.
Injection moulding process of the present invention and requirement can be with reference to other thermoplasticss.
Implement as Fig. 4 manufactured size Φ 181/ Φ 158 * 13.8
Fig. 4 is a product structure synoptic diagram of the present invention
This product uses through on-the-spot, and effect is fine, has satisfied customer requirement.
The technical indicator that this product reaches is as follows, sees Table 2.
Table 2
| Characteristic | State | Testing method | Unit | Index |
| Density | The noncrystalline attitude of crystal form | ISO1183 | g/cm 3 | 1.51 |
| Water-absorbent | 24 hours 23 ℃ | ISO62 | Part | 0.11 |
| Fusing point | DSC | ℃ | 343 | |
| Thermal expansivity | ASTM D696 | 10 -5℃ -1 | 2.2 | |
| Continuous use temperature | Electricapparatus | UL746B | ℃ | 240 |
| Specific inductivity | 50HZ 0℃～150℃ | 1EC250 | n/a | 3.7 |
| Tensile strength | Surrender 23 ℃ | ISO 527-2/18/50 | MPa | 155 |
| Stretch percentage elongation | Rupture 23 ℃ | ISO 527-2/18/50 | |
2 |
| Compressive strength | The parallel direction vertical direction | ASTM D695 | MPa | 215 149 |
| Rockwell hardness | The M level | ASTM D785 | 107 |
Claims (10)
1. polyether-ether-ketone composite material, it is characterized in that forming by polyether-ether-ketone, nanoparticle, packing material, promoter material, calculate by weight, it is composed as follows: 75～95 parts in polyether-ether-ketone powder, 5～10 parts of nanoparticles, 10～20 parts of packing materials, 2～5 parts of auxiliary agents.
2. by the described polyether-ether-ketone composite material of claim 1, it is characterized in that described packing material is: glass fibre, carbon fiber, silica powder, molybdenumdisulphide or carbon dust.
3. by the described polyether-ether-ketone composite material of claim 2, it is characterized in that glass fibre or carbon fiber add silica powder, molybdenumdisulphide or carbon dust a kind of, two kinds or two kinds, described ratio is weight ratio.
4. by the described polyether-ether-ketone composite material of claim 2, it is characterized in that glass fibre or carbon fiber mix filling.
5. by the described polyether-ether-ketone composite material of claim 2, it is characterized in that described auxiliary agent is: perfluoroethylene-propylene or polyphenylene sulfide.
6. by the described polyether-ether-ketone composite material of claim 2, it is characterized in that nano inoganic particle adopts pure nanometer SiO
2, Al
2O
3, MgO or major ingredient be SiO
2, Al
2O
3, MgO, and through purification, emulsification, ion-exchange, absorption and grafted nanometer natural clay.
7. the preparation method of polyether-ether-ketone composite material is characterized in that adopting the method for compression molding: by above-mentioned prescription batching; Batch mixing is poured automatic mixer into by the material that design requirements will prepare, and carries out batch mixing and mixing, and mixing time was at 0.5～3 minute, and the mixer rotating speed is 1000-3000 rev/min; Compacting adds the former powder behind the mixing in the mold cavity, and under the room temperature or the condition of slightly heating, gauge pressure reaches 10～50MPa/cm
2, beginning is venting progressively, and pressurize 2-10 minute then, the prefabrication moulding; With the prefabrication that suppresses, put into special sintering furnace, carry out sintering by following sintering process parameter: slowly evenly to be warming up to 390 ± 25C in 5-7 hour; And be incubated 3-5 hour; And slowly evenly reduced to room temperature from 390 ± 25C in 5-7 hour.
8. the preparation method of polyether-ether-ketone composite material, the preparation method who it is characterized in that polyether-ether-ketone composite material: adopt injection moulding, its step is as follows: drying, the polyether-ether-ketone feed particulate material is carried out drying, and go in the air circulating oven 150 ℃ ± 5 ℃ bakings 2～3 hours; The charging opening temperature of injection moulding machine should remain between 70 ℃～100 ℃; The temperature of sprue bush is controlled at more than 340 ℃.
9. by the preparation method of claim 7 or 8 described polyether-ether-ketone composite materials, it is characterized in that handling, in order to eliminate material stress distortion, 200 ℃ ± 20 ℃ of temperature, 2 ± 1 hours time through second annealing.
10. the application of polyether-ether-ketone composite material sealing member, the skeleton of sealing member adopts metalwork, wraps up in the described matrix material 1-3mm of one of claim 1 to 6 outward.
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