CN101475729A - Polyether-ether-ketone ketone resin special material for electric connector and preparation thereof - Google Patents
Polyether-ether-ketone ketone resin special material for electric connector and preparation thereof Download PDFInfo
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- CN101475729A CN101475729A CNA2009100664637A CN200910066463A CN101475729A CN 101475729 A CN101475729 A CN 101475729A CN A2009100664637 A CNA2009100664637 A CN A2009100664637A CN 200910066463 A CN200910066463 A CN 200910066463A CN 101475729 A CN101475729 A CN 101475729A
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Abstract
The invention relates to a special material for polyether ether-ketone ketone resin used for an electric connector and a preparation method thereof. The special material comprises the following compositions in percentage by weight: 60.0 to 100.0 percent of the polyether ether-ketone ketone resin, 0 to 3.0 percent of a high-temperature lubricant, 0 to 10 percent of a polyaryletherketone liquid crystal polymer, and 0 to 30 percent of a reinforced material. The polyether ether-ketone ketone resin has a logarithmic viscosity number of between 0.72 and 0.76, and a melt index of between 30 and 80g/10min. The high-temperature lubricant is granular or powdered GENIOPLAST Pellet S manufactured by Wacker Chemie AG; the polyaryletherketone liquid crystal polymer is a polyaryletherketone liquid crystal polymer containing fluorin; and the reinforced material can be glass fiber, basalt fiber or crystal whisker potassium titanate. The special material for the polyether ether-ketone ketone resin used for the electric connector can be made into various electric connectors with shapes and dimensions of die cavities through plasticized melting, injecting, filling, cool forming and demolding by a high-temperature injection machine.
Description
Technical field
The invention belongs to macromolecular material and field of compound material thereof, be specifically related to a kind of polyether-ether-ketone ketone resin special material for electric connector and preparation method thereof.
Background technology
Polyether-ether-ketone keto-resin is a kind of higher than the polyether-ether-ketone resin temperature classification half hitch crystal formation aromatic polymer of the special engineering plastics the Ministry of Education of Jilin University Engineering Research Center exploitation, has characteristics such as temperature classification height, radiation hardness, shock strength height, wear resistance and resistance to fatigue are good, fire-retardant, electrical property excellence.To obtain to use more widely in fields such as aerospace, automobile, electric, chemical industry, machinery and medical treatment.Because different field, different goods have different use properties requirements, single polyether-ether-ketone keto-resin can't satisfy service requirements, need to adopt strongtheners such as glass fibre, carbon fiber, basalt fibre to carry out modification, to satisfy the different demands in above-mentioned field.Purpose of the present invention is exactly the polyether-ether-ketone ketone resin special material for electric connector that satisfies the different user needs in order to prepare.
Background technology related to the present invention is the synthetic method technology (Chinese patent: " synthesizing of high-viscosity polyether-ether-ketone keto-resin containing biphenyl structure; the patent No.: ZL 97102708.0 " and " preparation of poly (aryl ether ketone) copolymer; the patent No.: ZL 01138739.4 " not only can prepare polyether ether ketone ketone, biphenyl contenting structure polyether ether ketone ketone but also can prepare polyether-ether-ketone resin and their multipolymer) of polyether-ether-ketone keto-resin.Further, utilize above-mentioned patent synthetic polyether-ether-ketone keto-resin to add processing aid or reinforced modifier, make polyether-ether-ketone ketone resin special material for electric connector by melt extruding process for granulating.Electric connector requires resin purity higher with resin, and electrical insulating property will be got well, and the melt flowability will be got well, and molding shrinkage is low, and the electric connector dimensional precision of making is higher.The electric connector PP Pipe Compound that the present invention developed can satisfy above-mentioned service requirements.
Summary of the invention
The objective of the invention is to prepare a kind of high-performance electric connector polyether ether ketone ketone PP Pipe Compound that is used for aerospace, field such as electric, promptly utilize additives such as polyether-ether-ketone keto-resin and high temperature lubricant, melt viscosity modifiers to prepare high-performance electric connector polyether ether ketone ketone PP Pipe Compound by melt extruding process for granulating.
Polyether-ether-ketone keto-resin molecular chain rigidity is bigger, and processing temperature is higher, and melt viscosity is higher, and processing fluidity is bad, influences the dimensional precision and the quality of electric connector, can't satisfy the service requirements of high-performance electric connector.
The present invention adopts high temperature lubricant, melt viscosity modifiers (is a poly aromatic ether ketone liquid crystal copolymer, concrete preparation method has applied for patent of invention " preparation of poly aromatic ether ketone liquid crystal copolymer; ZL 01103522.6 ") wait additive to improve the processing characteristics of electric connector usefulness polyether-ether-ketone keto-resin, adopt glass fibre, basalt fibre and whisker etc. are the enhancing modified material, make resin property can satisfy the service requirements of electric connector, enough processing fluidities are arranged again, thus can be by injection, methods such as mold pressing preparations is that the high-performance electric connector of insulating material is to satisfy the user demand of different field with polyether-ether-ketone keto-resin and modifying material.
High-performance polyether-ether-ketone ketone resin special material for electric connector of the present invention, press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 60.0～100.0wt%, the high temperature lubricant of 0～3.0wt%, the poly aromatic ether ketone liquid crystal copolymer of structural formula shown in (II) and the strongthener of 0～30wt% of 0～10.0wt%.
First kind of preferred implementation as high-performance polyether-ether-ketone ketone resin special material for electric connector of the present invention, press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 67.0～99.5wt%, the high temperature lubricant of 0.5～3.0wt% and the strongthener of 0～30wt%.Prescription a, d described below, e, f are the further preferred embodiments of this kind situation.
Second kind of preferred implementation as high-performance polyether-ether-ketone ketone resin special material for electric connector of the present invention, press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 60.0～98.0wt%, the poly aromatic ether ketone liquid crystal copolymer of structural formula shown in (II) and the strongthener of 0～30wt% of 2.0～10.0wt%.Prescription b, g described below, h, i are the further preferred embodiments of this kind situation.
The third preferred implementation as high-performance polyether-ether-ketone ketone resin special material for electric connector of the present invention, pressing each component and 100wt% calculates, the polyether-ether-ketone keto-resin that contains 87.0～97.5wt%, the high temperature lubricant of 0.5～3.0wt%, the poly aromatic ether ketone liquid crystal copolymer of the structural formula of 2～10.0wt% shown in (II).Prescription c described below is the further preferred embodiment of this kind situation.
As the 4th kind of preferred implementation of high-performance polyether-ether-ketone ketone resin special material for electric connector of the present invention, press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 70.0～85.0wt%, the strongthener of 15～30wt%.
Strongthener is mainly glass fibre, basalt fibre and potassium titanate crystal whisker, and glass fibre is a continuous fibre, and model is the non-twist winding yarn of E 1200TEX and high strength glass fiber SC11-1200TEX; Basalt fibre is a continuous fibre, and model is the 1200TEX roving, and the high temperature modification surface treatment agent is handled; The potassium titanate crystal whisker diameter is 0.5～2.5 μ m, and length is 10～100 μ m, and tensile strength is 7000MPa, and Young's modulus is 270Gpa, and Mohs' hardness is 4, and proportion is 3.1～3.3g/cm
3, fusing point is higher than 1300 ℃.
Further preferred implementation comprises following 9 kinds of prescriptions:
Prescription a:PEEKK resin 97.0～99.5wt%
High temperature lubricant 0.5～3.0wt%
Prescription b:PEEKK resin 90.0～98.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2.0～10.0wt%
Prescription c:PEEKK resin 87.0～97.5wt%
High temperature lubricant 0.5～3.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2.0～10wt%
Prescription d:PEEKK resin 67.0～79.5wt%
High temperature lubricant 0.5～3.0wt%
Glass fibre 20.0～30wt%
Prescription e:PEEKK resin 67.0～79.5wt%
High temperature lubricant 0.5～3.0wt%
Basalt fibre 20.0～30.0wt%
Prescription f:PEEKK resin 67.0～79.5wt%
High temperature lubricant 0.5～3.0wt%
Potassium titanate crystal whisker 20.0～30.0wt%
：
Prescription g PEEKK resin 60.0～78.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2～10.0wt%
Glass fibre 20.0～30.0wt%
Prescription h:PEEKK resin 60.0～78.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2～10.0wt%
Basalt fibre 20.0～30.0wt%
Prescription i:PEEKK resin 60.0～78.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2～10.0wt%
Potassium titanate crystal whisker 20.0～30.0wt%
The logarithmic specific concentration viscosity of polyether ether ketone ketone (PEEKK) is 0.72～0.76, melting index is 30～80g/10min, and its structural formula is shown in (I), and n is 〉=1 integer, the expression polymerization degree.
(I)
High temperature lubricant is that particulate state or the pulverulent GENIOPLASTPellet S that German Wacker company produces (is abbreviated as GPPS, the processing temperature of polyether-ether-ketone keto-resin is very high, general lubricant can't satisfy service requirements at all, has just decomposed before 360 ℃.This lubricant is that our seminar filters out for many years, and unique processing temperature that satisfies us is very effective again, has only this English name, does not have Chinese).
The structural formula of poly aromatic ether ketone liquid crystal copolymer is shown in (II):
Y=0.2～0.8, n is 〉=1 integer, the expression polymerization degree.
The preparation process of above-mentioned high-performance polyether-ether-ketone ketone resin special material for electric connector is as follows:
(1) with 1,4 '-(4-fluoro-benzoyl group) benzene, sulfobenzide join in the polymeric kettle that mechanical stirring, thermometer, nitrogen feeding mouth, thermoelectric Europe are housed, nitrogen protection, heated and stirred, in 140～170 ℃ of temperature ranges, add the mixed salt salt forming agent more successively, mix biphenol monomer '-biphenyl diphenol and Resorcinol, temperature programming, temperature is raised to 320 ℃ by 190 ℃, obtains polyether ether ketone ketone (PEEKK) polymkeric substance of logarithmic specific concentration viscosity 0.72～0.76, melting index 30～80g/10min after the temperature control reaction; To obtain pressed powder after polymkeric substance cooling, pulverizing, the filtration, again pressed powder is boiled, filters with ethanol or acetone boiling method, repeat 5～6 times, boil, filter with distilled water again, repeat 5～6 times, in rotatory drier, dry at last, obtain purified polyether ketone copolymer resin powder; Wherein to account for 0.1～2%, 1,4 '-(the 4-fluoro-benzoyl group) benzene monomer that mixes biphenol monomer be 1.00:0.970～0.995 with the mol ratio of mixing biphenol monomer to the '-biphenyl diphenol mole number; The mol ratio of mixing biphenol monomer and mixed salt salt forming agent is 1:1.05～1.20; The polymeric reaction solution solid content is 15～35%;
(2) ratio in prescription takes by weighing polyether ether ketone ketone (PEEKK) copolymer resin powder; high temperature lubricant and poly aromatic ether ketone liquid crystal copolymer; use the high-speed stirring mixer premix; put into the resin powder feeding hopper of twin screw extruder then; in extruder barrel under 365～410 ℃ of temperature fusion plastification; form melt; the glass fibre that will need ratio again; basalt fibre or potassium titanate crystal whisker strongthener are by the fiber spout feeding forcing machine of twin screw extruder; with the compound blend of PEEKK melt; processing temperature is 365～410 ℃; through head and four aperture template extruded stock bars; the material bar is carried through travelling belt; air cooling; lead into the hobboing cutter dicing machine; obtaining diameter is 2～4mm, and length is the cylindrical pellet of 4～6mm, promptly gets polyether-ether-ketone ketone resin special material for electric connector.
Temperature control reaction described in the aforesaid method is under agitation, be heated to 180～220 ℃ of temperature control reactions 0.5～2 hour, progressively stir again and be warmed up to 250～260 ℃ of isothermal reactions 0.5～1 hour, be warmed up to 280～300 ℃ of temperature control reactions 0.5～2 hour again, be heated to 300～320 ℃ of reactions 3～6 hours at last;
Mixed salt salt forming agent described in the aforesaid method is the mixing of salt of wormwood and yellow soda ash, and wherein the salt of wormwood mole number accounts for 10～90% of mixed salt salt forming agent.
Above-mentioned various insulation high-performance polyether-ether-ketone ketone resin special material for electric connector, again through injector fusion, injection melt in mould, cooling and shaping, the demoulding can make the electric connector of mold cavity shape and size.High-insulativity, high-mechanical property, high fluidity of molten and low molding shrinkage make material of the present invention can be used for electric connector.It mainly is the high-performance electric connector that aerospace, weaponry are used.
Description of drawings
Fig. 1: the adding of high temperature lubricant is to the curve of twin screw extruder screw torque influence;
Fig. 2: the adding of high temperature lubricant is to the thermally-stabilised sex curve of resin PP Pipe Compound;
Fig. 3: the adding of fluorinated poly arylene ether ketone liquid crystalline polymers is to the curve of resin PP Pipe Compound melting index (MI) influence;
The infrared spectra of Fig. 4: embodiment 1 synthetic polyether-ether-ketone ketone polymer.
As shown in Figure 1, after curve representation polyether-ether-ketone keto-resin and glass fiber compound material do not add high temperature lubricant and add high temperature lubricant, the changing conditions of twin screw extruder screw torque when producing electric connector with the polyether ether ketone ketone PP Pipe Compound, as seen from the figure, for pure polyether-ether-ketone keto-resin, the interpolation weight percentage is 1% high temperature lubricant GPPS, the moment of torsion of extruder screw drops to 68Nm by original 90Nm, add weight percentage and be 3% high temperature lubricant GPPS, the moment of torsion of extruder screw drops to 60Nm (among the figure shown in the curve of square mark); And for glass fibre reinforced modified polyether ether ketone ketone matrix material, the interpolation weight percentage is 1% high temperature lubricant GPPS, the moment of torsion of extruder screw drops to 67Nm by original 92Nm, add weight percentage and be 3% high temperature lubricant GPPS, the moment of torsion of extruder screw drops to 57Nm (among the figure shown in the curve of circular ring marks).This shows, can significantly reduce the melt viscosity of polyether-ether-ketone keto-resin and glass fiber reinforced polyester ether ether ketone ketone matrix material behind the adding high temperature lubricant.
Whether can the thermal characteristics of polyether-ether-ketone keto-resin be impacted after studying the adding high temperature lubricant, we have tested pure polyether-ether-ketone keto-resin and have added the thermal weight loss of the polyether-ether-ketone keto-resin of high temperature lubricant.As shown in Figure 2, two curves are arranged wherein, one is pure polyether-ether-ketone ketone resin special material thermostability curve, and one is that as seen polyether-ether-ketone ketone resin special material thermostability curve does not almost have difference between the two after adding high temperature lubricant.
After Fig. 3 shows that polyether-ether-ketone keto-resin adds fluorinated poly arylene ether ketone liquid crystalline polymers, the changing conditions of resin melting index, curve following among the figure is that shear-stress is 5kg/mm
2, the melting index that the polyether-ether-ketone keto-resin that records under 400 ℃ adds the blend of fluorinated poly arylene ether ketone liquid crystalline polymers changes.Clearly, can significantly increase the melting index of polyether-ether-ketone keto-resin after liquid crystalline polymers adds.
Among Fig. 4,1648cm
-1The place is the stretching vibration absorption peak of carbonyl; 1495cm
-1And 1602cm
-1The place is the phenyl ring vibration absorption peak; 1420cm
-1The place is an ehter bond stretching vibration absorption peak; 1220cm
-1The place is the vibration absorption peak of phenylate group, shows that institute's synthetic polymkeric substance is a polyether-ether-ketone keto-resin.
Embodiment
Embodiment 1:
With 1 of purifying, 4 '-(4-fluoro-benzoyl group) benzene, sulfobenzide join in the polymeric kettle that mechanical stirring, thermometer, nitrogen feeding mouth, thermopair are housed, nitrogen protection, heated and stirred, in the time of 150 ℃, add mixed salt salt forming agent, '-biphenyl diphenol, Resorcinol successively, continue to be stirred and heated to 190 ℃ of temperature control reactions 1 hour, progressively stir again and be warmed up to 250 ℃ of isothermal reactions 0.5 hour, be warmed up to 290 ℃ of temperature control reactions 1 hour, be heated to 320 ℃ of reactions 4 hours at last, obtain polyether ether ketone ketone (PEEKK) polymkeric substance; With obtaining pressed powder after polymkeric substance cooling, pulverizing, the filtration, again pressed powder is boiled, filters with the ethanol boiling method, repeat 6 times, boil, filter with distilled water again, repeat 6 times, in rotatory drier, dry at last, obtain purified polyether ketone copolymer resin powder; Wherein '-biphenyl diphenol accounts for and mixes 0.1% of biphenol monomer total mole number; 1,4 '-(4-fluoro-benzoyl group) benzene monomer and mix biphenol monomer and mol ratio be 1.000:0.985; The mol ratio of biphenol monomer and mixed salt salt forming agent is 1:1.10; The polymeric reaction solution solid content is 25%; The mixed salt salt forming agent is the mixing of salt of wormwood and yellow soda ash, and wherein the salt of wormwood mole number accounts for 10% of mixed salt salt forming agent, makes logarithmic specific concentration viscosity and be 0.75 polyether-ether-ketone keto-resin, and melting index is 32g/10min.
Get the logarithmic specific concentration viscosity that makes previously and be 0.75 polyether-ether-ketone keto-resin (PEEKK) 1000 grams, in twin screw extruder, melt extrude granulation, extruder barrel adopts the heating of 8 segmentations, each section Heating temperature is respectively 260,370,385,400,410,390,380,370 ℃, PEEKK is 370,385,400,410,390,380, fusion plastification in 370 ℃ the temperature range, the screw torque of forcing machine is 88～90Nm (shown in Fig. 1 square mark curve), make non-additive polyether-ether-ketone ketone resin special material for electric connector, the tensile strength of PP Pipe Compound is 110MPa.
Embodiment 2:
As described in embodiment 1, the reduced viscosity of just taking the logarithm is 0.75 polyether-ether-ketone keto-resin (PEEKK) 990 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 67～69Nm (shown in Fig. 1 square mark curve), making particulate state high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 1wt%, the thermostability of PP Pipe Compound and pure polyether-ether-ketone ketone resin special material basic identical (as shown in Figure 2), the tensile strength of PP Pipe Compound is 113MPa.
Embodiment 3:
As described in embodiment 2, the reduced viscosity of just taking the logarithm is 0.75 polyether-ether-ketone keto-resin (PEEKK) 970 grams, granular high temperature lubricant GE NIOPLAST Pellet S 30 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 58～61Nm (shown in Fig. 1 square mark curve), making particulate state high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 3wt%, and the tensile strength of PP Pipe Compound is 112MPa.
Embodiment 4:
As described in embodiment 2, just change granular high temperature lubricant into pulverulent high temperature lubricant, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 67～69Nm, and making powder shape high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 1wt%, and the tensile strength of PP Pipe Compound is 113MPa.
Embodiment 5:
As described in embodiment 3, just change granular high temperature lubricant into pulverulent high temperature lubricant, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 58～61Nm, and making powder shape high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 3wt%, and the tensile strength of PP Pipe Compound is 112MPa.
Embodiment 6:
With 1 of purifying, 4 '-(4-fluoro-benzoyl group) benzene, sulfobenzide join in the polymeric kettle that mechanical stirring, thermometer, nitrogen feeding mouth, thermopair are housed, nitrogen protection, heated and stirred, in the time of 150 ℃, add mixed salt salt forming agent, '-biphenyl diphenol, Resorcinol successively, continue to be stirred and heated to 190 ℃ of temperature control reactions 1 hour, progressively stir again and be warmed up to 250 ℃ of isothermal reactions 1 hour, be warmed up to 290 ℃ of temperature control reactions 1 hour, be heated to 320 ℃ of reactions 4 hours at last, obtain polyether ether ketone ketone (PEEKK) polymkeric substance; With obtaining pressed powder after polymkeric substance cooling, pulverizing, the filtration, again pressed powder is boiled, filters with ethanol or acetone boiling method, repeat 6 times, boil, filter with distilled water again, repeat 6 times, in rotatory drier, dry at last, obtain purified polyether ketone copolymer product; Wherein '-biphenyl diphenol accounts for and mixes 0.1% of biphenol monomer total mole number; 1,4 '-(4-fluoro-benzoyl group) benzene monomer and two kinds of biphenol monomers and mol ratio be 1.000:0.975; The mol ratio of biphenol monomer and mixed salt salt forming agent is 1:1.10; The polymeric reaction solution solid content is 25%; The mixed salt salt forming agent is the mixing of salt of wormwood and yellow soda ash, and wherein the salt of wormwood mole number accounts for 15% of mixed salt salt forming agent, makes logarithmic specific concentration viscosity and be 0.73 electric connector polyether-ether-ketone keto-resin, and melting index is 66g/10min.
The reduced viscosity of taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 1000 grams, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,400,410,390,380,370 ℃, screw torque is 79～82Nm, make non-additive polyether-ether-ketone ketone resin special material for electric connector, the tensile strength of PP Pipe Compound is 110MPa.
Embodiment 7:
As described in embodiment 6, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 990 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 63～65Nm, making particulate state high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 1wt%, and the tensile strength of PP Pipe Compound is 114MPa.
Embodiment 8:
As described in embodiment 7, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone resin (PEEK) 970 grams, granular high temperature lubricant GENIOPLAST Pellet S 30 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 52～53Nm, making particulate state high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 3wt%, and the tensile strength of PP Pipe Compound is 112MPa.
Embodiment 9:
As described in embodiment 7, just change granular high temperature lubricant into pulverulent high temperature lubricant, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 63～65Nm, and making particulate state high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 1wt%, and its result is identical with embodiment 7.
Embodiment 10:
As described in embodiment 8, just change granular high temperature lubricant into pulverulent high temperature lubricant, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 52～53Nm, and making powder shape high temperature lubricant addition is the polyether-ether-ketone ketone resin special material for electric connector of 3wt%, and the tensile strength of PP Pipe Compound is 112MPa.
Embodiment 11:
Getting the melting index that embodiment 1 makes is polyether-ether-ketone keto-resin (PEEKK) 980 grams of 32g/10min, fluorinated poly arylene ether ketone liquid crystalline polymers 20 grams, its structural formula is shown in (III), the numerical value of y is 0.3, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,395,400,400,390,385,370 ℃, make the polyether-ether-ketone ketone resin special material for electric connector that the liquid crystalline polymers addition is 2wt%, the PP Pipe Compound melting index is 34.3g/10min (as shown in Figure 3), and the tensile strength of PP Pipe Compound is 112MPa.
Embodiment 12:
As described in embodiment 11, just get the polyether-ether-ketone keto-resin that melting index is 32g/10min (PEEKK) 960 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 40 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,380,395,395,395,390,385,370 ℃, make the polyether-ether-ketone ketone resin special material for electric connector that the liquid crystalline polymers addition is 4wt%, the PP Pipe Compound melting index is 37.4g/10min (accompanying drawing 3), and the tensile strength of PP Pipe Compound is 114MPa.
Embodiment 13:
As described in embodiment 11, just get the polyether-ether-ketone keto-resin that melting index is 32g/10min (PEEKK) 940 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 60 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, make the polyether-ether-ketone ketone resin special material for electric connector that the liquid crystalline polymers addition is 6wt%, the PP Pipe Compound melting index is that the tensile strength of 42.2g/10min (accompanying drawing 3) PP Pipe Compound is 116MPa.
Embodiment 14:
As described in embodiment 11, just get the polyether-ether-ketone keto-resin that melting index is 32g/10min (PEEKK) 920 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 80 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, make the polyether-ether-ketone ketone resin special material for electric connector that the liquid crystalline polymers addition is 8wt%, the PP Pipe Compound melting index is that the tensile strength of 47g/10min (accompanying drawing 3) PP Pipe Compound is 115MPa.
Embodiment 15:
As described in embodiment 11, just get the polyether-ether-ketone keto-resin that melting index is 32g/10min (PEEKK) 900 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 100 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, make the polyether-ether-ketone ketone resin special material for electric connector that the liquid crystalline polymers addition is 10wt%, the PP Pipe Compound melting index is 50g/10min (accompanying drawing 3), and the tensile strength of PP Pipe Compound is 117MPa.
Embodiment 16:
As described in embodiment 1, make logarithmic specific concentration viscosity and be 0.75 electric connector polyether-ether-ketone keto-resin, get polyether-ether-ketone keto-resin 935 grams, granular high temperature lubricant GENIOPLAST P ellet S 5 grams, fluorinated liquid crystal polymkeric substance 60 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 62～64Nm, making particulate state high temperature lubricant addition is 0.5wt%, fluorinated liquid crystal polymkeric substance addition is 6wt%, the polyether-ether-ketone keto-resin consumption is the polyether-ether-ketone ketone resin special material for electric connector of 93.5wt%, the thermostability of PP Pipe Compound is same as pure polyether-ether-ketone ketone resin special material, the moment of torsion of extruder screw is lower, and the tensile strength of PP Pipe Compound is 113MPa.
Embodiment 17:
As described in embodiment 16, get polyether-ether-ketone keto-resin 930 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, fluorinated liquid crystal polymkeric substance 60 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 56～58Nm, making particulate state high temperature lubricant addition is 1wt%, fluorinated liquid crystal polymkeric substance addition is 6wt%, the polyether-ether-ketone keto-resin consumption is the polyether-ether-ketone ketone resin special material for electric connector of 93wt%, the thermostability of PP Pipe Compound is same as pure polyether-ether-ketone ketone resin special material, the moment of torsion of extruder screw is lower, and the tensile strength of PP Pipe Compound is 115MPa.
Embodiment 18:
As described in embodiment 16, get polyether-ether-ketone keto-resin 910 grams, granular high temperature lubricant GENIOPLAST Pellet S 30 grams, fluorinated liquid crystal polymkeric substance 60 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 50～53Nm, making particulate state high temperature lubricant addition is 3wt%, fluorinated liquid crystal polymkeric substance addition is 6wt%, the polyether-ether-ketone keto-resin consumption is the polyether-ether-ketone ketone resin special material for electric connector of 91wt%, the thermostability of PP Pipe Compound is same as pure polyether-ether-ketone ketone resin special material, the moment of torsion of extruder screw is lower, and the tensile strength of PP Pipe Compound is 114MPa.
Embodiment 19:
As described in embodiment 16, get polyether-ether-ketone keto-resin 950 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, fluorinated liquid crystal polymkeric substance 40 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 58～60Nm, making particulate state high temperature lubricant addition is 1wt%, fluorinated liquid crystal polymkeric substance addition is 4wt%, the polyether-ether-ketone keto-resin consumption is the polyether-ether-ketone ketone resin special material for electric connector of 95wt%, the thermostability of PP Pipe Compound is same as pure polyether-ether-ketone ketone resin special material, the moment of torsion of extruder screw is lower, and the tensile strength of PP Pipe Compound is 115MPa.
Embodiment 20:
As described in embodiment 16, get polyether-ether-ketone keto-resin 930 grams, granular high temperature lubricant GE NIOPLAST Pellet S 30 grams, fluorinated liquid crystal polymkeric substance 40 grams, behind the high-speed stirring mixer premix, in twin screw extruder, melt extrude granulation, each of extruder barrel section Heating temperature is respectively 260,370,385,390,390,385,375,365 ℃, screw torque is 54～56Nm, making particulate state high temperature lubricant addition is 3wt%, fluorinated liquid crystal polymkeric substance addition is 4wt%, the polyether-ether-ketone keto-resin consumption is the polyether-ether-ketone ketone resin special material for electric connector of 93wt%, the thermostability of PP Pipe Compound is same as pure polyether-ether-ketone ketone resin special material, the moment of torsion of extruder screw is lower, and the tensile strength of PP Pipe Compound is 112MPa.
Embodiment 21:
As described in embodiment 6, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 800 grams, (model is the non-twist winding yarn of E 1200TEX with the 200g continuous glass fibre, Zhongcai Sci. ﹠ Tech. Co., Ltd, Nanjing) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,410,410,390,380,370 ℃, extruding pelletization, screw torque is 90～93Nm (shown in Fig. 1 circular ring marks curve), making the glass fibre addition is 20wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 80wt% glass fiber reinforced polyester ether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 140MPa.
Embodiment 22:
As described in embodiment 21, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 790 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, behind the high-speed stirring mixer premix, (model is the non-twist winding yarn of E1200TEX with continuous glass fibre, Zhongcai Sci. ﹠ Tech. Co., Ltd, Nanjing) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,400,400,390,380,370 ℃, the feed glass fibre content is 20wt%, extruding pelletization, screw torque is 66～68Nm (shown in Fig. 1 circular ring marks curve), making particulate state high temperature lubricant addition is 1wt%, the glass fibre addition is 20wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 79wt% glass fiber reinforced polyester ether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 144MPa.
Embodiment 23:
As described in embodiment 21, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 670 grams, granular high temperature lubricant GENIOPLAST Pellet S 30 grams, behind the high-speed stirring mixer premix, (model is the non-twist winding yarn of E 1200TEX with continuous glass fibre, Zhongcai Sci. ﹠ Tech. Co., Ltd, Nanjing) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,400,400,390,380,370 ℃, the feed glass fibre content is 30wt%, extruding pelletization, screw torque is 56～58Nm (shown in Fig. 1 circular ring marks curve), making particulate state high temperature lubricant addition is 3wt%, the glass fibre addition is 30wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 67wt% glass fiber reinforced polyester ether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 156MPa.
Embodiment 24:
As described in embodiment 21, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 720 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 80 grams, behind the high-speed stirring mixer premix, (model is the non-twist winding yarn of E 1200TEX with continuous glass fibre, Zhongcai Sci. ﹠ Tech. Co., Ltd, Nanjing) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,400,400,390,380,370 ℃, the feed glass fibre content is 20wt%, extruding pelletization, screw torque is 64～65Nm, making fluorinated poly arylene ether ketone liquid crystalline polymers addition is 8wt%, the glass fibre addition is 20wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 72wt% glass fiber reinforced polyester ether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 146MPa.
Embodiment 25:
As described in embodiment 21, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 800 grams, (model is the 1200TEX roving with continuous basalt fiber, the high temperature modification surface treatment agent is handled, Mudanjiang basalt fibre branch office of electric power Industry Group Co.,Ltd) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,410,410,390,380,370 ℃, control basalt fibre content is 20wt%, extruding pelletization, screw torque is 92～93Nm, making the basalt fibre addition is 20wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 80wt% basalt fibre reinforced polyether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 148MPa.
Embodiment 26:
As described in embodiment 21, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 790 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, behind the high-speed stirring mixer premix, (model is the 1200TEX roving with continuous basalt fiber, the high temperature modification surface treatment agent is handled, Mudanjiang basalt fibre branch office of electric power Industry Group Co.,Ltd) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,400,400,390,380,370 ℃, control basalt fibre content is 20wt%, extruding pelletization, screw torque is 67～70Nm, making particulate state high temperature lubricant addition is 1wt%, the basalt fibre addition is 20wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 79wt% basalt fibre reinforced polyether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 155MPa.
Embodiment 27:
As described in embodiment 26, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 620 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 80 grams, behind the high-speed stirring mixer premix, (model is the 1200TEX roving with continuous basalt fiber, the high temperature modification surface treatment agent is handled, Mudanjiang basalt fibre branch office of electric power Industry Group Co.,Ltd) fusion is compound in twin screw extruder, each of extruder barrel section Heating temperature is respectively 260,370,385,400,400,390,380,370 ℃, control basalt fibre content is 30wt%, extruding pelletization, screw torque is 70～72Nm, making fluorinated poly arylene ether ketone liquid crystalline polymers addition is 8wt%, the basalt fibre addition is 30wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 62wt% basalt fibre reinforced polyether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 167MPa.
Embodiment 28:
As described in embodiment 21, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 800 grams, potassium titanate crystal whisker 200 gram (crystal whisker of hexa potassium titanate, diameter is 0.5-2.5 μ m, length is 10-100 μ m, and tensile strength is 7000MPa, and Young's modulus is 270Gpa, Mohs' hardness is 4, and proportion is 3.1-3.3g/cm
3Fusing point is higher than 1300 ℃, Shanghai Jingxu Composite Material Co., Ltd.), behind the high-speed stirring mixer premix, fusion is compound in twin screw extruder, extruding pelletization, each of extruder barrel section Heating temperature is respectively 260,370,385,400,400,390,380,370 ℃, screw torque is 86～88Nm, making the potassium titanate crystal whisker addition is that 20wt%, polyether-ether-ketone keto-resin consumption are the electric connector potassium titanate crystal whisker reinforced polyether ether ketone ketone matrix material PP Pipe Compound of 80wt%, and the tensile strength of PP Pipe Compound is 124MPa.
Embodiment 29:
As described in embodiment 28, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 790 grams, granular high temperature lubricant GENIOPLAST Pellet S 10 grams, (crystal whisker of hexa potassium titanate, diameter are 0.5-2.5 μ m to potassium titanate crystal whisker 200 grams, and length is 10-100 μ m, tensile strength is 7000MPa, Young's modulus is 270Gpa, and Mohs' hardness is 4, and proportion is 3.1-3.3g/cm
3Fusing point is higher than 1300 ℃, Shanghai Jingxu Composite Material Co., Ltd.), behind the high-speed stirring mixer premix, fusion is compound in twin screw extruder, extruding pelletization, each of extruder barrel section Heating temperature is respectively 260,370,385,395,395,385,375,365 ℃, screw torque is 65～66Nm, making particulate state high temperature lubricant addition is 1wt%, the potassium titanate crystal whisker addition is 20wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 79wt% potassium titanate crystal whisker reinforced polyether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 128MPa.
Embodiment 30:
As described in embodiment 29, the reduced viscosity of just taking the logarithm is 0.73 polyether-ether-ketone keto-resin (PEEKK) 620 grams, fluorinated poly arylene ether ketone liquid crystalline polymers 80 grams, (crystal whisker of hexa potassium titanate, diameter are 0.5-2.5 μ m to potassium titanate crystal whisker 300 grams, and length is 10-100 μ m, tensile strength is 7000MPa, Young's modulus is 270Gpa, and Mohs' hardness is 4, and proportion is 3.1-3.3g/cm
3Fusing point is higher than 1300 ℃, Shanghai Jingxu Composite Material Co., Ltd.), behind the high-speed stirring mixer premix, fusion is compound in twin screw extruder, extruding pelletization, each of extruder barrel section Heating temperature is respectively 260,370,385,395,395,385,375,365 ℃, screw torque is 62～64Nm, making fluorinated poly arylene ether ketone liquid crystalline polymers addition is 8wt%, the potassium titanate crystal whisker addition is 30wt%, the polyether-ether-ketone keto-resin consumption is the electric connector of a 62wt% potassium titanate crystal whisker reinforced polyether ether ketone ketone matrix material PP Pipe Compound, and the tensile strength of PP Pipe Compound is 135MPa.
Claims (10)
1, polyether-ether-ketone ketone resin special material for electric connector, it is characterized in that: press each component and 100wt% and calculate, the polyether-ether-ketone keto-resin that contains 60.0～100.0wt%, the glass fibre of the high temperature lubricant of 0～3.0wt%, the poly aromatic ether ketone liquid crystal copolymer of 0～10.0wt% and 0～30wt%, basalt fibre or potassium titanate crystal whisker strongthener.
2, polyether-ether-ketone ketone resin special material for electric connector as claimed in claim 1, it is characterized in that: press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 67.0～99.5wt%, the high temperature lubricant of 0.5～3.0wt% and the strongthener of 0～30wt%.
3, polyether-ether-ketone ketone resin special material for electric connector as claimed in claim 1, it is characterized in that: press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 60.0～98.0wt%, the poly aromatic ether ketone liquid crystal copolymer of 2.0～10.0wt% and the strongthener of 0～30wt%.
4, polyether-ether-ketone ketone resin special material for electric connector as claimed in claim 1, it is characterized in that: press each component and press 100wt% calculating, the polyether-ether-ketone keto-resin that contains 87.0～97.5wt%, the high temperature lubricant of 0.5～3.0wt%, the poly aromatic ether ketone liquid crystal copolymer of 2.0～10.0wt%.
5, polyether-ether-ketone ketone resin special material for electric connector as claimed in claim 1 is characterized in that: press each component and 100wt% and calculate, contain the polyether-ether-ketone keto-resin of 70.0～85.0wt%, the strongthener of 15～30wt%.
6, polyether-ether-ketone ketone resin special material for electric connector as claimed in claim 1 is characterized in that: the structural formula of poly aromatic ether ketone liquid crystal copolymer is as follows,
R=Cl, Ph, CH
3O, t-C
4H
9Or
Or
Wherein, y=0.2～0.8, n is a positive integer, the expression polymerization degree.
7, the preparation method of any one described polyether-ether-ketone ketone resin special material for electric connector of claim 1～6, its step is as follows:
1) with 1,4 '-(4-fluoro-benzoyl group) benzene, sulfobenzide join in the polymeric kettle that mechanical stirring, thermometer, nitrogen feeding mouth, thermoelectric Europe are housed, nitrogen protection, heated and stirred, in 140～170 ℃ of temperature ranges, add the mixed salt salt forming agent successively, mix biphenol monomer '-biphenyl diphenol and Resorcinol, temperature programming, temperature is raised to 320 ℃ by 190 ℃, obtains the polyether-ether-ketone ketone polymer of logarithmic specific concentration viscosity 0.72～0.76, melting index 30～80g/10min after the temperature control reaction; To obtain pressed powder after polymkeric substance cooling, pulverizing, the filtration, again pressed powder is boiled, filters with ethanol or acetone boiling method, repeat 5～6 times, boil, filter with distilled water again, repeat 5～6 times, in rotatory drier, dry at last, obtain purified polyether ketone copolymer resin powder; Wherein to account for 0.1～2%, 1,4 '-(the 4-fluoro-benzoyl group) benzene monomer that mixes biphenol monomer be 1.00:0.970～0.995 with the mol ratio of mixing biphenol monomer to the '-biphenyl diphenol mole number; The mol ratio of mixing biphenol monomer and mixed salt salt forming agent is 1:1.05～1.20; The polymeric reaction solution solid content is 15～35%;
2) ratio in prescription takes by weighing polyether ketone copolymer resin powder; high temperature lubricant and poly aromatic ether ketone liquid crystal copolymer; use the high-speed stirring mixer premix; put into the resin powder feeding hopper of twin screw extruder then; in extruder barrel under 365～410 ℃ of temperature fusion plastification; form the polyether ether ketone ketone melt; the glass fibre that will need ratio again; basalt fibre or potassium titanate crystal whisker strongthener are by the fiber spout feeding forcing machine of twin screw extruder; with the compound blend of polyether ether ketone ketone melt; processing temperature is 365～410 ℃; through head and four aperture template extruded stock bars; the material bar is carried through travelling belt; air cooling; lead into the hobboing cutter dicing machine; obtaining diameter is 2～4mm, and length is the cylindrical pellet of 4～6mm, promptly gets polyether-ether-ketone ketone resin special material for electric connector.
8, as the preparation method of polyether-ether-ketone ketone resin special material for electric connector as described in the claim 7, it is characterized in that: described temperature control reaction is 180～220 ℃ of temperature control reactions 0.5～2 hour, progressively stir again and be warmed up to 250～260 ℃ of isothermal reactions 0.5～1 hour, be warmed up to 280～300 ℃ of temperature control reactions 0.5～2 hour, be heated to 300～320 ℃ of reactions 3～6 hours at last.
9, as the preparation method of polyether-ether-ketone ketone resin special material for electric connector as described in the claim 8, it is characterized in that: the mixed salt salt forming agent is the mixing of salt of wormwood and yellow soda ash, and wherein the salt of wormwood mole number accounts for 10～90% of mixed salt salt forming agent.
10, any one described polyether-ether-ketone ketone resin special material for electric connector of claim 1～6 obtains the various electric connectors of mold cavity shape and size through high temperature injection machine plastifying fusion, injection, mold filling, cooling and shaping, the demoulding.
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| CN101974204A (en) * | 2010-11-18 | 2011-02-16 | 吉林大学 | Basalt fibre reinforced polyetheretherketone (PEEK) composite and preparation method thereof |
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