CN105860284B - A kind of motor turning dust cover thermoplastic vulcanizate material and preparation method thereof - Google Patents
A kind of motor turning dust cover thermoplastic vulcanizate material and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
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Abstract
The invention discloses a kind of motor turning dust cover thermoplastic vulcanizate materials and preparation method thereof, and raw material includes by weight：100 300 parts of EPDM, 20 80 parts of polypropylene, 10 50 parts of linear low density polyethylene, 40 100 parts of thermoplastic polyurethane elastomer, 5 15 parts of ethylene octene copolymer, 5 15 parts of compatilizer, 10 80 parts of inorganic filler, 35 parts of silane coupling agent, 0.2 10 parts of crosslinking agent, 15 parts of active Zinc Oxide, 13 parts of primary antioxidant, 0.5 1 parts of auxiliary anti-oxidant, 13 parts of ultra-violet absorber, 20 100 parts of processing oil, 26 parts of lubricant.The present invention, the thermoplastic vulcanizate material has excellent intensity, heat-resisting quantity and flexibility, and blow processability can be excellent.
Description
Technical field
The present invention relates to technical field of rubber material, especially a kind of motor turning dust cover thermoplastic vulcanizates material
Material and preparation method thereof.
Background technology
The major function of motor turning dust cover is to prevent dust, moisture, oil product, mud, sandstone etc. from entering turning machine system
System generates corrosion to pull rod, generates abrasion to sealing ring and cause entirely to turn to failure；By enging cabin high temperature and building ring
The influence in border requires its manufacture material to have higher high temperature resistance, ozone resistance, resistance to oil property and weather resistance, because
This requirement to material is also extremely important.Thermoplastic vulcanizates has good elasticity and compression resistant morphotropism, resistance to environment, resistance to
Aging is equivalent to EP rubbers, while its oil resistant solvent resistance is equally matched with polychloroprene rubber for general purpose.Thermoplastic vulcanizates
Rubber bodies can use in -60 DEG C of -135 DEG C of temperature ranges, and when thermoplastic vulcanizates body use need not vulcanize, can be direct
By modes machine-shapings such as blowings, processing process can be shortened, reduce processing cost.Mainstream turns to dust-proof currently on the market
Cover product uses thermoplastic vulcanizate material.
United States Patent (USP) US4311628/0272871A1 discloses the method for preparing thermoplastic vulcanizates, the elasticity
Body is EP rubbers, and resin is polypropylene, and it is vulcanization accelerator that vulcanizing system, which is Phenolic resin curative, two hydrated stannous chlorides,
Thermoplastic vulcanizates is prepared using dynamic vulcanization technology, but the vulcanized rubber for motor turning dust cover intensity,
Heat-resisting quantity and flexility are relatively poor, blowing processing or relatively difficult, therefore it is dust-proof to be not met by motor turning
The performance requirement of cover.
Invention content
The problem of based on background technology, the present invention propose a kind of motor turning dust cover thermoplastic vulcanizates rubber
Glue material and preparation method thereof, the thermoplastic vulcanizate material have excellent intensity, heat-resisting quantity and flexibility, and
And blow processability can be excellent.
A kind of motor turning dust cover thermoplastic vulcanizate material, raw material include by weight：EPDM100-300
Part, 20-80 parts of polypropylene, 10-50 parts of linear low density polyethylene, 40-100 parts of thermoplastic polyurethane elastomer, ethylene-octene
5-15 parts of copolymer, 5-15 parts of compatilizer, 10-80 parts of inorganic filler, 3-5 parts of silane coupling agent, 0.2-10 parts of crosslinking agent, activity
1-5 parts of Zinc Oxide, 1-3 parts of primary antioxidant, 0.5-1 parts of auxiliary anti-oxidant, 1-3 parts of ultra-violet absorber, 20-100 parts of processing oil, profit
2-6 parts of lubrication prescription；
Wherein, the EPDM is the E type ethylene-propylene-diene monomers for ethenylidene norbornene by the Third monomer of 40-60wt%
Glue, 10-30wt% Third monomer be the D types ethylene propylene diene rubber of dicyclopentadiene and the Third monomer of 20-40wt% is 1,
The H-type ethylene propylene diene rubber of 4- hexadienes forms；
The thermoplastic polyurethane elastomer is graphite modified polyurethane elastomer, and preparation method includes：By graphite powder
It is added in the mixed acid solution of concentrated nitric acid and concentrated sulfuric acid composition, water-bath after supersound process filters, washing, obtains oxidation stone
Ink；After polyetherdiol is dehydrated, isocyanates is added, is stirred to react 1-3h after being warming up to 80-100 DEG C, obtains isocyanate terminated
The performed polymer of base；Ultrasonic disperse in DMF is added in the graphite oxide, under conditions of nitrogen protection, is added isocyanate terminated
The performed polymer and catalyst dibutyl tin dilaurate of base, are stirred to react 1-3h after being warming up to 60-80 DEG C, be added chain extender and
Accelerating agent trihydroxymethyl propane, quickly stirs 0.01-0.02h, and stirring 0.01-0.02h is further continued for after vacuumizing, is filtered, and washing is ripe
Change, obtains the graphite modified polyurethane elastomer.
In a specific embodiment, the parts by weight of EPDM can be 105,110,130,150,160,180,195,200,
210、235、250、265、280、295；Polyacrylic parts by weight can be 25,30,35,45,50,60,65,70,75；It is linear low
The parts by weight of density polyethylene can be 12,15,17,20,25,28,31,33,36,39,41,45,47；Thermoplastic polyurethane bullet
Property body parts by weight can be 45,50,55,60,65,70,75,80,85,90,95；, the parts by weight of ethylene-octene copolymer can
Think 6,7,8,9,10,11,12,13,14；The parts by weight of compatilizer can be 6,7,8,9,10,11,12,13,14；It is inorganic to fill out
The parts by weight of material can be 12,16,18,20,24,30,35,42,56,60,65,70,75,78；The parts by weight of crosslinking agent can be with
It is 0.3,0.5,0.7,1,3,4,5,6,7,8,9.5；The parts by weight of processing oil can be 22,26,30,35,40,53,68,75,
80、85、90、95、98。
Preferably, the graphite modified method for preparing polyurethane elastic body includes：It is 1 that volume ratio, which is added, in graphite powder:
In the concentrated nitric acid of 1-3 and the mixed acid solution of the concentrated sulfuric acid, 1-3h is ultrasonically treated at 20-40 DEG C, then in 80-100 DEG C of water-bath
It is stirred to react 1-3h, is cooled to room temperature, is filtered, is washed with deionized to neutrality, obtains graphite oxide；Polyetherdiol is heated up
It is dehydrated 3-5h to 90-120 DEG C and after being evacuated to pressure≤- 0.09Mpa, is cooled to 40-60 DEG C, isocyanates is added, is risen
Temperature obtains the performed polymer of terminal isocyanate group to 1-3h is stirred to react after 80-100 DEG C；The graphite oxide is added in DMF and is surpassed
Performed polymer and the catalyst dibutyl tin osmanthus of terminal isocyanate group is added under conditions of nitrogen protection in sound dispersion 0.5-1h
Sour tin is stirred to react 1-3h after being warming up to 60-80 DEG C, chain extender and accelerating agent trihydroxymethyl propane is added, in 1000-
0.01-0.02h is quickly stirred under 1200rpm, and stirring 0.01-0.02h is further continued for after vacuumizing, with polytetrafluoroethylene (PTFE) membrane filtration,
Washing, cures 5-10h in 100-120 DEG C of drying box, obtains the graphite modified polyurethane elastomer；Preferably, graphite
Powder, polyetherdiol, isocyanates, dibutyl tin dilaurate, trihydroxymethyl propane weight proportion be 1:50-70:20-35:10-
20:0.05-0.1:2-4。
Preferably, the polyetherdiol is the tetrahydrofuran polyether PTMG or hydroquinone that number-average molecular weight is 800-1200
Two (2- ethoxys) ether HQEE；The isocyanates is hexamethylene diisocyanate, 2,4- toluene di-isocyanate(TDI)s, 2,6- first
At least one of phenylene diisocyanate, 2,4- methyl diphenylene diisocyanates, 4,4- methyl diphenylene diisocyanates；Institute
It is at least one of ethylene glycol, 1,4-butanediol, 1,6- hexylene glycols to state chain extender.
Preferably, the polypropylene is the homopolymerization type polypropylene of the copolymerized type propene polymer and 55-75wt% by 25-45wt%
Composition, and the melt index of the copolymerized type propene polymer is 0.5-10.0g/10min；The polyacrylic melting of homopolymerization type refers to
Number is 0.5-5.0g/10min.
Preferably, the compatilizer is maleic anhydride grafted ethene-octene copolymer POE-g-MAH, maleic anhydride is grafted
Styrene-ethylene-butadiene-styrene copolymer SEBS-g-MAH, maleic anhydride grafting ethylene propylene diene rubber EPDM-g-MAH
At least one of；The inorganic filler be wollastonite, talcum powder, glass microballoon, barium sulfate, mica powder, in clay at least
It is a kind of；The silane coupling agent is at least one of Silane coupling reagent KH-570, silane coupling A -137.
Preferably, it is 3-5 that the crosslinking agent, which is by weight proportion,:1 peroxide cross-linking agent and assistant crosslinking agent composition；It is excellent
Selection of land, the peroxide cross-linking agent are 2,5- dimethyl -2,5- bis(t-butylperoxy)s hexin, 2,5- dimethyl -2,5-
At least one of bis(t-butylperoxy) hexane, cumyl peroxide；The assistant crosslinking agent is polyester substance, poly- fourth
At least one of diene substance, cyanate substance, isocyanates substance, acrylate substance.
Preferably, the primary antioxidant is at least one of antioxidant 1010, antioxidant 3114, antioxidant DSTP；Institute
It is at least one in 2-mercaptobenzimidazole MB, triphenyl phosphite TPP, dilauryl thiodipropionate DLTP to state auxiliary anti-oxidant
Kind.
Preferably, the ultra-violet absorber be ultraviolet absorbent uv-326, in ultra-violet absorber UV-9 at least
It is a kind of；The processing oil is at least one of paraffin oil, naphthenic oil, hydrocarbon oil；The lubricant is that ethylene is double stearic
At least one of sour amide, oleamide, zinc stearate, calcium stearate.
A kind of preparation method of motor turning dust cover thermoplastic vulcanizate material, including：By EPDM, polypropylene,
It is linear low density polyethylene, thermoplastic polyurethane elastomer, ethylene-octene copolymer, compatilizer, inorganic filler, silane coupled
Mixing is uniform in agent, primary antioxidant, auxiliary anti-oxidant, ultra-violet absorber, processing oil and lubricant addition mixer, is re-fed into list
First time plastics are carried out in screw extruder, wherein screw speed is 200-400r/min, and the processing temperature plasticated for the first time is
160-180 DEG C, rubber master batch is obtained after pelletizing；The rubber master batch and crosslinking agent, active Zinc Oxide are added in high mixer,
0.3-0.5h is mixed under the speed conditions of 400-500rpm, transfers in double screw extruder and is plasticated for the second time, wherein
Screw slenderness ratio is 55-64, and feeding rotating speed is 30-80rpm, screw speed 300-500rpm, the processing temperature plasticated for the second time
Degree is 160-250 DEG C, and tie rod is cooling, and pelletizing obtains the motor turning dust cover thermoplastic vulcanizate material.
Preferably, the processing temperature plasticated for the second time is specially：One 160-180 DEG C of area's temperature, two area temperature 200-
210 DEG C, three 220-230 DEG C of area's temperature, four 240-250 DEG C of area's temperature, five 240-250 DEG C of area's temperature, six area temperature 235-245
DEG C, seven 225-235 DEG C of area's temperature, eight 210-220 DEG C of area's temperature, nine 205-215 DEG C of area's temperature, ten 200-210 DEG C of area's temperature.
In the present invention, the thermoplastic vulcanizate material uses the E types ethylene propylene diene rubber of specific proportioning, D type ternarys
The source of EP rubbers and H-type ethylene propylene diene rubber as EPDM makes its tensile strength, bending modulus and cross-linked polymeric degree all
In a rational state, in for motor turning dust cover, excellent durability and machine-shaping property can get；It is poly-
It is strong that the addition of propylene and linear low density polyethylene then not only enables the elastomeric material to obtain required melt forming
Degree, and can further improve the blow processability energy of the material；And due to polypropylene have good solvent resistance,
Heat resistance and processing fluidity can substantially improve the flexibility of elastomeric material itself when being compounded with EPDM, to meet
The performance requirement of motor turning dust cover；The ethylene-octene copolymer and compatilizer being added simultaneously can then significantly improve respectively
Compatibility between major ingredient obtains good comprehensive performance.
In addition, in the present invention, the thermoplastic polyurethane elastomer is modified it using graphite, by by graphite powder
Molecule has entered inside graphite after pickling, and the inside interlamellar spacing of graphite is widened, and interplanar distance increases, and makes after sonicated
It obtains graphite flakes shape structure to be destroyed, to increase the spacing of graphite platelet structure, graphite internal structure is made to become loosely simultaneously
And volume expands, and then forms the groups such as activity hydroxy on surface, then by with the polyurethane with terminal isocyanate group
Prepolymer reaction, and chain extender sealing end is added, a kind of graphite modified polyurethane elastomer is thus obtained, is realized to graphite surface
While activation, graphite platelet structure, thus obtained modification polyurethane elastomer are also introduced on the molecule of polyurethane elastomer
Body can form fine and close, efficient carbon-coating structure on the surface of the vulcanized rubber material, to effectively absorb heat, hinder heat
It is transmitted to elastomeric material internal layer, assigns the material good high temperature resistance；And above-mentioned modified thermoplastic polyurethane bullet
Property body make graphite platelet structure and be evenly dispersed in inside the matrixes such as EPDM with the state removed, the work of skeletal support can be played
With, or solid phase charcoal core is served as, enhance interfacial effect, is conducive to rubber material and obtains the mechanical effects such as excellent intensity.
In addition, the present invention is during preparing the thermoplastic vulcanizate material, using dynamic vulcanization technology, with organic
Peroxide cross-linking system can efficiently control the crosslinking degree of cross-linked material and uniform performance as vulcanizing agent；And make
With the processing technology of plasticating under special parameter so that Blending Processes are more abundant, the rubber phase grain size smaller in blend, distribution
Evenly, the entanglement effect of molecule interchain is smaller, and solution twines relatively easily, is avoided with this because caused by rubber material over cure
Mobility variation effect；It is additionally added a certain amount of antioxidant, lubricant and ultra-violet absorber in the present invention, thus makes system
Standby obtained thermoplastic vulcanizate material has good weather resistance and mechanical property.
Specific implementation mode
The technical scheme of the invention is described in detail through specific implementation examples.
Embodiment 1
A kind of motor turning dust cover thermoplastic vulcanizate material, raw material include by weight：EPDM100 parts,
80 parts of polypropylene, 10 parts of linear low density polyethylene, 100 parts of thermoplastic polyurethane elastomer, 5 parts of ethylene-octene copolymer, horse
15 parts of maleic anhydride grafted ethylene-octene copolymer POE-g-MAH, 10 parts of wollastonite, 5 parts of Silane coupling reagent KH-570, crosslinking
0.2 part of agent, 5 parts of active Zinc Oxide, 1 part of antioxidant 1010,1 part of 2-mercaptobenzimidazole MB, ultraviolet absorbent uv-326
1 part, 100 parts of paraffin oil, 2 parts of ethylene bis stearic acid amide；
Wherein, the EPDM is the E type ethylene-propylene-diene monomers for ethenylidene norbornene by the Third monomer of 40wt%
Glue, 30wt% Third monomer be the D types ethylene propylene diene rubber of dicyclopentadiene and the Third monomer of 30wt% be Isosorbide-5-Nitrae-oneself two
The H-type ethylene propylene diene rubber of alkene forms；
The thermoplastic polyurethane elastomer is graphite modified polyurethane elastomer, and preparation method includes：By graphite powder
It is 1 that volume ratio, which is added,:In 1 concentrated nitric acid and the mixed acid solution of the concentrated sulfuric acid, 1h is ultrasonically treated at 40 DEG C, then in 100 DEG C of water
It is stirred to react 1h in bath, is cooled to room temperature, filters, is washed with deionized to neutrality, obtains graphite oxide；By polyetherdiol liter
Temperature is dehydrated 3h to 120 DEG C and after being evacuated to pressure≤- 0.09Mpa, is cooled to 60 DEG C, and isocyanates is added, is warming up to 80
It is stirred to react 3h after DEG C, obtains the performed polymer of terminal isocyanate group；Ultrasonic disperse 0.5h in DMF is added in the graphite oxide,
Under conditions of nitrogen protection, the performed polymer and catalyst dibutyl tin dilaurate of terminal isocyanate group is added, is warming up to 80
It is stirred to react 1h after DEG C, adds chain extender and accelerating agent trihydroxymethyl propane, 0.01h is quickly stirred at 1200rpm, takes out true
Stirring 0.02h is further continued for after sky, with polytetrafluoroethylene (PTFE) membrane filtration, washing cures 10h in 100 DEG C of drying box, obtains described
Graphite modified polyurethane elastomer；Wherein, graphite powder, polyetherdiol, isocyanates, dibutyl tin dilaurate, three methanol third
The weight proportion of alkane is 1:50:35:10:0.1:2；The polyetherdiol is the tetrahydrofuran polyether that number-average molecular weight is 800
PTMG；The isocyanates is hexamethylene diisocyanate；The chain extender is ethylene glycol；
The polypropylene is made of the copolymerized type propene polymer of 25wt% and the homopolymerization type polypropylene of 75wt%, and described total
The poly- polyacrylic melt index of type is 0.5g/10min；The polyacrylic melt index of homopolymerization type is 5.0g/10min；It is described
It is 3 that crosslinking agent, which is by weight proportion,:1 2,5- dimethyl -2,5- bis(t-butylperoxy)s hexin and polyesters material composition；
The ultra-violet absorber is ultraviolet absorbent uv-326.
Embodiment 2
A kind of motor turning dust cover thermoplastic vulcanizate material, raw material include by weight：EPDM300 parts,
20 parts of polypropylene, 50 parts of linear low density polyethylene, 40 parts of thermoplastic polyurethane elastomer, 15 parts of ethylene-octene copolymer, horse
5 parts of maleic anhydride grafted styrene-ethylene-butadiene-styrene copolymer SEBS-g-MAH, 80 parts of talcum powder are silane coupled
3 parts of agent A-137,10 parts of crosslinking agent, 1 part of active Zinc Oxide, 3 parts of antioxidant 3114,0.5 part of triphenyl phosphite TPP are purple
UV-93 parts of ultraviolet absorbers, 20 parts of naphthenic oil, 6 parts of oleamide；
Wherein, the EPDM be by 60wt% Third monomer be ethenylidene norbornene E types ethylene propylene diene rubber,
The Third monomer of 10wt% is the D types ethylene propylene diene rubber of dicyclopentadiene and the Third monomer of 30wt% is Isosorbide-5-Nitrae-hexadiene
H-type ethylene propylene diene rubber forms；
The thermoplastic polyurethane elastomer is graphite modified polyurethane elastomer, and preparation method includes：By graphite powder
It is 1 that volume ratio, which is added,:In 3 concentrated nitric acid and the mixed acid solution of the concentrated sulfuric acid, 3h is ultrasonically treated at 20 DEG C, then in 80 DEG C of water-baths
In be stirred to react 3h, be cooled to room temperature, filter, be washed with deionized to neutrality, obtain graphite oxide；Polyetherdiol is heated up
It is dehydrated 5h to 90 DEG C and after being evacuated to pressure≤- 0.09Mpa, is cooled to 40 DEG C, isocyanates is added, is warming up to 100 DEG C
After be stirred to react 1h, obtain the performed polymer of terminal isocyanate group；Ultrasonic disperse 1h in DMF is added in the graphite oxide, in nitrogen
Under conditions of gas shielded, the performed polymer and catalyst dibutyl tin dilaurate of terminal isocyanate group is added, after being warming up to 60 DEG C
It is stirred to react 3h, chain extender and accelerating agent trihydroxymethyl propane is added, 0.02h is quickly stirred at 1000rpm, after vacuumizing
It is further continued for stirring 0.01h, with polytetrafluoroethylene (PTFE) membrane filtration, washing cures 5h in 120 DEG C of drying box, obtains the graphite
Modified polyurethane elastomer；Wherein, graphite powder, polyetherdiol, isocyanates, dibutyl tin dilaurate, trihydroxymethyl propane
Weight proportion is 1:70:20:20:0.05:4；The polyetherdiol is (the 2- hydroxyl second of hydroquinone two that number-average molecular weight is 1200
Base) ether HQEE；The isocyanates is 2,4- toluene di-isocyanate(TDI)s；The chain extender is 1,4-butanediol；
The polypropylene is made of the copolymerized type propene polymer of 45wt% and the homopolymerization type polypropylene of 55wt%, and described total
The poly- polyacrylic melt index of type is 10.0g/10min；The polyacrylic melt index of homopolymerization type is 0.5g/10min；It is described
Compatilizer is maleic anhydride graft phenylethene-ethylene-butadiene-styrene copolymer SEBS-g-MAH；The inorganic filler is
Talcum powder；The silane coupling agent is silane coupling A -137；It is 5 that the crosslinking agent, which is by weight proportion,:1 2,5- diformazans
Base -2,5- bis(t-butylperoxy)s hexane and polybutadiene species composition.
Embodiment 3
A kind of motor turning dust cover thermoplastic vulcanizate material, raw material include by weight：EPDM200 parts,
50 parts of polypropylene, 30 parts of linear low density polyethylene, 70 parts of thermoplastic polyurethane elastomer, 10 parts of ethylene-octene copolymer, horse
10 parts of maleic anhydride grafted ethylene propylene diene rubber EPDM-g-MAH, 45 parts of glass microballoon, 4 parts of Silane coupling reagent KH-570, crosslinking
5 parts of agent, 3 parts of active Zinc Oxide, 0.7 part of 2 parts of antioxidant DSTP, dilauryl thiodipropionate DLTP, ultra-violet absorber
2 parts of UV-326,60 parts of hydrocarbon oil, 4 parts of zinc stearate；
Wherein, the EPDM be by 50wt% Third monomer be ethenylidene norbornene E types ethylene propylene diene rubber,
The Third monomer of 10wt% is the D types ethylene propylene diene rubber of dicyclopentadiene and the Third monomer of 40wt% is Isosorbide-5-Nitrae-hexadiene
H-type ethylene propylene diene rubber forms；
The thermoplastic polyurethane elastomer is graphite modified polyurethane elastomer, and preparation method includes：By graphite powder
It is 1 that volume ratio, which is added,:In 2 concentrated nitric acid and the mixed acid solution of the concentrated sulfuric acid, 2h is ultrasonically treated at 30 DEG C, then in 90 DEG C of water-baths
In be stirred to react 2h, be cooled to room temperature, filter, be washed with deionized to neutrality, obtain graphite oxide；Polyetherdiol is heated up
It is dehydrated 4h to 105 DEG C and after being evacuated to pressure≤- 0.09Mpa, is cooled to 50 DEG C, isocyanates is added, is warming up to 90 DEG C
After be stirred to react 2h, obtain the performed polymer of terminal isocyanate group；Ultrasonic disperse 0.7h in DMF is added in the graphite oxide,
Under conditions of nitrogen protection, the performed polymer and catalyst dibutyl tin dilaurate of terminal isocyanate group is added, is warming up to 70 DEG C
After be stirred to react 2h, add chain extender and accelerating agent trihydroxymethyl propane, quickly stir 0.015h at 1100rpm, take out true
Stirring 0.015h is further continued for after sky, with polytetrafluoroethylene (PTFE) membrane filtration, washing cures 7h in 110 DEG C of drying box, obtains described
Graphite modified polyurethane elastomer, wherein graphite powder, polyetherdiol, isocyanates, dibutyl tin dilaurate, trihydroxymethyl propane
Weight proportion be 1:60:25:15:0.07:3；The polyetherdiol is the tetrahydrofuran polyether that number-average molecular weight is 1000
PTMG；The isocyanates is 2,6- toluene di-isocyanate(TDI)s；The chain extender is 1,6- hexylene glycols；
The polypropylene is made of the copolymerized type propene polymer of 35wt% and the homopolymerization type polypropylene of 65wt%, and described total
The poly- polyacrylic melt index of type is 5.0g/10min；The polyacrylic melt index of homopolymerization type is 3.0g/10min；It is described
It is 4 that crosslinking agent, which is by weight proportion,:1 cumyl peroxide and cyanate material composition.
Embodiment 4
A kind of motor turning dust cover thermoplastic vulcanizate material, raw material include by weight：EPDM250 parts,
60 parts of polypropylene, 20 parts of linear low density polyethylene, 80 parts of thermoplastic polyurethane elastomer, 12 parts of ethylene-octene copolymer, phase
Hold 8 parts of agent, 40 parts of inorganic filler, 4 parts of silane coupling agent, 3 parts of crosslinking agent, 2 parts of active Zinc Oxide, 2 parts of primary antioxidant, auxiliary antioxygen
0.8 part of agent, 2 parts of ultra-violet absorber, 50 parts of processing oil, 3 parts of lubricant；
Wherein, the EPDM be by 60wt% Third monomer be ethenylidene norbornene E types ethylene propylene diene rubber,
The Third monomer of 20wt% is the D types ethylene propylene diene rubber of dicyclopentadiene and the Third monomer of 20wt% is Isosorbide-5-Nitrae-hexadiene
H-type ethylene propylene diene rubber forms；
The thermoplastic polyurethane elastomer is graphite modified polyurethane elastomer, and preparation method includes：By graphite powder
It is 1 that volume ratio, which is added,:In 2 concentrated nitric acid and the mixed acid solution of the concentrated sulfuric acid, 1.5h is ultrasonically treated at 25 DEG C, then in 95 DEG C of water
It is stirred to react 2.5h in bath, is cooled to room temperature, filters, is washed with deionized to neutrality, obtains graphite oxide；By polyetherdiol
It is warming up to 100 DEG C and is dehydrated 4.5h after being evacuated to pressure≤- 0.09Mpa, be cooled to 45 DEG C, isocyanates, heating is added
It is stirred to react 1h after to 95 DEG C, obtains the performed polymer of terminal isocyanate group；Ultrasonic disperse in DMF is added in the graphite oxide
The performed polymer and catalyst dibutyl tin dilaurate of terminal isocyanate group is added under conditions of nitrogen protection in 0.8h, heating
It is stirred to react 2h after to 75 DEG C, chain extender and accelerating agent trihydroxymethyl propane is added, is quickly stirred at 1100rpm
0.01h is further continued for stirring 0.02h after vacuumizing, with polytetrafluoroethylene (PTFE) membrane filtration, washing cures in 110 DEG C of drying box
8h obtains the graphite modified polyurethane elastomer；Wherein, graphite powder, polyetherdiol, isocyanates, dibutyl tin cinnamic acid
Tin, trihydroxymethyl propane weight proportion be 1:60:30:10:0.08:3；The polyetherdiol is pair that number-average molecular weight is 1000
Benzenediol two (2- ethoxys) ether HQEE；The isocyanates is 2,4- methyl diphenylene diisocyanates and 4,4- diphenylmethyls
The mixture of alkane diisocyanate；The chain extender is 1,4-butanediol and 1, the mixture of 6- hexylene glycols；
The polypropylene is made of the copolymerized type propene polymer of 30wt% and the homopolymerization type polypropylene of 70wt%, and described total
The poly- polyacrylic melt index of type is 4.0g/10min；The polyacrylic melt index of homopolymerization type is 2.0g/10min；It is described
Compatilizer is maleic anhydride grafted ethene-octene copolymer POE-g-MAH and maleic anhydride is grafted ethylene propylene diene rubber EPDM-g-
The mixture of MAH；The inorganic filler is the mixture of barium sulfate, mica powder and clay；The silane coupling agent is that silane is even
Join the mixture of agent KH-570 and silane coupling A -137；It is 4 that the crosslinking agent, which is by weight proportion,:1 peroxide crosslinking
Agent and assistant crosslinking agent composition, and the peroxide cross-linking agent be 2,5- dimethyl -2,5- bis(t-butylperoxy) hexins and
The mixture of cumyl peroxide, the assistant crosslinking agent are the mixture of isocyanates substance and acrylate substance；
The primary antioxidant is the mixture of antioxidant 1010 and antioxidant DSTP；The auxiliary anti-oxidant be triphenyl phosphite TPP and
The mixture of dilauryl thiodipropionate DLTP；The ultra-violet absorber is ultraviolet absorbent uv-326；The processing
Oil be paraffin oil, naphthenic oil and hydrocarbon oil mixture；The lubricant is the mixture of zinc stearate and calcium stearate.
The preparation method of motor turning dust cover thermoplastic vulcanizate material described in above-described embodiment 1-4, including：It will
EPDM, it polypropylene, linear low density polyethylene, thermoplastic polyurethane elastomer, ethylene-octene copolymer, compatilizer, inorganic fills out
It is equal that mixing in mixer is added in material, silane coupling agent, primary antioxidant, auxiliary anti-oxidant, ultra-violet absorber, processing oil and lubricant
It is even, progress first time plastics in single screw extrusion machine are re-fed into, wherein screw speed is 200-400r/min, is plasticated for the first time
Processing temperature is 160-180 DEG C, and rubber master batch is obtained after pelletizing；The rubber master batch and crosslinking agent, active Zinc Oxide are added
In high mixer, 0.3-0.5h is mixed under the speed conditions of 400-500rpm, transfers to and carries out second in double screw extruder
Secondary to plasticate, wherein screw slenderness ratio is 55-64, and feeding rotating speed is 30-80rpm, screw speed 300-500rpm, second of modeling
The processing temperature of refining is 160-250 DEG C, and tie rod is cooling, and pelletizing obtains the motor turning dust cover thermoplastic vulcanizates
Material；Wherein, the processing temperature plasticated for the second time is specially：One 160-180 DEG C of area's temperature, two 200-210 DEG C of area's temperature,
Three 220-230 DEG C of area's temperature, four 240-250 DEG C of area's temperature, five 240-250 DEG C of area's temperature, six 235-245 DEG C of area's temperature, 7th area
225-235 DEG C of temperature, eight 210-220 DEG C of area's temperature, nine 205-215 DEG C of area's temperature, ten 200-210 DEG C of area's temperature.
Motor turning dust cover described in above-described embodiment 1-4 is tested for the property with thermoplastic vulcanizate material,
As a result as follows：
In the present invention, the thermoplastic vulcanizate material uses the E types ethylene propylene diene rubber of specific proportioning, D type ternarys
The source of EP rubbers and H-type ethylene propylene diene rubber as EPDM makes its tensile strength, bending modulus and cross-linked polymeric degree all
In a rational state, in for motor turning dust cover, excellent durability and machine-shaping property can get；It is poly-
It is strong that the addition of propylene and linear low density polyethylene then not only enables the elastomeric material to obtain required melt forming
Degree, and can further improve the blow processability energy of the material；And due to polypropylene have good solvent resistance,
Heat resistance and processing fluidity can substantially improve the flexibility of elastomeric material itself when being compounded with EPDM, to meet
The performance requirement of motor turning dust cover；The ethylene-octene copolymer and compatilizer being added simultaneously can then significantly improve respectively
Compatibility between major ingredient obtains good comprehensive performance.
In addition, in the present invention, the thermoplastic polyurethane elastomer is modified it using graphite, by by graphite powder
Molecule has entered inside graphite after pickling, and the inside interlamellar spacing of graphite is widened, and interplanar distance increases, and makes after sonicated
It obtains graphite flakes shape structure to be destroyed, to increase the spacing of graphite platelet structure, graphite internal structure is made to become loosely simultaneously
And volume expands, and then forms the groups such as activity hydroxy on surface, then by with the polyurethane with terminal isocyanate group
Prepolymer reaction, and chain extender sealing end is added, a kind of graphite modified polyurethane elastomer is thus obtained, is realized to graphite surface
While activation, graphite platelet structure, thus obtained modification polyurethane elastomer are also introduced on the molecule of polyurethane elastomer
Body can form fine and close, efficient carbon-coating structure on the surface of the vulcanized rubber material, to effectively absorb heat, hinder heat
It is transmitted to elastomeric material internal layer, assigns the material good high temperature resistance；And above-mentioned modified thermoplastic polyurethane bullet
Property body make graphite platelet structure and be evenly dispersed in inside the matrixes such as EPDM with the state removed, the work of skeletal support can be played
With, or solid phase charcoal core is served as, enhance interfacial effect, is conducive to rubber material and obtains the mechanical effects such as excellent intensity.
In addition, the present invention is during preparing the thermoplastic vulcanizate material, using dynamic vulcanization technology, with organic
Peroxide cross-linking system can efficiently control the crosslinking degree of cross-linked material and uniform performance as vulcanizing agent；And make
With the processing technology of plasticating under special parameter so that Blending Processes are more abundant, the rubber phase grain size smaller in blend, distribution
Evenly, the entanglement effect of molecule interchain is smaller, and solution twines relatively easily, is avoided with this because caused by rubber material over cure
Mobility variation effect；It is additionally added a certain amount of antioxidant, lubricant and ultra-violet absorber in the present invention, thus makes system
Standby obtained thermoplastic vulcanizate material has good weather resistance and mechanical property.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (12)
1. a kind of motor turning dust cover thermoplastic vulcanizate material, which is characterized in that its raw material includes by weight：
100-300 parts of EPDM, 20-80 parts of polypropylene, 10-50 parts of linear low density polyethylene, thermoplastic polyurethane elastomer 40-100
Part, 5-15 parts of ethylene-octene copolymer, 5-15 parts of compatilizer, 10-80 parts of inorganic filler, 3-5 parts of silane coupling agent, crosslinking agent
0.2-10 parts, active Zinc Oxide 1-5 parts, 1-3 parts of primary antioxidant, 0.5-1 parts of auxiliary anti-oxidant, 1-3 parts of ultra-violet absorber, processing
It is 20-100 parts oily, 2-6 parts of lubricant；
Wherein, the EPDM be by 40-60wt% Third monomer be ethenylidene norbornene E types ethylene propylene diene rubber,
The Third monomer of 10-30wt% be the D types ethylene propylene diene rubber of dicyclopentadiene and the Third monomer of 20-40wt% be Isosorbide-5-Nitrae-oneself
The H-type ethylene propylene diene rubber of diene forms；
The thermoplastic polyurethane elastomer is graphite modified polyurethane elastomer, and preparation method includes：Graphite powder is added
In the mixed acid solution of concentrated nitric acid and concentrated sulfuric acid composition, water-bath after supersound process filters, and washing obtains graphite oxide；It will
After polyetherdiol dehydration, isocyanates is added, is stirred to react 1-3h after being warming up to 80-100 DEG C, obtains the pre- of terminal isocyanate group
Aggressiveness；Ultrasonic disperse in DMF is added in the graphite oxide, the pre- of terminal isocyanate group is added under conditions of nitrogen protection
Aggressiveness and catalyst dibutyl tin dilaurate are stirred to react 1-3h after being warming up to 60-80 DEG C, chain extender and accelerating agent is added
Trihydroxymethyl propane quickly stirs 0.01-0.02h, and stirring 0.01-0.02h is further continued for after vacuumizing, is filtered, is washed, and curing obtains
To the graphite modified polyurethane elastomer.
2. motor turning dust cover thermoplastic vulcanizate material according to claim 1, which is characterized in that the stone
Black method for preparing modified urethane elastomer includes：It is 1 that volume ratio, which is added, in graphite powder:The concentrated nitric acid of 1-3 and the concentrated sulfuric acid
In mixed acid solution, it is ultrasonically treated 1-3h at 20-40 DEG C, then 1-3h is reacted in 80-100 DEG C of stirred in water bath, is cooled to room
Temperature filters, is washed with deionized to neutrality, obtains graphite oxide；Polyetherdiol is warming up to 90-120 DEG C and is evacuated to
It is dehydrated 3-5h after pressure≤- 0.09Mpa, is cooled to 40-60 DEG C, isocyanates is added, is stirred after being warming up to 80-100 DEG C anti-
1-3h is answered, the performed polymer of terminal isocyanate group is obtained；Ultrasonic disperse 0.5-1h in DMF is added in the graphite oxide, in nitrogen
Under conditions of protection, the performed polymer and catalyst dibutyl tin dilaurate of terminal isocyanate group is added, after being warming up to 60-80 DEG C
It is stirred to react 1-3h, chain extender and accelerating agent trihydroxymethyl propane is added, 0.01- is quickly stirred at 1000-1200rpm
0.02h is further continued for stirring 0.01-0.02h after vacuumizing, with polytetrafluoroethylene (PTFE) membrane filtration, washing, in 100-120 DEG C of drying
5-10h is cured in case, obtains the graphite modified polyurethane elastomer.
3. motor turning dust cover thermoplastic vulcanizate material according to claim 2, which is characterized in that graphite
Powder, polyetherdiol, isocyanates, dibutyl tin dilaurate, trihydroxymethyl propane weight proportion be 1:50-70:20-35:10-
20:0.05-0.1:2-4。
4. motor turning dust cover thermoplastic vulcanizate material according to claim 2, which is characterized in that described poly-
Ether glycol is the tetrahydrofuran polyether PTMG that number-average molecular weight is 800-1200 or hydroquinone two (2- ethoxys) ether HQEE；Institute
It is hexamethylene diisocyanate, 2,4- toluene di-isocyanate(TDI)s, 2,6- toluene di-isocyanate(TDI)s, 2,4- hexichol to state isocyanates
At least one of dicyclohexylmethane diisocyanate, 4,4- methyl diphenylene diisocyanates；The chain extender is ethylene glycol, Isosorbide-5-Nitrae-
At least one of butanediol, 1,6- hexylene glycols.
5. according to claim 1-4 any one of them motor turning dust cover thermoplastic vulcanizate materials, feature exists
In the polypropylene is made of the copolymerized type propene polymer of 25-45wt% and the homopolymerization type polypropylene of 55-75wt%, and described
The melt index of copolymerized type propene polymer is 0.5-10.0g/10min；The polyacrylic melt index of homopolymerization type is 0.5-5.0g/
10min。
6. according to claim 1-4 any one of them motor turning dust cover thermoplastic vulcanizate materials, feature exists
In the compatilizer is maleic anhydride grafted ethene-octene copolymer POE-g-MAH, maleic anhydride graft phenylethene-ethylene-
At least one of butadiene-styrene copolymer SEBS-g-MAH, maleic anhydride grafting ethylene propylene diene rubber EPDM-g-MAH；
The inorganic filler is at least one of wollastonite, talcum powder, glass microballoon, barium sulfate, mica powder, clay；The silane
Coupling agent is at least one of Silane coupling reagent KH-570, silane coupling A -137.
7. according to claim 1-4 any one of them motor turning dust cover thermoplastic vulcanizate materials, feature exists
In it is 3-5 that the crosslinking agent, which is by weight proportion,:1 peroxide cross-linking agent and assistant crosslinking agent composition.
8. motor turning dust cover thermoplastic vulcanizate material according to claim 7, which is characterized in that the mistake
Oxide cross linking agent is 2,5- dimethyl -2,5- bis(t-butylperoxy)s hexin, bis- (the tertiary butyl mistakes of 2,5- dimethyl -2,5-
Oxygroup) hexane, at least one of cumyl peroxide；The assistant crosslinking agent be polyester substance, polybutadiene species,
At least one of cyanate substance, isocyanates substance, acrylate substance.
9. according to claim 1-4 any one of them motor turning dust cover thermoplastic vulcanizate materials, feature exists
In the primary antioxidant is at least one of antioxidant 1010, antioxidant 3114, antioxidant DSTP；The auxiliary anti-oxidant is
At least one of 2-mercaptobenzimidazole MB, triphenyl phosphite TPP, dilauryl thiodipropionate DLTP.
10. according to claim 1-4 any one of them motor turning dust cover thermoplastic vulcanizate materials, feature exists
In the ultra-violet absorber is at least one of ultraviolet absorbent uv-326, ultra-violet absorber UV-9；The processing
Oil is at least one of paraffin oil, naphthenic oil, hydrocarbon oil；The lubricant is ethylene bis stearic acid amide, oleic acid acyl
At least one of amine, zinc stearate, calcium stearate.
11. a kind of system according to claim 1-10 any one of them motor turning dust cover thermoplastic vulcanizate materials
Preparation Method, which is characterized in that including：By EPDM, polypropylene, linear low density polyethylene, thermoplastic polyurethane elastomer, second
Alkene-octene copolymer, compatilizer, inorganic filler, silane coupling agent, primary antioxidant, auxiliary anti-oxidant, ultra-violet absorber, processing
Mixing is uniform in oil and lubricant addition mixer, is re-fed into single screw extrusion machine and plasticate for the first time, wherein screw rod turns
Speed is 200-400r/min, and the processing temperature plasticated for the first time is 160-180 DEG C, and rubber master batch is obtained after pelletizing；By the rubber
Glue master batch and crosslinking agent, active Zinc Oxide are added in high mixer, and 0.3-0.5h is mixed under the speed conditions of 400-500rpm, then
It is transferred in double screw extruder and is plasticated for the second time, wherein screw slenderness ratio is 55-64, and feeding rotating speed is 30-80rpm,
Screw speed is 300-500rpm, and the processing temperature plasticated for the second time is 160-250 DEG C, and tie rod is cooling, pelletizing, is obtained described
Motor turning dust cover thermoplastic vulcanizate material.
12. the preparation method of motor turning dust cover thermoplastic vulcanizate material according to claim 11, described
The processing temperature plasticated for the second time is specially：One 160-180 DEG C of area's temperature, two 200-210 DEG C of area's temperature, three area temperature 220-
230 DEG C, four 240-250 DEG C of area's temperature, five 240-250 DEG C of area's temperature, six 235-245 DEG C of area's temperature, seven area temperature 225-235
DEG C, eight 210-220 DEG C of area's temperature, nine 205-215 DEG C of area's temperature, ten 200-210 DEG C of area's temperature.
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