CN112266614B - Polyphenylene sulfide composite material, preparation method thereof and injection molding part - Google Patents
Polyphenylene sulfide composite material, preparation method thereof and injection molding part Download PDFInfo
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 81
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 238000001746 injection moulding Methods 0.000 title abstract description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 46
- 239000004917 carbon fiber Substances 0.000 claims abstract description 46
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000945 filler Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- 239000000314 lubricant Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 239000010445 mica Substances 0.000 claims description 9
- 229910052618 mica group Inorganic materials 0.000 claims description 9
- -1 compatilizer Substances 0.000 claims description 6
- 229920001897 terpolymer Polymers 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 3
- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002530 phenolic antioxidant Substances 0.000 claims description 2
- AQRLNPVMDITEJU-UHFFFAOYSA-N triethylsilane Chemical compound CC[SiH](CC)CC AQRLNPVMDITEJU-UHFFFAOYSA-N 0.000 claims 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 238000012545 processing Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 5
- 239000002048 multi walled nanotube Substances 0.000 description 5
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- WBWXVCMXGYSMQA-UHFFFAOYSA-N 3,9-bis[2,4-bis(2-phenylpropan-2-yl)phenoxy]-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound C=1C=C(OP2OCC3(CO2)COP(OC=2C(=CC(=CC=2)C(C)(C)C=2C=CC=CC=2)C(C)(C)C=2C=CC=CC=2)OC3)C(C(C)(C)C=2C=CC=CC=2)=CC=1C(C)(C)C1=CC=CC=C1 WBWXVCMXGYSMQA-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002633 Kraton (polymer) Polymers 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- CNJPFZOQZWIGIB-UHFFFAOYSA-N ethene;methyl prop-2-enoate;oxiran-2-ylmethyl 2-methylprop-2-enoate Chemical compound C=C.COC(=O)C=C.CC(=C)C(=O)OCC1CO1 CNJPFZOQZWIGIB-UHFFFAOYSA-N 0.000 description 1
- 229920006258 high performance thermoplastic Polymers 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/02—Polythioethers; Polythioether-ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a polyphenylene sulfide composite material, a preparation method thereof and an injection molding part. The polyphenylene sulfide composite material comprises the following raw material components in percentage by weight: 42.5 to 90 percent of polyphenylene sulfide resin, 0.1 to 20 percent of nano layered silicate filler, 5 to 50 percent of carbon fiber, 0.5 to 5 percent of compatilizer, 0.1 to 0.8 percent of coupling agent, 0.1 to 2 percent of lubricant and 0.1 to 1 percent of antioxidant, and the polyphenylene sulfide resin material with good mechanical property and toughness is obtained through the synergistic effect of all the components, and can be applied to the manufacture of injection molded parts in the fields of machinery, automobiles, electronic appliances, aviation and the like which require high strength and high mechanical property.
Description
Technical Field
The invention relates to the field of polymer composite materials, in particular to a polyphenylene sulfide composite material, a preparation method thereof and an injection molding part.
Background
Polyphenylene Sulfide (PPS) is a high-performance thermoplastic polymer, is mainly applied to the preparation of special engineering plastics and precision parts, and is used in the fields of electronics and electricity, automobile industry, aviation, chemical and mechanical industries and the like. Polyphenylene sulfide has good flame retardancy, insulation and chemical resistance due to a rigid molecular chain formed by alternately arranging benzene rings and sulfur atoms, but also has the defects of low ductility, poor toughness and the like. The mechanical strength and toughness of non-reinforced PPS cannot meet the mechanical performance requirements in most applications.
Research relates to the method that boron phenolic resin is used as sizing agent to perform impregnation modification on carbon fiber, so that the interface bonding strength between the carbon fiber and PPS is effectively improved, and the carbon fiber/polyphenylene sulfide composite material with excellent tensile property is prepared. However, the carbon fiber reinforced polyphenylene sulfide composite material has undesirable properties under the condition of high concentration of the sizing agent due to poor interface bonding between the carbon fiber and the matrix resin.
In other researches, a carbon fiber reinforced polyphenylene sulfide composite material is prepared by taking a polyphenylene sulfide non-woven fabric as a raw material and utilizing a carbon fiber reinforced polyphenylene sulfide composite material through a hot pressing method, so that the tensile strength, the bending strength and the impact strength of the carbon fiber reinforced polyphenylene sulfide composite material are greatly improved, but the size and the application of the polyphenylene sulfide composite material are limited due to the preparation method.
Disclosure of Invention
Based on the above, in order to satisfy the application of the polyphenylene sulfide composite material in multiple sizes and multiple fields, it is necessary to provide a polyphenylene sulfide composite material which is suitable for extrusion processing and has good mechanical properties and toughness.
The specific technical scheme is as follows:
the polyphenylene sulfide composite material comprises the following raw material components in percentage by weight:
in one embodiment, the polyphenylene sulfide composite material comprises the following raw material components in percentage by weight:
in one embodiment, the melt flow rate of the polyphenylene sulfide resin at 316 ℃ and 5kg is 200 g-600 g/10min.
In one embodiment, the carbon fibers are polyacrylonitrile-based chopped carbon fibers, the diameter of the carbon fibers is 5-15 μm, and the length of the carbon fibers is 3-7 mm.
In one embodiment, the nano layered silicate filler is nano mica with an average diameter/thickness ratio of 20 to 80.
In one embodiment, the compatibilizer is an ethylene-methyl acrylate-glycidyl methacrylate terpolymer.
In one embodiment, the coupling agent is selected from at least one of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-mercaptopropyltriethylsilane, and 3-mercaptopropyltrimethoxysilane.
In one of the embodiments, the lubricant is selected from at least one of silicone and pentaerythritol stearate.
In one embodiment, the antioxidant is selected from at least one of hindered phenolic antioxidants and phosphorous antioxidants.
The invention also provides a preparation method of the polyphenylene sulfide composite material, which comprises the following steps: mixing polyphenylene sulfide, nano layered silicate filler, compatilizer, coupling agent, antioxidant, lubricant and carbon fiber, and melting and extruding.
The invention also provides an injection molded part which contains the polyphenylene sulfide composite material.
According to the invention, the nano-layered silicate filler and the carbon fiber are compounded, the modified polyphenylene sulfide is enhanced, the compatilizer and other additives are added, and the dispersion of the carbon fiber is improved through the synergistic effect of the nano-filler and the carbon fiber, so that the mechanical property of the composite material is improved, and the composite material has better toughness, and can be applied to the manufacturing of injection molded parts in the fields of machinery, automobiles, electronic appliances, aviation and the like which require high strength and high mechanical property.
Detailed Description
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a polyphenylene sulfide composite material which comprises the following raw material components in percentage by weight:
preferably, the polyphenylene sulfide composite material comprises the following raw material components in percentage by weight:
in a specific example, the polyphenylene sulfide resin has a melt flow rate of 200g to 600g/10min at 316 ℃ and 5 kg.
In one particular example, the carbon fibers are polyacrylonitrile-based chopped carbon fibers, optionally having a diameter of 5 to 15 μm and a length of 3 to 7mm.
Although the carbon fiber has higher specific modulus and higher heat conductivity, the carbon fiber is difficult to generate effective interface combination with PPS due to smooth surface, large chemical inertia and low surface energy, and the polyacrylonitrile can improve the chemical bonding effect between the carbon fiber and a PPS matrix and the wettability between the carbon fiber and polyphenylene sulfide resin after the surface treatment of the carbon fiber, thereby improving the interface bonding performance of the composite material and being beneficial to improving the overall performance of the polyphenylene sulfide resin composite material.
In one particular example, the nano-layered silicate filler is nano-mica with an average diameter/thickness ratio of 20 to 80.
The nano mica has a layered structure, so that the specific surface area is large, the surface adsorption capacity is strong, and the nano mica is combined with dispersed carbon fibers, so that the strength retention rate of the polyphenylene sulfide resin composite material is favorably improved.
In one particular example, the compatibilizer is an ethylene-methyl acrylate-glycidyl methacrylate terpolymer.
In one specific example, the coupling agent is at least one of gamma- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560), gamma-mercaptopropyltriethylsilane (KH-580), and 3-mercaptopropyltrimethoxysilane (KH-590).
In one particular example, the lubricant is selected from at least one of silicone and pentaerythritol stearate.
In a specific example, the antioxidant is selected from at least one of hindered phenol-based antioxidants and phosphorus-based antioxidants.
The invention provides a preparation method of a polyphenylene sulfide composite material, which comprises the following specific steps:
mixing polyphenylene sulfide, nano layered silicate filler, compatilizer, coupling agent, antioxidant, lubricant and carbon fiber, and melting and extruding.
In a specific example, the polyphenylene sulfide, the nano layered silicate filler, the compatilizer, the coupling agent, the antioxidant, the lubricant and the carbon fiber are uniformly stirred, and the polyphenylene sulfide composite material is obtained through melt extrusion, cooling, drying and grain cutting.
In a specific example, the polyphenylene sulfide, the nano layered silicate filler, the compatilizer, the coupling agent, the antioxidant and the lubricant are uniformly stirred, added into a main feed inlet of a double-screw extruder, the carbon fiber is added through a side feeding device for processing, the processing temperature is 250-300 ℃, and the polyphenylene sulfide composite material is obtained after the extrusion, the cooling, the drying and the grain cutting.
Specifically, the processing temperature zones are set as follows: the temperature of the first zone is 260-280 ℃, the temperature of the second zone is 280-295 ℃, the temperature of the third zone is 280-295 ℃, the temperature of the fourth zone is 280-295 ℃, the temperature of the fifth zone is 280-295 ℃, the temperature of the sixth zone is 270-285 ℃, the temperature of the seventh zone is 270-285 ℃, the temperature of the eighth zone is 270-285 ℃ and the temperature of the ninth zone is 280-295 ℃.
In one specific example, the extruder main engine rotates at 240-400 rpm, and the output is 100kg/h.
The crystallization performance of the polyphenylene sulfide resin is improved through the synergistic effect of the added carbon fibers and the nano mica, and the interface cohesiveness and compatibility among the components of the composite material are further improved by combining the compatilizer, the coupling agent, the antioxidant and the lubricant, so that the polyphenylene sulfide material with good mechanical property and toughness is finally obtained.
The polyphenylene sulfide composite material and the method for preparing the same according to the present invention will be described in further detail with reference to the following specific examples.
The melt flow rate of polyphenylene sulfide used below at 316 ℃ under 5kg is 200g to 600g/10min, produced by Mr. Kyoho, zhuhai, under the designation CXP300; the polyacrylonitrile-based chopped Carbon fiber is produced by SGL Carbon company in Germany, and has the mark number of SIGRAFIL C30S003PUT; the nano mica is produced by Cisco mica of Lingshu county; compatibilizer 1 ethylene methyl acrylate glycidyl methacrylate terpolymer manufactured by arkema under the designation AX8900, compatibilizer 2 maleic anhydride grafted styrene-ethylene-butadiene-styrene block copolymer manufactured by kraton, usa under the designation FG1901; the multi-walled carbon nanotubes are produced by Shenzhen nanometer Port Limited; the coupling agent is KH-580 manufactured by Chenguang corporation; the lubricant is PETS produced by Lonza company in the United states; the antioxidant 1010 was prepared by mixing the antioxidant 1010 and S9228 as described in 1, wherein the antioxidant 1010 was manufactured by Dover, USA under the trade name IRGANOX 1010 under the chemical name of tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester, and the antioxidant S9228 was manufactured by Dover, USA under the trade name Doverpho S-9228 under the chemical name of bis (2, 4-dicumylphenyl) pentaerythritol diphosphite.
Example 1
The embodiment provides a polyphenylene sulfide composite material, which comprises the following raw material components in percentage by weight:
the preparation method of the polyphenylene sulfide composite material comprises the following steps:
stirring polyphenylene sulfide, nano layered silicate filler, compatilizer, coupling agent, lubricant and antioxidant in a high-speed mixer for 3 minutes, adding the mixture into a double-screw extruder, adding carbon fiber through a side feeding device, and processing the double-screw extruder as follows: the temperature of the first zone is 270 ℃, the temperature of the second zone is 285 ℃, the temperature of the third zone is 290 ℃, the temperature of the fourth zone is 290 ℃, the temperature of the fifth zone is 290 ℃, the temperature of the sixth zone is 280 ℃, the temperature of the seventh zone is 275 ℃, the temperature of the eighth zone is 275 ℃, the temperature of the ninth zone is 275 ℃, the rotating speed of the main engine is 300 revolutions per minute, and the yield is 100kg/h. And cooling, drying and dicing after extrusion to obtain the polyphenylene sulfide composite material.
Example 2
The embodiment provides a polyphenylene sulfide composite material, which comprises the following raw material components in percentage by weight:
in this example, the preparation method of the polyphenylene sulfide composite material was the same as that of example 1.
Example 3
The embodiment provides a polyphenylene sulfide composite material, which comprises the following raw material components in percentage by weight:
in this example, the preparation method of the polyphenylene sulfide composite material was the same as that of example 1.
Example 4
The embodiment provides a polyphenylene sulfide composite material, which comprises the following raw material components in percentage by weight:
in this example, the preparation method of the polyphenylene sulfide composite material was the same as that of example 1.
Example 5
The embodiment provides a polyphenylene sulfide composite material, which comprises the following raw material components in percentage by weight:
in this example, the preparation method of the polyphenylene sulfide composite material was the same as that of example 1.
Example 6
The embodiment provides a polyphenylene sulfide composite material, which comprises the following raw material components in percentage by weight:
in this example, the preparation method of the polyphenylene sulfide composite material was the same as that of example 1.
Comparative example 1
The polyphenylene sulfide composite material does not contain nano layered silicate filler in the raw materials of the comparative example 1, and comprises the following raw material components in percentage by weight:
in this comparative example, the polyphenylene sulfide composite was prepared in the same manner as in example 1.
Comparative example 2
The raw material of comparative example 2 is multi-walled carbon nanotubes instead of Carbon Fibers (CF), and the polyphenylene sulfide composite material comprises the following raw material components in percentage by weight:
in this comparative example, the polyphenylene sulfide composite was prepared in the same manner as in example 1.
Comparative example 3
The raw materials of the comparative example 3 change the type of the compatilizer, and the polyphenylene sulfide composite material comprises the following raw material components in percentage by weight:
in this comparative example, the polyphenylene sulfide composite was prepared in the same manner as in example 1.
Performance detection method and result analysis:
tensile Strength test was conducted according to ASTM-D638, specimen type I, specimen size (mm): (165. + -.2) × (12.70. + -. 0.2) × (3.20. + -. 0.2), and the drawing speed was 50mm/min.
Flexural strength and flexural modulus were examined according to ASTM-D790, specimen size (mm): (127. + -. 2) × (12.7. + -. 0.2) × (3.20. + -. 0.2), and the bending speed was 13mm/min.
Notched impact strength was tested according to ASTM-D256, and the specimen type was V notch type, specimen size (mm): 63.5 × (12.7 ± 0.2) × (3.2 ± 0.2); the notch type is V-notch type, and the residual thickness of the notch is 10.16mm.
The raw materials and the corresponding weight percentages of the examples and the comparative examples are shown in table 1, and the performance test results of the examples and the comparative examples are shown in table 2:
TABLE 1
TABLE 2
In the polyphenylene sulfide composite materials of examples 1 to 4, the carbon fibers significantly enhanced the tensile strength and flexural strength of the polyphenylene sulfide composite materials, but too much carbon fibers resulted in a decrease in impact strength. On the basis of a certain carbon fiber content, the tensile strength, the bending strength and the impact strength of the composite material are improved along with the addition of the nano layered silicate filler in a certain range. In example 6, when the content of the nano mica is 10%, the impact strength is reduced, which is probably because the layered nano filler and the carbon fiber are dispersed together in the resin matrix, and the multi-carbon fiber of the layered nano filler plays a certain separation role, so that the carbon fiber can be better dispersed, and the carbon fiber is prevented from agglomerating to play a role in reinforcing the carbon fiber; meanwhile, the small-size nano lamellar filler plays a role in heterogeneous nucleation on the polyphenylene sulfide, and is beneficial to improving the crystallization speed and the crystallinity of the polyphenylene sulfide, so that the polyphenylene sulfide has better mechanical property and toughness. However, when the content of the nano filler is too high, the nano filler is easy to agglomerate, and the mechanical property of the composite material is reduced. The ethylene-methyl acrylate-glycidyl methacrylate terpolymer serving as the compatilizer is favorable for improving the interface strength of the composite material, so that the composite material has higher mechanical property and toughness, and the maleic anhydride grafted styrene-ethylene-butadiene-styrene block copolymer serving as the compatilizer can play a role in interface compatibilization and increase the toughness, but the mechanical property and the modulus are greatly reduced, so that the ethylene-methyl acrylate-glycidyl methacrylate terpolymer serving as the compatilizer is more favorable for improving the compatibility among the interfaces of the composite material. The mechanical properties of the composite material are remarkably improved by adding 10% of chopped carbon fibers in example 1, while the mechanical strength of the multi-walled carbon nanotube reinforced composite material in the same amount in comparative example 2 is lower, probably because the multi-walled carbon nanotubes have a diameter less than 100nm, but the multi-walled carbon nanotubes are difficult to achieve an ideal dispersion degree in the extrusion processing process, so that the reinforcing effect is limited. The invention produces excellent reinforcing effect on the mechanical property and toughness of the polyphenylene sulfide composite material by the synergistic effect of the carbon fiber, the layered silicate filler, the compatilizer and other auxiliaries.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. The polyphenylene sulfide composite material is characterized by comprising the following raw material components in percentage by weight:
wherein the nano layered silicate filler is nano mica, and the average value of the diameter/thickness ratio is 20-80;
the compatilizer is ethylene-methyl acrylate-glycidyl methacrylate terpolymer;
the coupling agent is at least one selected from gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-mercaptopropyl triethyl silane and 3-mercaptopropyl trimethoxy silane.
2. The polyphenylene sulfide composite material according to claim 1, wherein the polyphenylene sulfide resin has a melt flow rate of 200g to 600g/10min at 316 ℃ and 5 kg.
3. The polyphenylene sulfide composite material according to claim 1, wherein the carbon fibers are polyacrylonitrile-based chopped carbon fibers, have a diameter of 5 μm to 15 μm and a length of 3mm to 7mm.
4. The polyphenylene sulfide composite of claim 1, wherein the lubricant is selected from at least one of silicone and pentaerythritol stearate.
5. The polyphenylene sulfide composite of claim 1, wherein the antioxidant is selected from at least one of hindered phenolic antioxidants and phosphorous antioxidants.
6. The method for preparing the polyphenylene sulfide composite material according to any one of claims 1 to 5, comprising the steps of: mixing polyphenylene sulfide, nano layered silicate filler, compatilizer, coupling agent, antioxidant, lubricant and carbon fiber, and melting and extruding.
7. An injection molded article comprising the polyphenylene sulfide composite material according to any one of claims 1 to 5.
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| CN102746668A (en) * | 2012-06-27 | 2012-10-24 | 深圳市科聚新材料有限公司 | Carbon fiber-reinforced polyphenylene sulfide material and preparation method thereof |
| CN103772987A (en) * | 2012-10-17 | 2014-05-07 | 合肥杰事杰新材料股份有限公司 | High-strength low-warping modified polyphenylene sulfide material and preparation method thereof |
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| CN105860525A (en) * | 2016-06-07 | 2016-08-17 | 安徽新华学院 | Low-smell polyphenylene sulfide composite and preparation method thereof |
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