CN102888111A - Preparing method of polyphenylene sulfide ceramic alloy - Google Patents
Preparing method of polyphenylene sulfide ceramic alloy Download PDFInfo
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- CN102888111A CN102888111A CN2011101998505A CN201110199850A CN102888111A CN 102888111 A CN102888111 A CN 102888111A CN 2011101998505 A CN2011101998505 A CN 2011101998505A CN 201110199850 A CN201110199850 A CN 201110199850A CN 102888111 A CN102888111 A CN 102888111A
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- polyphenylene sulfide
- oxidation
- screw extruder
- glass fibre
- polymethylmethacrylate
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 82
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910002110 ceramic alloy Inorganic materials 0.000 title abstract 2
- 239000002131 composite material Substances 0.000 claims abstract description 31
- -1 poly(methyl methacrylate) Polymers 0.000 claims abstract description 31
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 21
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000008187 granular material Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000012756 surface treatment agent Substances 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 5
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims description 28
- 238000007254 oxidation reaction Methods 0.000 claims description 28
- 239000011347 resin Substances 0.000 claims description 24
- 229920005989 resin Polymers 0.000 claims description 24
- 239000003365 glass fiber Substances 0.000 claims description 17
- NWODFYYWMUKPPE-UHFFFAOYSA-N C(C(=C)C)(=O)OC(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.P(O)(O)O Chemical compound C(C(=C)C)(=O)OC(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.P(O)(O)O NWODFYYWMUKPPE-UHFFFAOYSA-N 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 12
- 239000000835 fiber Substances 0.000 claims description 12
- 238000005453 pelletization Methods 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 10
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 3
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 abstract description 12
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 229920001971 elastomer Polymers 0.000 abstract description 6
- 239000000806 elastomer Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 238000004925 denaturation Methods 0.000 abstract description 4
- 230000036425 denaturation Effects 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 4
- 239000011152 fibreglass Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 235000006708 antioxidants Nutrition 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 239000003208 petroleum Substances 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 15
- 239000002253 acid Substances 0.000 description 14
- 239000011159 matrix material Substances 0.000 description 14
- 229920006389 polyphenyl polymer Polymers 0.000 description 13
- 150000003568 thioethers Chemical class 0.000 description 13
- 150000001875 compounds Chemical class 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 238000012856 packing Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
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- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
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- 239000000463 material Substances 0.000 description 5
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- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 239000012764 mineral filler Substances 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- JRSJRHKJPOJTMS-MDZDMXLPSA-N trimethoxy-[(e)-2-phenylethenyl]silane Chemical compound CO[Si](OC)(OC)\C=C\C1=CC=CC=C1 JRSJRHKJPOJTMS-MDZDMXLPSA-N 0.000 description 3
- QHMVQKOXILNZQR-UHFFFAOYSA-N 1-methoxyprop-1-ene Chemical group COC=CC QHMVQKOXILNZQR-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- NHFDKKSSQWCEES-UHFFFAOYSA-N dihydrogen phosphate;tris(2-hydroxyethyl)azanium Chemical compound OP(O)(O)=O.OCCN(CCO)CCO NHFDKKSSQWCEES-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical class CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009533 lab test Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- UUIPAJHTKDSSOK-UHFFFAOYSA-N (2-nonylphenyl) dihydrogen phosphate Chemical compound CCCCCCCCCC1=CC=CC=C1OP(O)(O)=O UUIPAJHTKDSSOK-UHFFFAOYSA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 1
- XWUCFAJNVTZRLE-UHFFFAOYSA-N 7-thiabicyclo[2.2.1]hepta-1,3,5-triene Chemical compound C1=C(S2)C=CC2=C1 XWUCFAJNVTZRLE-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 208000000848 Autosomal recessive primary microcephaly Diseases 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 235000019241 carbon black Nutrition 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 231100001010 corrosive Toxicity 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002169 ethanolamines Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229960001708 magnesium carbonate Drugs 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 230000026731 phosphorylation Effects 0.000 description 1
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- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 201000001729 primary autosomal recessive microcephaly Diseases 0.000 description 1
- AMCPECLBZPXAPB-UHFFFAOYSA-N propane-1,2,3-triol;sodium Chemical compound [Na].OCC(O)CO AMCPECLBZPXAPB-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
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- 229910052623 talc Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
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- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a preparing method of polyphenylene sulfide ceramic alloy The method comprises adding an anti-oxidant, elastomer powder of poly(methyl methacrylate), alumina ceramic powder with nanoscale of 95% and other fillers into the crosslinked polyphenylene sulfide, fully and uniformly mixing in a high-speed mixer to obtain a premix of the polyphenylene sulfide, inputting the premix of the polyphenylene sulfide and the fiberglass treated by a surface treatment agent of beta-(3,4-epoxy cyclohexyl)ethyltrimethoxysilane into a double-screw extruder for mixing, extruding and molding, and then cooling and cutting to form the finished composite granulates. The composite granulates obtained by the method has advantages of high thermal denaturation stability and tensile strength, and low metal corrosion, and can be widely applied in the fields of electronic appliances, machinery, chemical industry, petroleum, military industry, and aerospace.
Description
Affiliated technical field
The invention belongs to speciality polymer material Application Areas
Background technology
Polyphenylene sulfide (PPS) good heat stability, has outstanding high thermal resistance, fusing point reaches 285 ℃, other special engineering plastics that are higher than present suitability for industrialized production, the PPS composite granule has good injection processing characteristics, can be processed into the PPS composite product of all size, different shape.But in the more harsh field of some application conditions, explore and find that the more good PPS matrix material of performance is still the target that people pursue.
Introduced among the Chinese patent CN:1667044A and a kind ofly added aromatic phosphoric ester and polyphenylene oxides is the manufacture method of the polyphenyl thioether composite material of resin, its objective is at injection molding SHI and improve the heat-resistant stability of matrix material and the surface smoothness of shaped material.But the dispersion effect of aromatic phosphoric ester in polyphenylene sulfide is undesirable, easily forms the parcel phenomenon when producing under the general technology level, thereby directly have influence on high-temperature mechanical property in pellet.
Introduced among the Chinese patent CN:1253149A and a kind ofly added epoxy silane compounds and high component is inorganic, the manufacture method of the polyphenylene sulfide of organic fibre (PPS) matrix material, its objective is and want to reduce this matrix material at the overlap of injection molded.Thereby provide a kind of have good processing characteristics, the polyphenyl thioether composite material of physical strength, although the overlap behind the packing materials such as adding epoxy silane compounds when being injected into part reduces, and has but reduced resistance to impact shock and the tensile strength of polyphenyl thioether composite material.
Introduced the manufacture method that employing zinc oxide palpus crystalline substance and glass fibre or carbon fiber and polyphenylene sulfide (PPS) resin carry out polyphenylene sulfide (PPS) matrix material of blending and modifying among the Chinese patent CN:1272124A, its objective is that adopting zinc oxide is that corrosion inhibitor improves corrosion of metal, can eliminate the detrimentally affect of mechanical-physical character; But after adding zinc oxide, tensile strength and the elongation at break of the polyphenylene sulfide of making (PPS) matrix material injection forming decrease, and its resistance to impact shock also decreases.
Introduced a kind of production method that adds the polyphenylene sulfide ceramal of thermo-stabilizer and mineral filler in Chinese patent application number NO:200710049503.8, this patent is to adopt very common method poly-p-phenylene sulfide ether resin to carry out modification to strengthen in fact.
In view of the above shortcoming of prior art, the objective of the invention is to study a kind ofly produce shock-resistant, high stabile against thermal denaturation, tensile strength is good and the polyphenylene sulfide ceramal matrix material that contains glass fibre low to metallic corrosion, good processability.
Summary of the invention:
Its main technique comprises:
A kind of manufacture method of polyphenylene sulfide ceramal, polyphenylene sulfide Preblend behind adding oxidation inhibitor, the ceramic powder is fully mixed in homogenizer, be shaped, form composite granule through cooling, pelletizing with glass fibre input parallel dual-screw extruding machine mixing extrusion again, it is characterized in that, adopt following processing step:
1), be 3-5 ten thousand with weight-average molecular weight, melt flow index is that 300-600g/10min and molecular weight distribution are the linear polyphenylene sulfide resin of 2.5-3.0, adds the crosslinked 2-3h of the heat of oxidation in the crosslinked device of the heat of oxidation;
2), will be 1) in homogenizer, fully mix after adding the weighting agents such as antioxidant, polymethylmethacrylate elastomerics in the polyphenylene sulfide cross-linked resin that obtains, the weight ratio of used antioxidant phosphorous acid triphenylmethyl methacrylate in the ninth of the ten Heavenly Stems and polyphenylene sulfide is 3-3.5: 100; The weight ratio of polymethylmethacrylate elastomerics and polyphenylene sulfide is 3-5: 100, and granularity is that the nano level 95% alumina-ceramic powder of 5-10nm and the weight ratio of polyphenylene sulfide are 30-40: 100 obtain polyphenylene sulfide Preblend with this;
3), with (2) gained polyphenylene sulfide Preblend 60-70%wt again with through β-(3, the 4-epoxycyclohexyl) the 40-30%wt diameter was the glass fibre input twin screw extruder of 20-30um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, and formed the finished product composite granule through the shaping of twin screw extruder mixing extrusion, cooling, pelletizing.
4), in polyphenylene sulfide Preblend manufacturing processed, need to add the polymethylmethacrylate elastomerics, the overlap length of moulding is 0.3-0.5um, improve simultaneously the toughness of 30-40% polyphenyl thioether composite material, and the melt strength of polyphenyl thioether composite material improves 15-20%.
Melt strength refers to that polymkeric substance supports the ability of sole mass under molten state. macromolecule melt intensity (Melt Strength), sometimes be also referred to as melt elasticity (Melt Elasticity), approximately measuring polymer melting elongational viscosity (Elongational Viscosity) on the engineering, itself and molecular weight of polymers (MW), molecular weight distribution (MWD), branch chain (Branching) what/length etc. is relevant.Be exactly the degree of entanglement (Degree of Polymer Chain Entanglement at MelT) that depends under the polymer molten state in fact in the final analysis, degree of entanglement is high, and melt strength is just high.So can improve macromolecule melt intensity by branch chain or crosslinked (Cross-linking).
In general, the product that melt strength is high relatively is fit to extrude, and the product that melt strength is low relatively is fit to injection moulding; It is rightabout that melt strength and molten finger numerically are into, that is to say that melt strength is higher, and molten finger is lower.But whether be fit to extrude or injection moulding less than obviously distinguishing, relevant with processing condition.Also have, the melt strength of injection moulding is embodied under the high-shear, therefore still should be noted that here.Melt strength is not only relevant with molecular weight, and the quantity of the side chain in the molecule and length relation are very large.
In the manufacture method of the polyphenylene sulfide alloy that contains the porcelain powder of the present invention, the melt strength of matrix material is not measure under the condition that strengthens with fortifying fibre.
The composite granule that adopts as above method to make has high stabile against thermal denaturation and tensile strength, and is low to the metallic corrosion rate.Can be widely used in electronic apparatus, machinery, chemical industry, oil, military project, field of aerospace.
Adding the elastomeric purpose of polymethylmethacrylate in the process of the present invention is the burr (overlap) that reduces on the one hand moulding, improve on the other hand the melt strength of matrix material in injection moulding process, the 3rd, reduce the degree of crystallinity of matrix material and the crystallization velocity of raising matrix material, can reduce so the various losses of matrix material in injection moulding process, improve the yield rate of moulding.
In homogenizer, stir 2-3h after adding polyphenylene sulfide cross-linked resin, oxidation inhibitor, polymethylmethacrylate elastomerics, ceramics powder, make it be mixed into homogeneous polyphenylene sulfide mixture, then with process β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 20-30um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, form the finished product composite granule through the shaping of twin screw extruder mixing extrusion, cooling, pelletizing, pack at last, put in storage, use.
The inventive method gained composite granule has high stabile against thermal denaturation and tensile strength, and is low to the metallic corrosion rate.Can be widely used in electronic apparatus, machinery, chemical industry, oil, military project, field of aerospace.
Description of drawings:
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the product performance table that embodiment of the invention experiment obtains.
Embodiment
Embodiment 1
Be 30,000 with weight-average molecular weight, melt flow index is that 600g/10min and molecular weight distribution are 3.0 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 3h of the heat of oxidation stand-by
In homogenizer, add 64%wt polyphenylene sulfide cross-linked resin, 3%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, 3%wt polymethylmethacrylate elastomerics, the 30%wt granularity is to stir 3h behind the nano level 95% alumina-ceramic powder of 5nm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 60%wt polyphenylene sulfide and 40%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 30um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
Embodiment 2
Be 50,000 with weight-average molecular weight, melt flow index is that 300g/10min and molecular weight distribution are 2.5 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 2h of the heat of oxidation stand-by
In homogenizer, add 51.5%wt polyphenylene sulfide cross-linked resin, 3.5%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, 5%wt polymethylmethacrylate elastomerics, the 40%wt granularity is to stir 2h behind the nano level 95% alumina-ceramic powder of 10hm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 70%wt polyphenylene sulfide and 30%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 20um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
The comparative example 1
Be 40,000 with weight-average molecular weight, melt flow index is that 430g/10min and molecular weight distribution are 2.8 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 3h of the heat of oxidation stand-by
In homogenizer, add 60%wt polyphenylene sulfide cross-linked resin, 3%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, the 37%wt granularity is to stir 3h behind the nano level 95% alumina-ceramic powder of 5nm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 70%wt polyphenylene sulfide and 30%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 30um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
Embodiment 3
Be 40,000 with weight-average molecular weight, melt flow index is that 451g/10min and molecular weight distribution are 2.7 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 3h of the heat of oxidation stand-by
In homogenizer, add 56%wt polyphenylene sulfide cross-linked resin, 3.3%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, 3.7%wt polymethylmethacrylate elastomerics, the 37%wt granularity is to stir 2.5h behind the nano level 95% alumina-ceramic powder of 6nm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 65%wt polyphenylene sulfide and 35%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 25um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
Embodiment 4
Be 4.5 ten thousand with weight-average molecular weight, melt flow index is that 360g/10min and molecular weight distribution are 2.5 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 2.8h of the heat of oxidation stand-by
In homogenizer, add 60%wt polyphenylene sulfide cross-linked resin, 3.4%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, 4.6%wt polymethylmethacrylate elastomerics, the 32%wt granularity is to stir 3h behind the nano level 95% alumina-ceramic powder of 7nm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 64%wt polyphenylene sulfide and 36%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 26um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
Embodiment 5
Be 3.8 ten thousand with weight-average molecular weight, melt flow index is that 420g/10min and molecular weight distribution are 2.9 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 3h of the heat of oxidation stand-by
In homogenizer, add 58%wt polyphenylene sulfide cross-linked resin, 3.5%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, 4.5%wt polymethylmethacrylate elastomerics, the 34%wt granularity is to stir 2.6h behind the nano level 95% alumina-ceramic powder of 8nm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 63%wt polyphenylene sulfide and 37%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 28um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
The comparative example 2
Be 50,000 with weight-average molecular weight, melt flow index is that 324g/10min and molecular weight distribution are 3.0 linear polyphenylene sulfide resin, adds in the crosslinked device of the heat of oxidation the crosslinked 3h of the heat of oxidation stand-by
In homogenizer, add 51.5%wt polyphenylene sulfide cross-linked resin, 3.5%wt phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems oxidation inhibitor, the 45%wt granularity is to stir 2h behind the nano level 95% alumina-ceramic powder of 10hm, make it be mixed into homogeneous polyphenylene sulfide mixture, then the Preblend of 60%wt polyphenylene sulfide and 40%wt are through β-(3, the 4-epoxycyclohexyl) single fiber diameter was the glass fibre input twin screw extruder of 30um after ethyl trimethoxy silane (A-168) surface treatment agent was processed, be shaped through the twin screw extruder mixing extrusion, cooling, pelletizing forms the finished product composite granule, at last packing, warehouse-in, use.
The various physicalies of the polyphenyl thioether composite material that obtains with aforesaid method will show in Table 1.
Can see by tabulation one among Fig. 2: behind the polymethylmethacrylate elastomer compounds, the melt strength of polyphenylene sulfide (PPS) matrix material has obviously improved, overlap length obviously reduces, impact resistance, anti-bent pleat intensity, tensile strength obviously strengthen, and elongation at break also increases significantly with same type of material.
Owing to melting mixed very even with polyphenylene sulfide after adding polymethylmethacrylate elastomer compounds and phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems compound, can not produce parcel phenomenon or last shape, improved the processing performance of material, so just the balanced technique intensity index that has improved polyphenylene sulfide.
Product indices and employed detection method in Fig. 2 table:
Tensile strength and elongation are all carried out by GB/T1040-1992, and test speed is 10mm/min; Bent pleat intensity is pressed GB/T9341-1988 and is carried out, and resistance to impact shock is pressed GB/T1843-1996 and carried out, and heat-drawn wire is pressed the regulation of GB/T1634-1979 (1989) and carried out.
Performance index by Fig. 2 can be found out, the thermostability of product improves, and commercially available Japanese firm is contained glass fibre 40% like product parallel laboratory test, and its tensile strength, elongation, the bent pleat intensity of glass, resistance to impact shock are respectively 281Mpa, 3.7%, 315Mpa and 18.4j/m2.
After also finding in the experiment to add thicker glass fibre, for example single fiber diameter 35um parallel laboratory test, its resistance to impact shock has obvious enhancing.The elastomeric adding of polymethylmethacrylate also significantly improves the help that forward is provided to tensile strength and the elongation at break of product of the present invention.
After adding polymethylmethacrylate elastomer compounds and phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems compound, polyphenylene sulfide (PPS) matrix material is when thermostability obviously improves, and product overlap length is reduction trend.Since after adding polymethylmethacrylate elastomer compounds and phosphorous acid triphenylmethyl methacrylate in ninth of the ten Heavenly Stems compound, molten mixed very even with polyphenylene sulfide, can not produce parcel phenomenon or last shape yet.The improvement of all these processing condition makes some physical propertiess of product and processing performance obtain comprehensive improvement.
Although embodiments of the invention are with hexamethylene six alkane methyl alcohol polyoxy vinylbenzene ether phosphate amine salt (diethyls, three second), glycerine polyoxy vinylbenzene ether phosphate triethanolamine salt is what provide, also can consider wider Fatty Alcohol(C12-C14 and C12-C18) polyoxy vinylbenzene ether phosphate compounds in the actual production, for example: the aliphatic alcohol polyoxyvinethene phosphate sodium salt, hexamethylene six alkane methyl alcohol polyoxy vinylbenzene ether phosphate amine salt (diethyls, three second), fatty alcohol-ether (7) phosphoric acid ester triethanolamine salt, fatty alcohol-ether (9) phosphoric acid ester triethanolamine salt, octanol phophoric ester MCPH, octanol polyoxyethylene phosphate OPEK, nonyl phenol phosphate sylvite, nonyl phenol ether phosphoric acid monoesters ethanolamine salt, Nonyl pheno (7) ether phosphoric acid, single, dibasic acid esters Nonyl pheno (4-10) ether phosphoric acid, single, dibasic acid esters, the glycerin polyoxyethylene ether phosphoric acid ester, glycerine polyoxy vinylbenzene ether phosphate triethanolamine salt, PAPE, higher alcohols phosphoric acid ester sodium and phosphorylation Viscotrol C sodium salt, Stearinsaeure, the sulfuric ester of glycerol sodium salt, Castor Oil Phosphate Ester Salt, one or more compounds of the phosphate ester salts such as phosphorous acid triphenylmethyl methacrylate in the ninth of the ten Heavenly Stems.
The polymethylmethacrylate elastomer resin compound that adds in the present invention, can reduce the overlap (burr) that polyphenyl thioether composite granulates produces when injection moulded products is shaped, make the surface smoothness height of its molded article and the toughness of injection molded goods, these organoalkoxysilane resins can be vinyltrimethoxy silanes, vinyltriethoxysilane, the styryl triethoxyl silane, the styryl Trimethoxy silane, 3 monomethyl propenyloxy group propyl group methyl dimethoxysilanes, 3 monomethyl propenyloxy group propyl trimethoxy silicanes, 3 monomethyl propenyloxy group propyl group methyldiethoxysilane, 3 monomethyl propenyloxy group propyl-triethoxysilicanes, in the organoalkoxysilanes such as 3-propenyloxy group propyl trimethoxy silicane one or more, especially with vinyltrimethoxy silane, vinyltriethoxysilane, the styryl triethoxyl silane, the styryl Trimethoxy silane, the polymethylmethacrylate elastomerics is better, with the styryl triethoxyl silane, the styryl Trimethoxy silane, the polymethylmethacrylate elastomerics is best.
The objectionable impurities trapping agent that the present invention can also add is inclined to one side zincic acid/zincic acid or its esters compound, and they are: zincic acid, partially zincic acid, inclined to one side zincic acid calcium, partially zincic acid magnesium, partially zincic acid barium, zincic acid calcium, zincic acid magnesium, zincic acid barium, zinc carbonate, etc. contain the compound of zinc, with zincic acid, partially zincic acid is best, and they not only can suppress the generation of corrosives and impurity, can also replenish among the pellet as mineral filler.
Employed fiberglass surface treating agent is to adopt well-known β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane (A-168) surface treatment agent among the present invention.The mineral filler that can also add among the present invention reduces the overlap (burr) of polyphenylene sulfide resin composite material model when injection forming, these mineral fillers can be carbon blacks, nanometer grade silica, nanometer order quartz sand, glass microballon, the nanometer glass powder, Calucium Silicate powder, pure aluminium silicate, talcum, clay, mica, diatomite, the silicate such as wollastonite, ferric oxide, Nano titanium dioxide, zinc oxide, aluminum oxide, light calcium carbonate, nanometer grade calcium carbonate, magnesiumcarbonate, plaster stone, barium sulfate, silicon carbide, silicon nitride, boron nitride etc. are especially with nanometer grade calcium carbonate, nanometer grade silica, Nano titanium dioxide is best.
Claims (3)
1. the manufacture method of a polyphenylene sulfide ceramal, polyphenylene sulfide Preblend behind adding oxidation inhibitor, the ceramic powder is fully mixed in homogenizer, be shaped, form composite granule through cooling, pelletizing with glass fibre input parallel dual-screw extruding machine mixing extrusion again, it is characterized in that, comprise following processing step:
1) be 3-5 ten thousand with weight-average molecular weight, melt flow index is that 300-600g/10min and molecular weight distribution are the linear polyphenylene sulfide resin of 2.5-3.0, adds the crosslinked 2-3h of the heat of oxidation in the crosslinked device of the heat of oxidation;
2) will be 1) in homogenizer, fully mix after adding the weighting agents such as antioxidant, polymethylmethacrylate elastomerics in the polyphenylene sulfide cross-linked resin that obtains, the weight ratio of used antioxidant phosphorous acid triphenylmethyl methacrylate in the ninth of the ten Heavenly Stems and polyphenylene sulfide is 3-3.5: 100; The weight ratio of polymethylmethacrylate elastomerics and polyphenylene sulfide is 3-5: 100, and the weight ratio of ceramics powder and polyphenylene sulfide is 30-40: 100 obtain polyphenylene sulfide Preblend with this;
3) with 2) gained polyphenylene sulfide Preblend 60-70%wt again with through β-(3, the 4-epoxycyclohexyl) the ethyl trimethoxy silane surface treatment agent is processed later 40-30%wt glass fibre input twin screw extruder, forms the finished product composite granule through the shaping of twin screw extruder mixing extrusion, cooling, pelletizing.
2. the manufacture method of described a kind of polyphenylene sulfide ceramal according to claim 1 is characterized in that, described ceramic powder is nano level 95% alumina-ceramic powder, and its granularity is 5-10nm.
3. the manufacture method of described a kind of polyphenylene sulfide ceramal according to claim 1 is characterized in that, described glass fibre single fiber diameter is 20-30um.
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