CN101921486B - Polyphenylene sulfide compound film or fiber and manufacture method thereof - Google Patents
Polyphenylene sulfide compound film or fiber and manufacture method thereof Download PDFInfo
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- CN101921486B CN101921486B CN 201010285896 CN201010285896A CN101921486B CN 101921486 B CN101921486 B CN 101921486B CN 201010285896 CN201010285896 CN 201010285896 CN 201010285896 A CN201010285896 A CN 201010285896A CN 101921486 B CN101921486 B CN 101921486B
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- polyphenylene sulfide
- film
- fiber
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 104
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 104
- 239000000835 fiber Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title abstract description 45
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 150000001875 compounds Chemical class 0.000 title abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000012766 organic filler Substances 0.000 claims abstract description 5
- 125000000623 heterocyclic group Chemical group 0.000 claims description 45
- -1 Phosphate Ester Salt Chemical class 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 31
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 26
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 22
- 239000002131 composite material Substances 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 13
- 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 claims description 10
- 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 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 150000002148 esters Chemical class 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- 150000001298 alcohols Chemical class 0.000 claims description 6
- 239000004359 castor oil Substances 0.000 claims description 6
- 235000019438 castor oil Nutrition 0.000 claims description 6
- 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 claims description 6
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 6
- 239000012764 mineral filler Substances 0.000 claims description 5
- 230000026731 phosphorylation Effects 0.000 claims description 5
- 238000006366 phosphorylation reaction Methods 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 235000010216 calcium carbonate Nutrition 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- UUIPAJHTKDSSOK-UHFFFAOYSA-N (2-nonylphenyl) dihydrogen phosphate Chemical compound CCCCCCCCCC1=CC=CC=C1OP(O)(O)=O UUIPAJHTKDSSOK-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 3
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 3
- 150000002169 ethanolamines Chemical class 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 208000000848 Autosomal recessive primary microcephaly Diseases 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000006004 Quartz sand Substances 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 2
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 229910052570 clay Inorganic materials 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001095 magnesium carbonate Substances 0.000 claims description 2
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
- 229960001708 magnesium carbonate Drugs 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011505 plaster Substances 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 201000001729 primary autosomal recessive microcephaly Diseases 0.000 claims description 2
- AMCPECLBZPXAPB-UHFFFAOYSA-N propane-1,2,3-triol;sodium Chemical compound [Na].OCC(O)CO AMCPECLBZPXAPB-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 235000012222 talc Nutrition 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 239000010456 wollastonite Substances 0.000 claims description 2
- 229910052882 wollastonite Inorganic materials 0.000 claims description 2
- 239000011667 zinc carbonate Substances 0.000 claims description 2
- 235000004416 zinc carbonate Nutrition 0.000 claims description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 abstract description 3
- 230000003078 antioxidant effect Effects 0.000 abstract description 3
- 125000006615 aromatic heterocyclic group Chemical group 0.000 abstract 2
- 239000012760 heat stabilizer Substances 0.000 abstract 2
- 239000011256 inorganic filler Substances 0.000 abstract 2
- 229910003475 inorganic filler Inorganic materials 0.000 abstract 2
- 239000002861 polymer material Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 39
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 32
- 238000009413 insulation Methods 0.000 description 28
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 24
- 229920006026 co-polymeric resin Polymers 0.000 description 23
- 239000000126 substance Substances 0.000 description 20
- 238000005096 rolling process Methods 0.000 description 19
- 235000010265 sodium sulphite Nutrition 0.000 description 19
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 18
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 239000003795 chemical substances by application Substances 0.000 description 15
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 238000000605 extraction Methods 0.000 description 12
- 238000001914 filtration Methods 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 10
- 239000012752 auxiliary agent Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000012280 lithium aluminium hydride Substances 0.000 description 10
- 238000002203 pretreatment Methods 0.000 description 10
- 208000005156 Dehydration Diseases 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 230000018044 dehydration Effects 0.000 description 9
- 238000006297 dehydration reaction Methods 0.000 description 9
- 239000004744 fabric Substances 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000004721 Polyphenylene oxide Substances 0.000 description 8
- 238000002242 deionisation method Methods 0.000 description 8
- ODFPJHVZYSBZQO-UHFFFAOYSA-N ethenoxyethene;phosphoric acid Chemical compound C=COC=C.OP(O)(O)=O ODFPJHVZYSBZQO-UHFFFAOYSA-N 0.000 description 8
- 229920006380 polyphenylene oxide Polymers 0.000 description 8
- 230000003252 repetitive effect Effects 0.000 description 8
- 238000005201 scrubbing Methods 0.000 description 8
- 238000007669 thermal treatment Methods 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 8
- AKCRQHGQIJBRMN-UHFFFAOYSA-N 2-chloroaniline Chemical compound NC1=CC=CC=C1Cl AKCRQHGQIJBRMN-UHFFFAOYSA-N 0.000 description 7
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 5
- 230000004927 fusion Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- XRZITQCNEOBRRP-UHFFFAOYSA-N NC1=CC=C(C=C1)Cl.CC1=C(C(=O)O)C=CC=C1C(=O)O Chemical compound NC1=CC=C(C=C1)Cl.CC1=C(C(=O)O)C=CC=C1C(=O)O XRZITQCNEOBRRP-UHFFFAOYSA-N 0.000 description 4
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- QHMVQKOXILNZQR-UHFFFAOYSA-N 1-methoxyprop-1-ene Chemical group COC=CC QHMVQKOXILNZQR-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910052728 basic metal Inorganic materials 0.000 description 3
- 150000003818 basic metals Chemical class 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VMADQUDNIAMBCH-UHFFFAOYSA-N 1-chloro-2-nitronaphthalene Chemical compound C1=CC=CC2=C(Cl)C([N+](=O)[O-])=CC=C21 VMADQUDNIAMBCH-UHFFFAOYSA-N 0.000 description 2
- ZTSYGXLLTYTXCS-UHFFFAOYSA-N 1-chloronaphthalen-2-amine Chemical compound C1=CC=CC2=C(Cl)C(N)=CC=C21 ZTSYGXLLTYTXCS-UHFFFAOYSA-N 0.000 description 2
- VVWZVMNIZMMNTG-UHFFFAOYSA-N 4-chloro-2,3,5,6-tetramethylaniline Chemical compound CC1=C(C(=C(C(=C1C)Cl)C)C)N VVWZVMNIZMMNTG-UHFFFAOYSA-N 0.000 description 2
- JCLZLZKUISPXDC-UHFFFAOYSA-N 4-chloro-2,6-dimethylaniline Chemical compound CC1=CC(Cl)=CC(C)=C1N JCLZLZKUISPXDC-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- KMKVQFSRXDJXAQ-UHFFFAOYSA-N CC1=C(C=C(C(=C1)Cl)C)N.CC1=C(C=CC(=C1C)Cl)N Chemical compound CC1=C(C=C(C(=C1)Cl)C)N.CC1=C(C=CC(=C1C)Cl)N KMKVQFSRXDJXAQ-UHFFFAOYSA-N 0.000 description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 2
- OVBJJZOQPCKUOR-UHFFFAOYSA-L EDTA disodium salt dihydrate Chemical compound O.O.[Na+].[Na+].[O-]C(=O)C[NH+](CC([O-])=O)CC[NH+](CC([O-])=O)CC([O-])=O OVBJJZOQPCKUOR-UHFFFAOYSA-L 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- QGGIFPRVTBQAPW-UHFFFAOYSA-N NC1=CC=C(C=C1)Cl.CC1(CC(C(=O)O)=CC=C1)C(=O)O Chemical compound NC1=CC=C(C=C1)Cl.CC1(CC(C(=O)O)=CC=C1)C(=O)O QGGIFPRVTBQAPW-UHFFFAOYSA-N 0.000 description 2
- VEKNPFQTLIPTMM-UHFFFAOYSA-N NC1=CC=C(C=C1)Cl.CC1=CC=C(C=C1C(=O)O)C(=O)O Chemical compound NC1=CC=C(C=C1)Cl.CC1=CC=C(C=C1C(=O)O)C(=O)O VEKNPFQTLIPTMM-UHFFFAOYSA-N 0.000 description 2
- OAPMGEJEQUFGNL-UHFFFAOYSA-N NC1=CC=C(C=C1)Cl.CC=1C=C(C=C(C(=O)O)C1)C(=O)O Chemical compound NC1=CC=C(C=C1)Cl.CC=1C=C(C=C(C(=O)O)C1)C(=O)O OAPMGEJEQUFGNL-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 2
- ZQPPLYAHRYNJOK-UHFFFAOYSA-N [N+](=O)([O-])C1=CC=C(C=C1)Cl.CC1=C(C(=O)O)C=CC=C1C(=O)O Chemical compound [N+](=O)([O-])C1=CC=C(C=C1)Cl.CC1=C(C(=O)O)C=CC=C1C(=O)O ZQPPLYAHRYNJOK-UHFFFAOYSA-N 0.000 description 2
- PCDKXXGCDQCBTG-UHFFFAOYSA-N [N+](=O)([O-])C1=CC=C(C=C1)Cl.CC1=CC=C(C=C1C(=O)O)C(=O)O Chemical compound [N+](=O)([O-])C1=CC=C(C=C1)Cl.CC1=CC=C(C=C1C(=O)O)C(=O)O PCDKXXGCDQCBTG-UHFFFAOYSA-N 0.000 description 2
- BTJZWKGBFRKLKM-UHFFFAOYSA-N [N+](=O)([O-])C1=CC=C(C=C1)Cl.CC=1C=C(C=C(C(=O)O)C1)C(=O)O.[N+](=O)([O-])C1=CC=C(C=C1)Cl.CC1(CC(C(=O)O)=CC=C1)C(=O)O Chemical compound [N+](=O)([O-])C1=CC=C(C=C1)Cl.CC=1C=C(C=C(C(=O)O)C1)C(=O)O.[N+](=O)([O-])C1=CC=C(C=C1)Cl.CC1(CC(C(=O)O)=CC=C1)C(=O)O BTJZWKGBFRKLKM-UHFFFAOYSA-N 0.000 description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N glutaric acid Chemical compound OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000003352 sequestering agent Substances 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 150000003504 terephthalic acids Chemical class 0.000 description 2
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- NWAOUFGCGKRZBR-UHFFFAOYSA-N 1-chloro-2,3-dimethyl-4-nitrobenzene Chemical compound CC1=C(C)C([N+]([O-])=O)=CC=C1Cl NWAOUFGCGKRZBR-UHFFFAOYSA-N 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- BYPIKLIXBPMDBY-UHFFFAOYSA-N 2-hydroxypropanoic acid;potassium Chemical compound [K].CC(O)C(O)=O BYPIKLIXBPMDBY-UHFFFAOYSA-N 0.000 description 1
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- FDMSHDARBBGHGL-UHFFFAOYSA-N 4-chloro-2,3,5,6-tetramethyl-1-nitronaphthalene Chemical compound CC1=C(C2=CC=C(C(=C2C(=C1C)Cl)C)C)[N+](=O)[O-] FDMSHDARBBGHGL-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- GOMPLJOPYGQBPL-UHFFFAOYSA-K [F-].[F-].[F-].F.[B+3] Chemical compound [F-].[F-].[F-].F.[B+3] GOMPLJOPYGQBPL-UHFFFAOYSA-K 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- HCPOCMMGKBZWSJ-UHFFFAOYSA-N ethyl 3-hydrazinyl-3-oxopropanoate Chemical compound CCOC(=O)CC(=O)NN HCPOCMMGKBZWSJ-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000003176 fibrotic effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000004247 glycine and its sodium salt Substances 0.000 description 1
- 235000013905 glycine and its sodium salt Nutrition 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 1
- XKPJKVVZOOEMPK-UHFFFAOYSA-M lithium;formate Chemical compound [Li+].[O-]C=O XKPJKVVZOOEMPK-UHFFFAOYSA-M 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 235000011147 magnesium chloride Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- UICBCXONCUFSOI-UHFFFAOYSA-N n'-phenylacetohydrazide Chemical compound CC(=O)NNC1=CC=CC=C1 UICBCXONCUFSOI-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 235000012771 pancakes Nutrition 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 description 1
- 229940067157 phenylhydrazine Drugs 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229960004249 sodium acetate Drugs 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 229940029258 sodium glycinate Drugs 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 description 1
- WUWHFEHKUQVYLF-UHFFFAOYSA-M sodium;2-aminoacetate Chemical compound [Na+].NCC([O-])=O WUWHFEHKUQVYLF-UHFFFAOYSA-M 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- HSYFJDYGOJKZCL-UHFFFAOYSA-L zinc;sulfite Chemical compound [Zn+2].[O-]S([O-])=O HSYFJDYGOJKZCL-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention relates to a polyphenylene sulfide compound film or fiber and a manufacture method thereof. The film or fiber comprises the following raw materials in percentage by weight: 60-90 percent of polyphenylene sulfide resin, 0-35 percent of polyphenylene sulfide resin containing aromatic heterocyclic rings, 0.5-0.7 percent of heat stabilizer, 0.4-0.8 percent of antioxidant, 3-5.8 percent of high polymer material, 0.2-0.6 percent of inorganic filler and 0.5-2.5 percent of organic filler. The manufacture method comprises the following steps of: pretreating the polyphenylene sulfide resin and the polyphenylene sulfide resin containing the aromatic heterocyclic rings, then adding the heat stabilizer and uniformly mixing for granulating and molding; drying obtained granules, adding the antioxidant, the high polymer material, the inorganic filler and the organic filler, and uniformly mixing; and finally, extruding the mixed material into films or fibers by using an extruder. The film or the fiber has the advantages of excellent insulating property and high self structural strength, and the toughness and the tensile breaking elongation of the film or the fiber are obviously superior to that of the film or the fiber manufactured in the prior art.
Description
The original bill application number of this division application is 2008100465751, and the applying date is on November 17th, 2008, and denomination of invention is " containing polyphenylene sulfide copolymer of fragrant heterocycle and preparation method thereof, purposes and goods ".
Technical field
The present invention relates to polyphenylene sulfide, relate in particular to a kind of polyphenylene sulfide copolymer that contains fragrant heterocycle and preparation method thereof, purposes and goods.
Background technology
Along with the development of scientific-technical progress and society, people are more and more extensive to exploitation, the application of new technology and novel material, and are more and more higher to the requirement of electronics, electrical apparatus insulation material, the electrically insulating material that especially has high heat resistance, hydrolytic resistance.
Polyphenylene sulfide has excellent chemical resistance and the thermostability under the high temperature, and suction, moisture absorption are very low, and has good fire-retardant, insulation, radiation hardness.
But, the goods made from this material merely, toughness, intensity are relatively poor, easily embrittlement, especially film, fibre product, toughness and tension fracture elongation rate are low, can not satisfy service requirements.
The investigators of countries in the world seek to make PPS (polyphenylene sulfide) films, Fibrotic method constantly making great efforts to explore always, and present technique means is, other intensity of fusion, material that toughness is higher in polyphenylene sulfide improve intensity, the toughness of goods.But the intensity of these adulterants self, toughness also are not very high, and very limited with the compatible degree of polyphenylene sulfide yet, and the toughness of goods, intensity still are not very high.Especially as film, fiber, toughness and tension fracture elongation rate are low, can not satisfy service requirements.For example, the manufacture method of the disclosed a kind of PPS (polyphenylene sulfide) films of Chinese patent (application number: 200580038776.1), it is to adopt polyphenylene sulfide and polyamide resin ultrafine particulate to be mixed in certain proportion mixture, manufacture method by diaxial orientation obtains PPS (polyphenylene sulfide) films, yet the problems such as the toughness of the PPS (polyphenylene sulfide) films of making in this way and elongation at break are not still solved at all.
Summary of the invention
One of purpose of the present invention provides a kind of polyphenylene sulfide copolymer that contains fragrant heterocycle, and this multipolymer has special molecular structure, and self intensity is high, and fine with the compatible degree of polyphenylene sulfide, and with itself and polyphenylene sulfide fusion, toughness, the intensity of resulting product are high.
Two of purpose of the present invention provides the preparation method that this contains the polyphenylene sulfide copolymer of fragrant heterocycle.
Three of purpose of the present invention, provide the polyphenylene sulfide copolymer that a kind of usefulness contains fragrant heterocycle, film/fiber and the manufacture method thereof that the polyphenylene sulfide compound material is made, the toughness of this film/fiber and tension fracture elongation rate obviously are better than film/fiber that prior art is made.
The technical scheme that realizes above-mentioned purpose is:
A kind of polyphenylene sulfide copolymer that contains fragrant heterocycle, this multipolymer are the molecular structure embedding-Har-S-structures at-Ar-S-, form following structure:
-Ar-S-Har-S-
In the formula, Har represents fragrant heterocycle.
These molecular structures may be ordered arrangement, lack of alignment even by feeding in raw material to control molecular structure---be the molecular structure of blocked, such purpose is to improve the intensity index of polyphenylene sulfide copolymer resin.
The above-mentioned preparation method who contains the polyphenylene sulfide copolymer of fragrant heterocycle, with sodium sulphite, the santochlor of mol ratio 1: 0.6-0.9: 0.4-0.1,2-(4-chloro phenyl)-5-chloro benzoglyoxaline is raw material, take METHYLPYRROLIDONE as solvent, polycondensation is synthesized under the effect of basic metal solubility promoter, and step is as follows:
(1). in sodium sulphite, add auxiliary agent, stirred lower slow intensification 2-8 hour, be warming up to 190-203 ℃ of lower dehydration;
(2). the sodium sulphite after will dewatering, santochlor, basic metal solubility promoter add in the METHYLPYRROLIDONE solvent, are warming up to 200-280 ℃, polyreaction 1-3 hour;
(3). add 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, be warming up to 200-280 ℃, polyreaction 4-6 hour;
(4). add the 1.0-5.0%mol molecular weight regulator, be warming up to 200-280 ℃, polyreaction 2-3 hour;
(5). be warmed up to again 210-280 ℃ the 150-190 ℃ of lower 1.0-3.3%mol of adding adjusting agent and continue to stir 1 hour;
(6). under 100-200 ℃, add the 0.1-1.3%mol deionizer, deviate from ion;
(7). 100-200 ℃ of lower the filtration, extract with extraction agent when filter cake is cooled to 50-80 ℃, obtain after filtration containing again the polyphenylene sulfide copolymer of fragrant heterocycle.
Described auxiliary agent is take material with strong reducing power as main: such as lithium aluminum hydride, lithium hydride sodium, lithium hydride potassium, formaldehyde, acetaldehyde, sodium borohydride, POTASSIUM BOROHYDRIDE, sodium borohydride, Thiovanic acid, hydrazine hydrate, phenylhydrazine, pyrodin, phosphorous acid ester, Sodium Nitrite, tetrafluoride boron, 4, in the two sulfonyl hydrazides of 4-oxo any, especially take lithium aluminum hydride as best.
Described basic metal solubility promoter be in lithium chloride, lithium sulfide, Quilonum Retard, lithium formate, Lithium Acetate, sodium formiate, sodium-acetate, calcium formiate, lime acetate, magnesium formiate, magnesium acetate, potassium formiate, the potassium acetate any.
Described molecular weight regulator is mainly to contain the halogenated compound of amino or nitro, can be one or several the mixture in the following material: to amino-chloro-benzene, p-Nitrophenyl chloride, to amino chloronaphthalene, to the nitro chloronaphthalene, 2-methyl isophthalic acid-amino-4-chlorobenzene, 5-methyl isophthalic acid-amino-4-chlorobenzene, 3-methyl isophthalic acid-amino-4-chlorobenzene, 6-methyl isophthalic acid-amino-4-chlorobenzene, 2-methyl isophthalic acid-amino-4-chlorobenzene, 2-methyl isophthalic acid-nitro-4-chlorobenzene, 3-methyl isophthalic acid-nitro-4-chlorobenzene 5-methyl isophthalic acid-nitro-4-chlorobenzene, 6-methyl isophthalic acid-nitro-4-chlorobenzene, 2,3-dimethyl-1-amino-4-chlorobenzene 2,5-dimethyl-1-amino-4-chlorobenzene, 2,6-dimethyl-1-amino-4-chlorobenzene, 2,3,5-trimethylammonium-1-amino-4-chlorobenzene, 2,5,6-trimethylammonium-1-amino-4-chlorine, 2,3,5,6-tetramethyl--1-amino-4-chlorobenzene, 2,3-dimethyl-1-amino-4-chlorobenzene 2,5-dimethyl-1-amino-4-chlorobenzene, 2,6-dimethyl-1-amino-4-chlorobenzene, 2,3,5-trimethylammonium-1-amino-4-chlorobenzene, 2,5,6-trimethylammonium-1-amino-4-chlorine, 2,3,5,6-tetramethyl--1-amino-4-chlorobenzene, 2,3-dimethyl-1-nitro-4-chlorobenzene, 2,5,6-trimethylammonium-1-nitro-4-chloronaphthalene, 2,3,5,6-tetramethyl--1-nitro-4-chloronaphthalene etc. contains the halogenated compound of amino or nitro; Take to amino-chloro-benzene, p-Nitrophenyl chloride, to amino chloronaphthalene, to nitro chloronaphthalene, 2-methyl isophthalic acid-amino-4-chlorobenzene, 5-methyl isophthalic acid-amino-4-chlorobenzene, 3-methyl isophthalic acid-amino-4-chlorobenzene, 6-methyl isophthalic acid-amino-4-chlorobenzene, 2-methyl isophthalic acid-amino-4-chlorobenzene, 2-methyl isophthalic acid-nitro-4-chlorobenzene, 3-methyl isophthalic acid-nitro-4-chlorobenzene 5-methyl isophthalic acid-nitro-4-chlorobenzene, 6-methyl isophthalic acid-nitro-4-chlorobenzene as better, especially take to amino-chloro-benzene, p-Nitrophenyl chloride as best.
Described adjusting agent is as main take acidic substance, or even the weak base salt of these materials, can be one or several of following material: organic acid: as to the acid of benzene two Shens, oxalic acid, propanedioic acid, Succinic Acid, formic acid, acetic acid, propionic acid, palmitinic acid, citric acid, lauric acid, hexanodioic acid, butyric acid, n-nonanoic acid, Sorbic Acid, stearic acid, toxilic acid, pentanedioic acid, isoamyl diacid; Mineral acid: such as sulfuric acid, hydrochloric acid, especially take terephthalic acid as best.
Described deionizer is as main take ammonium salt or zinc salt or sulfonate or sequestrant, can be one or several of following material: ammonium sulfate, magnesium chloride, ammonium chloride, ammonium sulphite, zinc sulfate, zinc sulfite, zinc chloride, sebacic acid penta 2 ammoniums, ammonium nitrate, Soduxin, hexanodioic acid sodium, ethylenediamine tetraacetic acid (EDTA), disodium EDTA, Piao Linhuan, calcium acetate, Sodium Glycinate, hydroxy-propionic acid potassium, tetrasodium ethylenediamine tetraacetate, dodecylbenzene sulfonate, sodium allyl sulfonate, sodium cetanesulfonate, with ethylenediamine tetraacetic acid (EDTA), disodium EDTA, Piao Linhuan, tetrasodium ethylenediamine tetraacetate is especially take ethylenediamine tetraacetic acid (EDTA) or plain quinoline ring sequestrant as best.
Described extraction agent is take low boiling point organic solvent as main, they can be in methyl alcohol, ethanol, propyl alcohol, butanols, acetone, monochloro methane, methylene dichloride, chloroform, the benzene,toluene,xylene any, especially take methyl alcohol, ethanol, chloroform, benzene as best.
This multipolymer is owing to using 2-(4-chloro phenyl)-5-chloro benzoglyoxaline to be raw material, obtain the polyphenylene sulfide copolymer resin that contains fragrant heterocycle that polydispersity coefficient is lower and molecular weight distribution is very narrow, the degree of crystallinity of resin, whiteness, physical strength, melting viscosity, oxygen index, polydispersity coefficient are more excellent.
The above-mentioned polyphenylene sulfide copolymer that contains fragrant heterocycle is used for and the polyphenylene sulfide fusion, makes various injection mouldings or extrudate.
A kind of polyphenyl sulfide composite film/fiber, make with the raw material of following weight ratio:
Described thermo-stabilizer is one or both mixture of higher alcohols phosphoric acid ester sodium, Castor Oil Phosphate Ester Salt.
Described oxidation inhibitor be BHA (butyl hydroxyanisole), BHT (in 2,6 di tert butyl 4 methyl phenol, the pentaerythritol tetrathioglycollate any; The antioxidant that adds, purpose are the oxygenolysis that reduces polyphenylene sulfide and contain the polyphenylene sulfide copolymer resin of fragrant heterocycle.
Any or any several mixture in described macromolecular material polyethylene, polypropylene, tetrafluoroethylene, polyester, polycarbonate, polyphenylene sulfide acid amides, EVA, the polybenzoate; Add macromolecular material, purpose is to improve the elongation at break of film/fiber.
Described mineral filler is any or any several mixture in silicate, ferric oxide, Nano titanium dioxide, zinc oxide, aluminum oxide, light calcium carbonate, nanometer grade calcium carbonate, magnesiumcarbonate, calcium carbonate, zinc carbonate, plaster stone, barium sulfate, silicon carbide, silicon nitride, the boron nitride such as carbon black, nanometer grade silica, nanometer order quartz sand, glass microballon, nanometer glass powder, Calucium Silicate powder, pure aluminium silicate, talcum, clay, mica, diatomite, wollastonite.Add mineral filler, its objective is the mechanical property that improves goods.
Described organic filler is phosphate compounds and organoalkoxysilane resin, wherein, phosphate compounds is polyphenylene oxides Vinyl Ether phosphate monoester, polyphenylene oxides Vinyl Ether phosphoric acid ester sodium, polyphenylene oxides Vinyl Ether phosphoric acid ester diethylamine, polyphenylene oxides Vinyl Ether phosphoric acid ester triethylamine, 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, the higher alcohols phosphoric acid ester sodium, phosphorylation Viscotrol C sodium salt, Castor Oil Phosphate Ester Salt, nonyl phenol ether phosphoric acid monoesters ethanolamine salt, Nonyl pheno (7) ether phosphoric acid monoesters, Nonyl pheno (7) ether phosphoric acid dibasic acid esters, Nonyl pheno (4-10) ether phosphoric acid monoesters, Nonyl pheno (4-10) ether phosphoric acid dibasic acid esters, nonyl phenol polyphenylene oxides Vinyl Ether phosphoric acid ester diethanolamine salt, nonyl phenol polyphenylene oxides Vinyl Ether phosphoric acid ester triethanolamine salt, PAPE, higher alcohols phosphoric acid ester sodium and phosphorylation Viscotrol C sodium salt, Stearinsaeure, the sulfuric ester of glycerol sodium salt, any or any several mixture in the phosphate ester salts such as Castor Oil Phosphate Ester Salt are especially with the higher alcohols phosphoric acid ester sodium, phosphorylation Viscotrol C sodium salt, Castor Oil Phosphate Ester Salt, nonyl phenol phosphate sylvite, nonyl phenol ether phosphoric acid monoesters ethanolamine salt, Nonyl pheno (7) ether phosphoric acid monoesters, Nonyl pheno (7) ether phosphoric acid dibasic acid esters, Nonyl pheno (4-10) ether phosphoric acid monoesters, Nonyl pheno (4-10) ether phosphoric acid dibasic acid esters, nonyl phenol polyphenylene oxides Vinyl Ether phosphoric acid ester diethanolamine salt, nonyl phenol polyphenylene oxides Vinyl Ether phosphoric acid ester triethanolamine salt is better; Take higher alcohols phosphoric acid ester sodium, phosphorylation Viscotrol C sodium salt, Castor Oil Phosphate Ester Salt as best; The organoalkoxysilane resin is vinyltrimethoxy silane, vinyltriethoxysilane, the styryl triethoxyl silane, styryl trimethoxy silicon, 3 monomethyl propenyloxy group propyl group methyldiethoxysilane, 3 monomethyl propenyloxy group propyl-triethoxysilicanes, any or any several mixture in the organoalkoxysilanes such as 3-metacryloxy propyl trimethoxy silicane, especially with 3 monomethyl propenyloxy group propyl-triethoxysilicanes, 3-metacryloxy propyl trimethoxy silicane is better, take 3-metacryloxy propyl trimethoxy silicane as best.Add phosphate compounds, purpose is not lose other physical property, the especially thermal stability of polyphenylene sulfide when polyphenyl sulfide composite film is shaped, thereby when the crystallization velocity of polyphenylene sulfide improved, condition of surface was good during shaping.Add the organoalkoxysilane resin compound, purpose is to improve the consistency of the additives such as polyphenylene sulfide copolymer and other macromolecular materials, mineral filler, make simultaneously the surface smoothness of its molded article high, significantly reduce chemical substances such as using softening agent, brightening agent, can also improve the toughness of goods simultaneously.
The manufacture method of above-mentioned polyphenyl sulfide composite film/fiber comprises step:
1.. with polyphenylene sulfide, contain the respectively pre-treatment of polyphenylene sulfide copolymer resin of fragrant heterocycle, carrying out washing treatment is removed oligopolymer, ring compound, byproduct of reaction, reaction promoter and other impurity in the resin, and the weight percent of these impurity in resin is no more than 0.01%;
2.. add thermo-stabilizer and mix granulating and forming;
3.. pellet is dry, and water content drops to below 0.05%;
4.. get the polyphenylene sulfide pellet, contain polyphenylene sulfide pellet, thermo-stabilizer, oxidation inhibitor, macromolecular material, mineral filler, the organic filler of fragrant heterocycle by proportioning, mix;
5.. compound is extruded into film/fiber with forcing machine.
The described step 5. step of cast film is:
A. by the heating and melting device of forcing machine with the compound melting, melt temperature is controlled between 290-340 ℃;
B. by the volume pump of forcing machine melt is sent into the extruded films tool, be extruded into the sheet material of the wide 500-600mm of thick 1-2mm;
C. the insulation passage of sheet material in forcing machine sent into two-way drawing-off passage, by the rolling of forcing machine, drafting assembly with sheet material rolls, drawing-off becomes thick 0.025-0.05mm fabric width 1500-2000mm polyphenyl sulfide composite film; The temperature of insulation passage is controlled at 120-140 ℃;
D. with film not care about one's appearance trimmed, with the harvest film rolling of winder.
The described step 5. step of extruded fibers is:
A. by the heating and melting device of forcing machine with the compound melting, melt temperature is controlled between 290-340 ℃;
B. by the volume pump of forcing machine melt is sent into the extruded films tool, be spun into strand;
C. by multistage up-coiler drawing-off and furl strand, it is attenuated step by step, until the strand diameter meets the requirements, furl rolling.
Technique effect of the present invention:
The polyphenylene sulfide copolymer that contains fragrant heterocycle of the present invention, the structural strength of self is high, and with itself and polyphenylene sulfide fusion, toughness, the intensity of resulting product are high.Especially be fit to make film and fiber, subordinate list one has been listed the performance index of film.
The various characteristics of subordinate list one film
Film is used:
1. be the best insulating material that reaches the f level, can make electrical condenser, impedance electronic component, pancake coil skeleton, coating electric wire thing, cloak, vaporizer barrier film, temperature-sensitive printing material, soft disk, electronic photography sense etc.
2. can be used as H-F level electric insulation film, capacitor film, magnetic pipe recording material counterdie, flexible printed circuit substrate etc.
3. be widely used in parcel conductor, optical fiber etc. as insulating material.Electrical condenser (SMT, high temperature, high frequency, high reliability), variable electrical condenser, circuit card flexibly, keyboard membrane, insulating material, flat motor hawser, parcel, industrial tape, inner coverage rate material, sound equipment film, diaphragm, lithium cell packing.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
One. contain the synthetic example of the polyphenylene sulfide copolymer resin of fragrant heterocycle
Example 1
In autoclave, 120 kilograms of N-methyl-2 pyrrolidone (NMP) are solvent, add sodium sulphite (Na
2S.3H
2O) 42 kilograms, 0.1 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 203 ℃ of dehydrations with 2 hours times, add 24.9 kilograms of santochlor, 20 kilograms of NMP, being 200 ℃ in temperature reacted 3 hours, add 29.9 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline (being called for short DCPBI), like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.6: 0.4 again.When temperature is 280 ℃, reacted 4 hours, and under the condition of this temperature, adding is to 0.36 kilogram of amino-chloro-benzene, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 0.46 kilogram of the terephthalic acid and to process after 1 hour, be cooled to 200 ℃ and add 0.08 kilogram of deionizer mixture ethylenediamine tetraacetic acid (EDTA), and constantly stirred 1 hour, be cooled to 100 ℃ of filtrations, filter cake is cooled to 50 ℃ again, repeatedly the polymkeric substance that makes is extracted repeatedly with 40 liters of extraction agent methyl alcohol, filter, then with 40 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filter.100 ℃ of lower vacuum-dryings, obtain containing 36.89 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, adopt flash process to reclaim the polyphenylene sulfide copolymer of gained.Copolymer resin flow rate 143g/10min (ASTM-1238-70), 284.9 ℃ of fusing points, ash 0.37%, volatile matter 0.21% (150 ℃), Mw are about 5.2 ten thousand, polydispersity coefficient PD2.0, and oxygen index can reach 48.
Example 2
In autoclave, add N-methyl-2 pyrrolidone (NMP) 60 kilograms, sodium sulphite (Na
2S.3H
2O) 21.5 kilograms, 0.05 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 190 ℃ of dehydrations with 8 hours times, add 18.3 kilograms of santochlor, 10 kilograms of NMP, being 280 ℃ in temperature reacted 1 hour, add 3.75 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.9: 0.1 again.When temperature is 280 ℃, reacted 6 hours, and under the condition of this temperature, adding is to 0.89 kilogram of amino-chloro-benzene, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 0.75 kilogram of the terephthalic acid and to process after 1 hour, be cooled to 100 ℃ and add 0.54 kilogram of deionizer mixture ethylenediamine tetraacetic acid (EDTA), and constantly stirred 1 hour, be cooled to 50 ℃ 100 ℃ of filtrations, repeatedly the polymkeric substance that makes is extracted repeatedly with 400 liters of extraction agent methyl alcohol, filter, then with 200 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filter.100 ℃ of lower vacuum-dryings, obtain containing 13.5 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 121g/10min (ASTM-1238-70), 286.3 ℃ of fusing points, ash 0.20%, volatile matter 0.15% (150 ℃), Mw are about 5.8 ten thousand, polydispersity coefficient PD1.9, and oxygen index can reach 43.
Example 3
In autoclave, add N-methyl-2 pyrrolidone (NMP) 240 kilograms, sodium sulphite (Na
2S.3H
2O) 84 kilograms, 0.2 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 203 ℃ of dehydrations with 2 hours times, add 49.8 kilograms of santochlor, 40 kilograms of NMP, being 200 ℃ in temperature reacted 3 hours, add 59.8 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.6: 0.4 again.When temperature is 280 ℃, reacted 4 hours, and under the condition of this temperature, adding is to 3.56 kilograms of amino-chloro-benzenes, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 3.0 kilograms of the terephthalic acids and to process after 1 hour, be cooled to 200 ℃ and add 2.16 kilograms of deionizer mixture ethylenediamine tetraacetic acid (EDTA)s, and constantly stirred 1 hour, be cooled to 100 ℃ of filtrations, filter cake is cooled to 50 ℃ again, repeatedly the polymkeric substance that makes is extracted repeatedly with 80 liters of extraction agent methyl alcohol, filter, then with 40 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filter.100 ℃ of lower vacuum-dryings, obtain containing 77.78 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 103g/10min (ASTM-1238-70), 286.7 ℃ of fusing points, ash 0.17%, volatile matter 0.19% (150 ℃), Mw are about 5.9 ten thousand, polydispersity coefficient PD1.93, and oxygen index can reach 42.
Example 4
In autoclave, add N-methyl-2 pyrrolidone (NMP) 120 kilograms, sodium sulphite (Na
2S.3H
2O) 43 kilograms, 0.1 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 190 ℃ of dehydrations with 8 hours times, add 36.6 kilograms of santochlor, 20 kilograms of NMP, being 280 ℃ in temperature reacted 1 hour, add 7.5 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.9: 0.1 again.When temperature is 280 ℃, reacted 6 hours, and under the condition of this temperature, adding is to 0.36 kilogram of amino-chloro-benzene, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 0.46 kilogram of the terephthalic acid and to process after 1 hour, be cooled to 100 ℃ and add 0.08 kilogram of deionizer mixture ethylenediamine tetraacetic acid (EDTA), and constantly stirred 1 hour, be cooled to 50 ℃ 100 ℃ of filtrations, repeatedly the polymkeric substance that makes is repeatedly extracted, filters with 40 liters of extraction agent methyl alcohol, then with 40 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filtration.100 ℃ of lower vacuum-dryings, obtain containing 26.78 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 161g/10min (ASTM-1238-70), 285.1 ℃ of fusing points, ash 0.25%, volatile matter 0.20% (150 ℃), Mw are about 5.5 ten thousand, polydispersity coefficient PD2.01, and oxygen index can reach 41.
Example 5
In autoclave, add N-methyl-2 pyrrolidone (NMP) 120 kilograms, sodium sulphite (Na
2S.3H
2O) 42 kilograms, 0.1 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 203 ℃ of dehydrations with 2 hours times, add 24.9 kilograms of santochlor, 20 kilograms of NMP, being 200 ℃ in temperature reacted 3 hours, add 29.9 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.6: 0.4 again.When temperature is 280 ℃, reacted 4 hours, and under the condition of this temperature, add 0.43 kilogram of p-Nitrophenyl chloride, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 0.46 kilogram of the terephthalic acid and to process after 1 hour, be cooled to 200 ℃ and add 0.08 kilogram of deionizer mixture ethylenediamine tetraacetic acid (EDTA), and constantly stirred 1 hour, be cooled to 100 ℃ of filtrations, filter cake is cooled to 50 ℃ again, repeatedly the polymkeric substance that makes is extracted repeatedly with 400 liters of extraction agent methyl alcohol, filter, then with 400 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filter.100 ℃ of lower vacuum-dryings, obtain containing 36.44 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 143g/10min (ASTM-1238-70), 284.5 ℃ of fusing points, ash 0.27%, volatile matter 0.17% (150 ℃), Mw are about 5.5 ten thousand, polydispersity coefficient PD2.03, and oxygen index can reach 45.
Example 6
In autoclave, add N-methyl-2 pyrrolidone (NMP) 120 kilograms, sodium sulphite (Na
2S.3H
2O) 43 kilograms, 0.1 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 190 ℃ of dehydrations with 8 hours times, add 36.6 kilograms of santochlor, 20 kilograms of NMP, being 280 ℃ in temperature reacted 1 hour, add 7.5 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.9: 0.1 again.When temperature is 280 ℃, reacted 6 hours, and under the condition of this temperature, add 2.2 kilograms of p-Nitrophenyl chlorides, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 1.5 kilograms of the terephthalic acids and to process after 1 hour, be cooled to 100 ℃ and add 1.08 kilograms of deionizer mixture ethylenediamine tetraacetic acid (EDTA)s, and constantly stirred 1 hour, be cooled to 50 ℃ 100 ℃ of filtrations, repeatedly the polymkeric substance that makes is repeatedly extracted, filters with 400 liters of extraction agent methyl alcohol, then with 400 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filtration.100 ℃ of lower vacuum-dryings, obtain containing 25.71 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 114g/10min (ASTM-1238-70), 286.2 ℃ of fusing points, ash 0.21%, volatile matter 0.19% (150 ℃), Mw are about 5.8 ten thousand, polydispersity coefficient PD1.84, and oxygen index can reach 43.
Example 7
In autoclave, add N-methyl-2 pyrrolidone (NMP) 120 kilograms, sodium sulphite (Na
2S.3H
2O) 42 kilograms, 0.1 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 203 ℃ of dehydrations with 2 hours times, add 24.9 kilograms of santochlor, 20 kilograms of NMP, being 200 ℃ in temperature reacted 3 hours, add 29.9 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.6: 0.4 again.When temperature is 280 ℃, reacted 4 hours, and under the condition of this temperature, add 2.2 kilograms of p-Nitrophenyl chlorides, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 0.15 kilogram of the terephthalic acid and to process after 1 hour, be cooled to 200 ℃ and add 1.08 kilograms of deionizer mixture ethylenediamine tetraacetic acid (EDTA)s, and constantly stirred 1 hour, be cooled to 100 ℃ of filtrations, filter cake is cooled to 50 ℃ again, repeatedly the polymkeric substance that makes is extracted repeatedly with 400 liters of extraction agent methyl alcohol, filter, then with 400 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filter.100 ℃ of lower vacuum-dryings, obtain containing 36.10 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 107g/10min (ASTM-1238-70), 286.9 ℃ of fusing points, ash 0.17%, volatile matter 0.20% (150 ℃), Mw are about 5.9 ten thousand, polydispersity coefficient PD1.91, and oxygen index can reach 42.
Example 8
In autoclave, add N-methyl-2 pyrrolidone (NMP) 120 kilograms, sodium sulphite (Na
2S.3H
2O) 43 kilograms, 0.1 kilogram of lithium aluminum hydride (auxiliary agent), under the pressure of 0.01Mpa nitrogen, stir on one side, heat up on one side, rise to 190 ℃ of dehydrations with 8 hours times, add 36.6 kilograms of santochlor, 20 kilograms of NMP, being 280 ℃ in temperature reacted 1 hour, add 7.5 kilograms of 2-(4-chloro phenyl)-5-chloro benzoglyoxaline, like this, the mol ratio of sodium sulphite and santochlor and 2-(4-chloro phenyl)-5-chloro benzoglyoxaline is 1: 0.9: 0.1 again.When temperature is 280 ℃, reacted 6 hours, and under the condition of this temperature, add 0.43 kilogram of p-Nitrophenyl chloride, polyreaction is cooled to 185 ℃ after 2 hours, add and to be warmed up to 250 ℃ behind 0.46 kilogram of the terephthalic acid and to process after 1 hour, be cooled to 100 ℃ and add 0.08 kilogram of deionizer mixture ethylenediamine tetraacetic acid (EDTA), and constantly stirred 1 hour, be cooled to 50 ℃ 100 ℃ of filtrations, repeatedly the polymkeric substance that makes is extracted repeatedly with 400 liters of extraction agent methyl alcohol, filter, then with 400 liters of deionization moisture 6 times the polymkeric substance that makes is carried out repetitive scrubbing, filter.100 ℃ of lower vacuum-dryings, obtain containing 26.13 kilograms of the polyphenylene sulfide copolymer resins of fragrant heterocycle, flow rate 161g/10min (ASTM-1238-70), 285.1 ℃ of fusing points, ash 0.35%, volatile matter 0.29% (150 ℃), Mw are about 5.3 ten thousand, polydispersity coefficient PD2.05, and oxygen index can reach 46.
In actual production, if use Piao Linhuan to be used as the deionizer of polymkeric substance and use the effect of ethylenediamine tetraacetic acid (EDTA) the same, still use the Piao Lin ring can increase production cost; Although use acetone, chloroform, ethanol, benzene equal solvent to be used as extraction agent and can to obtain the same with the effect of using methyl alcohol to obtain, but as when using chloroform, benzene, toluene as extraction agent, also to come chloroform, benzene, toluene equal solvent in the washing leaching cake with methyl alcohol, ethanol, acetone at last, therefore the solvent that preferably uses methyl alcohol, ethanol, acetone etc. to dissolve each other with water is in order to better reclaim these solvents.
Two. PPS (polyphenylene sulfide) films is made example
Example 1
Then the good polyphenylene sulfide of pre-treatment and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle adopt following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe, expressing technique flow process and condition by forcing machine, be that the forcing machine that temperature is controlled between 290-340 ℃ is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 590mm of 1mm, melt forms the thick sheet material of 590mm that is for 1mm is wide by T-shaped mould ejection, sheet material is 120 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that horizontal or vertical three grades of twin shaft pinch rollers roll it and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 2000mm for the 0.025mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder, the processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the channel temperature of two-way drawing-off is controlled at 120 ℃, drawing-off multiplying power 3.0, drawing speed is 30m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 0.5pa, and its temperature remains on 120 ℃.
3). the rolling speed of winder is at 35m/min.
4). heat treatment time is 5 seconds, 270 ℃ of thermal treatment temps
The various characteristics of its film will show in Table 1.
Example 2
That this example adopts following prescription with the difference of example 1
Adopt above-mentioned technical recipe, expressing technique flow process and condition by forcing machine, be that the forcing machine that temperature is controlled between 290-340 ℃ is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 580mm of 1.2mm, melt forms the thick 580mm sheet material that is for 1.2mm is wide by T-shaped mould ejection, sheet material is 126 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that horizontal or vertical three grades of twin shaft pinch rollers roll it again and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 1860mm for the 0.028mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder, the processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the channel temperature of two-way drawing-off is controlled between 248 ℃, drawing-off multiplying power 3.6, drawing speed is 38m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 0.9Mpa, and its temperature remains on 130 ℃.
3). the rolling speed of winder is at 45m/min.
4). heat treatment time is 8 seconds, 249 ℃ of thermal treatment temps
The various characteristics of its film will show in Table 1.
Example 3
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe, expressing technique flow process and condition by forcing machine, the forcing machine that namely is controlled between 290-340 ℃ by temperature is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 570mm of 1.6mm, melt forms the thick sheet material of 570mm that is for 1.6mm is wide by T-shaped mould ejection, sheet material is 260 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that three grades of twin shaft pinch rollers roll it and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 2000mm for the 0.030mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder.
The processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the channel temperature of two-way drawing-off is controlled at 140 ℃, drawing-off multiplying power 4.2, drawing speed is 42m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 1.4Mpa, and its temperature remains on 131 ℃.
3). the rolling speed of winder is at 55m/min.
4). heat treatment time is 12 seconds, 260 ℃ of thermal treatment temps
The various characteristics of its film will show in Table 1.
Example 4
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe by expressing technique flow process and the condition of forcing machine, the forcing machine that namely is controlled between 290-340 ℃ by temperature is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 560mm of 1.5mm, melt forms the thick sheet material of 560mm that is for 1.5mm is wide by T-shaped mould ejection, sheet material is 136 ℃ belt passage in insulation, be transported to the passage of horizontal or vertical two-way drawing-off by passage, be transported to by passage that three grades of twin shaft pinch rollers roll it and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 2000mm for the 0.035mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder
The processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the channel temperature of two-way drawing-off is controlled at 138 ℃, drawing-off multiplying power 4.5, drawing speed is 60m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 2.3Mpa, and its temperature remains between 136 ℃.
3). the rolling speed of winder is at 65m/min.
4). heat treatment time is 5 seconds, 270 ℃ of thermal treatment temps.
The various characteristics of its film will show in Table 1.
Example 5
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe by expressing technique flow process and the condition of forcing machine, the forcing machine that namely is controlled between 290-340 ℃ by temperature is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 600mm of 2mm, melt forms the thick sheet material of 600mm that is for 2mm is wide by T-shaped mould ejection, sheet material is 136 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that three grades of twin shaft pinch rollers roll it again and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 2000mm for the 0.05mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder
The processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the channel temperature of two-way drawing-off is controlled at 140 ℃, drawing-off multiplying power 5, drawing speed is 60m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 3Mpa, and its temperature remains on 120 ℃.
3). the rolling speed of winder is at 65m/min.
4). heat treatment time is 30 seconds, 240 ℃ of thermal treatment temps
The various characteristics of its film will show in Table 1.
Example 6
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe by expressing technique flow process and the condition of forcing machine, the forcing machine that namely is controlled between 290-340 ℃ by temperature is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 520mm of 1.4mm, melt forms the thick sheet material of 520mm that is for 1.4mm is wide by T-shaped mould ejection, sheet material is 126 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that three grades of twin shaft pinch rollers roll it and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 1940mm for the 0.03mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder
The processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the path temperature of two-way drawing-off is controlled at 129 ℃, drawing-off multiplying power 4.4, drawing speed is 44m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 0.5-3Mpa, and its temperature remains on 128 ℃.
3). the rolling speed of winder is at 49m/min.
4). heat treatment time is 20 seconds, 244 ℃ of thermal treatment temps.
The various characteristics of its film will show in Table 1.
Example 7
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenyl that contains fragrant heterocycle
Then the thioether copolymer resin adopts following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe by expressing technique flow process and the condition of forcing machine, the forcing machine that namely is controlled between 290-340 ℃ by temperature is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 590mm of 1.6mm, melt forms the thick sheet material of 590mm that is for 1.6mm is wide by T-shaped mould ejection, sheet material is 134 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that three grades of twin shaft pinch rollers roll it again and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 1780mm for the 0.035mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder
The processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the path temperature of two-way drawing-off is controlled at 134 ℃, drawing-off multiplying power 4.8, drawing speed is 56m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 2.5Mpa, and its temperature remains on 136 ℃.
3). the rolling speed of winder is at 60m/min.
4). heat treatment time is 10 seconds, 251 ℃ of thermal treatment temps
The various characteristics of its film will show in Table 1.
Example 8
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
Adopt above-mentioned technical recipe by expressing technique flow process and the condition of forcing machine, the forcing machine that namely is controlled between 290-340 ℃ by temperature is extruded, arrive the T-shaped die nozzle insulation can of film by the head gear pump delivery, be equipped with volume pump at insulation can, polyphenylene sulfide is transported to by volume pump with the polyphenylene sulfide copolymer melt that contains fragrant heterocycle and is equipped with take wide as the long T-shaped mould as 600mm of 1.8mm, melt forms the thick sheet material of 600mm that is for 1.8mm is wide by T-shaped mould ejection, sheet material is 138 ℃ belt passage in insulation, be transported to the passage of two-way drawing-off by passage, be transported to by passage that three grades of twin shaft pinch rollers roll it again and drawing-off to be processed into thick be the polyphenyl sulfide composite film of 2000mm for the 0.045mm fabric width, at last with its not care about one's appearance trimmed, by the film rolling that is wound into of winder
The processing condition of two-way drawing-off polyphenyl sulfide composite film:
1). the path temperature of two-way drawing-off is controlled at 138 ℃, drawing-off multiplying power 4.8, drawing speed is 51m/min, and passes into nitrogen.
2). the pressure of twin shaft pinch roller is at 0.5-3Mpa, and its temperature remains on 138 ℃.
3). the rolling speed of winder is at 55m/min.
4). heat treatment time is 25 seconds, 244 ℃ of thermal treatment temps
The various characteristics of its film will show in Table 1.
The comparative example 1
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
Adopt the processing condition of example 7, the various characteristics that makes film will show in Table 1.
The comparative example 2
Adopt above-mentioned processing condition and the flow process polyphenylene sulfide that pre-treatment is good and the polyphenylene sulfide copolymer resin that contains fragrant heterocycle, then adopt following prescription that it is processed into mixture.
1) polyphenylene sulfide copolymer 33% that contains (1) fragrant heterocycle
Polyphenylene sulfide 62%
Polyphenylene sulfide acid amides 5%
Adopt technical process and the condition of example 8, the various characteristics that makes film will show in Table 1.
Three. polyphenylene sulfide fibre is made example
Make among the example 1-8 in above-mentioned PPS (polyphenylene sulfide) films, change the crowded die of forcing machine into a spray silk mould, will roll drafting assembly and change multistage coiling drafting assembly into.All the other are identical with PPS (polyphenylene sulfide) films manufacturing example 1-8.
Four. the polyphenylene sulfide injection-molded item is made
To contain polyphenylene sulfide copolymer and the polyphenylene sulfide fusion of fragrant heterocycle, with injection moulding machine and the required goods of corresponding mold injection.
Claims (1)
1. a polyphenyl sulfide composite film or fiber, it is characterized in that: the raw material with following weight ratio is made
The described polyphenylene sulfide that contains fragrant heterocycle is the molecular structure embedding-HAr-S-structure at-Ar-S-, forms following structure
-Ar-S-HAr-S-
In the formula, HAr represents fragrant heterocycle;
Described thermo-stabilizer is one or both mixture of higher alcohols phosphoric acid ester sodium, Castor Oil Phosphate Ester Salt; Described oxidation inhibitor be in butyl hydroxyanisole, the 2,6 di tert butyl 4 methyl phenol any; Any or any several mixture in described macromolecular material polyethylene, polypropylene, tetrafluoroethylene, polyester, polycarbonate, polyphenylene sulfide acid amides, EVA, the polybenzoate; Described mineral filler is any or any several mixture in carbon black, nanometer grade silica, nanometer order quartz sand, glass microballon, nanometer glass powder, Calucium Silicate powder, pure aluminium silicate, talcum, clay, mica, diatomite, wollastonite, ferric oxide, Nano titanium dioxide, zinc oxide, aluminum oxide, magnesiumcarbonate, calcium carbonate, zinc carbonate, plaster stone, barium sulfate, silicon carbide, silicon nitride, the boron nitride; Described organic filler is phosphate compounds/organoalkoxysilane resin, wherein, phosphate compounds is any or any several mixture in octanol phophoric ester MCPH, octanol polyoxyethylene phosphate OPEK, nonyl phenol phosphate sylvite, nonyl phenol ether phosphoric acid monoesters ethanolamine salt, Nonyl pheno (4-10) ether phosphoric acid monoesters, Nonyl pheno (4-10) ether phosphoric acid dibasic acid esters, PAPE and phosphorylation Viscotrol C sodium salt, the sulfuric ester of glycerol sodium salt; The organoalkoxysilane resin is any or any several mixture in vinyltrimethoxy silane, vinyltriethoxysilane, styryl triethoxyl silane, the styryl trimethoxy silicon.
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| CN103409835B (en) * | 2013-08-05 | 2015-07-29 | 江苏瑞泰科技有限公司 | The production method of thin dawn polyphony thioether short fiber |
| CN103849147B (en) * | 2014-03-14 | 2016-08-17 | 常州钟恒新材料有限公司 | Biaxial orientation polyphenyl sulfide composite film |
| CN103965631A (en) * | 2014-04-23 | 2014-08-06 | 安徽依采妮纤维材料科技有限公司 | Polyropylene fiber modified polyphenyl thioether material for automobile plastic part |
| CN103965608A (en) * | 2014-04-23 | 2014-08-06 | 安徽依采妮纤维材料科技有限公司 | Industrial magnesium calcium slag modified polyphenyl thioether material for automobile plastic part |
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| CN104262964A (en) * | 2014-09-24 | 2015-01-07 | 苏州冰心文化用品有限公司 | High temperature-resistant material and preparation method thereof |
| CN104328842B (en) * | 2014-10-13 | 2016-08-17 | 沈思维 | Anti-crack building foam battenboard process processed |
| CN105544001A (en) * | 2016-03-01 | 2016-05-04 | 苏州金泉新材料股份有限公司 | Method for directly preparing PPS (polyphenylene sulfide) modified short fibers through modification of PPS powder |
| CN105820535A (en) * | 2016-04-29 | 2016-08-03 | 太仓龙益塑业有限公司 | Improved polycarbonate plastic |
| CN106147231A (en) * | 2016-07-13 | 2016-11-23 | 张静 | A kind of preparation method of humidity steady resistance rate polyphenyl thioether composite material |
| CN109957125A (en) * | 2019-04-04 | 2019-07-02 | 德阳科吉高新材料有限责任公司 | A kind of manufacturing method of PPS films |
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