CN105838386A - Liquid crystalline polyester composition - Google Patents
Liquid crystalline polyester composition Download PDFInfo
- Publication number
- CN105838386A CN105838386A CN201610226654.5A CN201610226654A CN105838386A CN 105838386 A CN105838386 A CN 105838386A CN 201610226654 A CN201610226654 A CN 201610226654A CN 105838386 A CN105838386 A CN 105838386A
- Authority
- CN
- China
- Prior art keywords
- crystalline polyester
- liquid
- polyester composition
- repetitive
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 229920000728 polyester Polymers 0.000 title claims abstract description 109
- 239000000203 mixture Substances 0.000 title claims abstract description 98
- 239000007788 liquid Substances 0.000 title abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 58
- 239000011734 sodium Substances 0.000 claims abstract description 58
- 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 abstract description 56
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 28
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 238000010998 test method Methods 0.000 claims abstract description 8
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 49
- 230000003252 repetitive effect Effects 0.000 claims description 45
- 239000010936 titanium Substances 0.000 claims description 31
- 229910052719 titanium Inorganic materials 0.000 claims description 31
- -1 aromatic diol Chemical class 0.000 claims description 30
- 239000004973 liquid crystal related substance Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 19
- 125000003118 aryl group Chemical group 0.000 claims description 17
- 239000000945 filler Substances 0.000 claims description 17
- 239000000835 fiber Substances 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 11
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 10
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- 239000003365 glass fiber Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012765 fibrous filler Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 4
- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical compound C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- VCCBEIPGXKNHFW-UHFFFAOYSA-N biphenyl-4,4'-diol Chemical group C1=CC(O)=CC=C1C1=CC=C(O)C=C1 VCCBEIPGXKNHFW-UHFFFAOYSA-N 0.000 claims description 3
- 239000003086 colorant Substances 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 3
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004014 plasticizer Substances 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 229920000914 Metallic fiber Polymers 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 239000010425 asbestos Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- OQRWAMBQGTYSRD-UHFFFAOYSA-N dipotassium;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[K+].[K+].[Ti+4].[Ti+4].[Ti+4].[Ti+4] OQRWAMBQGTYSRD-UHFFFAOYSA-N 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052895 riebeckite Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 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
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000029087 digestion Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 24
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 13
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 11
- 238000002156 mixing Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 6
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000001632 sodium acetate Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- 230000002152 alkylating effect Effects 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000001636 atomic emission spectroscopy Methods 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 150000002484 inorganic compounds Chemical class 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 150000002989 phenols Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000001294 propane Substances 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- DAEPDZWVDSPTHF-UHFFFAOYSA-M sodium pyruvate Chemical compound [Na+].CC(=O)C([O-])=O DAEPDZWVDSPTHF-UHFFFAOYSA-M 0.000 description 4
- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 229920000106 Liquid crystal polymer Polymers 0.000 description 3
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 235000017281 sodium acetate Nutrition 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NMRPBPVERJPACX-UHFFFAOYSA-N (3S)-octan-3-ol Natural products CCCCCC(O)CC NMRPBPVERJPACX-UHFFFAOYSA-N 0.000 description 2
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 2
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Natural products C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- WOFPPJOZXUTRAU-UHFFFAOYSA-N 2-Ethyl-1-hexanol Natural products CCCCC(O)CCC WOFPPJOZXUTRAU-UHFFFAOYSA-N 0.000 description 2
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- BCEQKAQCUWUNML-UHFFFAOYSA-N 4-hydroxybenzene-1,3-dicarboxylic acid Chemical compound OC(=O)C1=CC=C(O)C(C(O)=O)=C1 BCEQKAQCUWUNML-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 description 2
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 description 2
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 description 2
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 2
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004378 air conditioning Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 238000005804 alkylation reaction Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- VKJLWXGJGDEGSO-UHFFFAOYSA-N barium(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Ba+2] VKJLWXGJGDEGSO-UHFFFAOYSA-N 0.000 description 2
- 125000001797 benzyl group Chemical class [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 230000006208 butylation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- MIHINWMALJZIBX-UHFFFAOYSA-N cyclohexa-2,4-dien-1-ol Chemical compound OC1CC=CC=C1 MIHINWMALJZIBX-UHFFFAOYSA-N 0.000 description 2
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 2
- KVGOXGQSTGQXDD-UHFFFAOYSA-M decane-1-sulfonate Chemical compound CCCCCCCCCCS([O-])(=O)=O KVGOXGQSTGQXDD-UHFFFAOYSA-M 0.000 description 2
- MRSOZKFBMQILFT-UHFFFAOYSA-L diazanium;oxalate;titanium(2+) Chemical compound [NH4+].[NH4+].[Ti+2].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O MRSOZKFBMQILFT-UHFFFAOYSA-L 0.000 description 2
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 description 2
- 125000003963 dichloro group Chemical group Cl* 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 150000004683 dihydrates Chemical class 0.000 description 2
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 description 2
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- HHFAWKCIHAUFRX-UHFFFAOYSA-N ethoxide Chemical compound CC[O-] HHFAWKCIHAUFRX-UHFFFAOYSA-N 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- JCDAAXRCMMPNBO-UHFFFAOYSA-N iron(3+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4].[Fe+3].[Fe+3] JCDAAXRCMMPNBO-UHFFFAOYSA-N 0.000 description 2
- 125000000468 ketone group Chemical group 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- SFDZETWZUCDYMD-UHFFFAOYSA-N monosodium acetylide Chemical compound [Na+].[C-]#C SFDZETWZUCDYMD-UHFFFAOYSA-N 0.000 description 2
- SJHHDDDGXWOYOE-UHFFFAOYSA-N oxytitamium phthalocyanine Chemical compound [Ti+2]=O.C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 SJHHDDDGXWOYOE-UHFFFAOYSA-N 0.000 description 2
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 2
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 2
- 229940047670 sodium acrylate Drugs 0.000 description 2
- ODZPKZBBUMBTMG-UHFFFAOYSA-N sodium amide Chemical compound [NH2-].[Na+] ODZPKZBBUMBTMG-UHFFFAOYSA-N 0.000 description 2
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 2
- 229960002218 sodium chlorite Drugs 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 235000017454 sodium diacetate Nutrition 0.000 description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 229940001584 sodium metabisulfite Drugs 0.000 description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 239000004324 sodium propionate Substances 0.000 description 2
- 235000010334 sodium propionate Nutrition 0.000 description 2
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 2
- 229960003212 sodium propionate Drugs 0.000 description 2
- 229940054269 sodium pyruvate Drugs 0.000 description 2
- 229960004025 sodium salicylate Drugs 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 229960001471 sodium selenite Drugs 0.000 description 2
- 239000011781 sodium selenite Substances 0.000 description 2
- 235000015921 sodium selenite Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 229940074404 sodium succinate Drugs 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 239000001433 sodium tartrate Substances 0.000 description 2
- 229960002167 sodium tartrate Drugs 0.000 description 2
- 235000011004 sodium tartrates Nutrition 0.000 description 2
- 229940048842 sodium xylenesulfonate Drugs 0.000 description 2
- QUCDWLYKDRVKMI-UHFFFAOYSA-M sodium;3,4-dimethylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1C QUCDWLYKDRVKMI-UHFFFAOYSA-M 0.000 description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 150000005846 sugar alcohols Chemical class 0.000 description 2
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- AEBYJSOWHQYRPK-UHFFFAOYSA-N 1,1'-biphenyl;sodium Chemical compound [Na].C1=CC=CC=C1C1=CC=CC=C1 AEBYJSOWHQYRPK-UHFFFAOYSA-N 0.000 description 1
- WSEFPKKOUNRCAJ-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;octadecanoic acid Chemical class OCC(CO)(CO)CO.CCCCCCCCCCCCCCCCCC(O)=O WSEFPKKOUNRCAJ-UHFFFAOYSA-N 0.000 description 1
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- HSSYVKMJJLDTKZ-UHFFFAOYSA-N 3-phenylphthalic acid Chemical compound OC(=O)C1=CC=CC(C=2C=CC=CC=2)=C1C(O)=O HSSYVKMJJLDTKZ-UHFFFAOYSA-N 0.000 description 1
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 229940111121 antirheumatic drug quinolines Drugs 0.000 description 1
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 1
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229920006038 crystalline resin Polymers 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical class [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002194 fatty esters Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000008450 motivation Effects 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- PRVDZBGQJZSFNF-UHFFFAOYSA-N nonyl phenyl hydrogen phosphite Chemical compound CCCCCCCCCOP(O)OC1=CC=CC=C1 PRVDZBGQJZSFNF-UHFFFAOYSA-N 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical class CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 150000004885 piperazines Chemical class 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/38—Polymers
- C09K19/3804—Polymers with mesogenic groups in the main chain
- C09K19/3809—Polyesters; Polyester derivatives, e.g. polyamides
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a liquid crystalline polyester composition. The weight content of the metallic sodium element is 1ppm-800ppm based on the total weight of the liquid crystalline polyester composition. The test method of the weight content of the metallic sodium element includes: drying the liquid crystalline polyester composition for 4h at 120 DEG C, taking out 1g sample to be treated, adding nitric acid and hydrogen peroxide, heating the mixture for 2h, adding nitric acid and hydrogen peroxide continuously during the reaction, taking the digested sample after the digestion of the sample completed, and analyzing the weight content of the metallic sodium element of the sample by using an automatic inductively coupled plasma atomic emission spectrometer with model of 720 ES of Agilent company. The tensile strength of the obtained liquid crystalline polyester composition is improved obviously by using the formula of the liquid crystalline polyester composition adding the metallic sodium element with weight content of 1ppm-800ppm based on the total weight of the liquid crystalline polyester composition, and the heat-resistant stability at high temperature is obviously improved unexpectedly.
Description
Technical field
The present invention relates to polymeric material field, particularly to a kind of liquid-crystalline polyester composition.
Background technology
Liquid crystal polyester (LCP) is as a kind of special engineered class material, compared with resins for universal use, there is higher fusing point and high heat-resistant stability, but thermally decompose or because of the strand chain rupture by external force hot shearing when liquid crystal polyester remains at high temperature processing, cause the phenomenon that various aspects of performance declines.In order to improve the heat-resistant stability of liquid crystal polyester, those skilled in the art have done many trials.
US5397502 discloses the liquid-crystalline polymer composition that a kind of heat-resistant stability improves, and compositions comprises the alkali metal of 15 ~ 3000ppm or the magnesium of 50 ~ 3000ppm or calcium；Liquid crystal polymer contains P-hydroxybenzoic acid, hydroquinone, '-biphenyl diphenol, p-phthalic acid, NDA and biphenyl dicarboxylic acid repetitive.The introducing of metallics improves fusing point and the heat distortion temperature of compositions, makes thermostability be improved.But patent is mentioned make liquid crystal polymer at high temperature contact with functional compound and long enough make its melt viscosity decline at least 10%.Well known to professional and technical personnel in the field, liquid crystalline resin processes for a long time under higher than its melt temperature, owing to thermal decomposition can cause the reduction of melt viscosity and molecular weight, and the decline also having mechanical property thus brought, and the generation of side reaction, this may increase the risk that resin bubbles.
CN1234749 discloses a kind of liquid-crystal polyester resin, the repetitive wherein containing 4 hydroxyisophthalic acid and/or salicylic acid and come is as copolymer composition, and containing the alkali metal compound of 10 ~ 5000ppm, and claim that the coloring of resin is excellent, thermostability is high, and mechanicalness is good.This invention mainly stresses the improvement of liquid crystal polyester degree of staining and impact property, and in embodiment or patent, other parts do not illustrate whether heat resistance changes.And whether this patent undeclared invention are applicable to liquid-crystalline polyester composition.
US6755991 discloses a kind of liquid-crystalline polyester composition, comprises at least one aromatic dicarboxylic acid, and at least one contains naphthalene nucleus carboxylic acid and at least one alkali metal of 1 ~ 1000ppm and at least one transition metal of 0 ~ 3000ppm.Liquid-crystalline polyester composition prepared by this invention has whiteness and the impact strength of improvement, and whether not mentioned high-temperature heat-resistance stability changes.
Up to the present, about interpolation metallic sodium element in liquid-crystalline polyester composition, the impact of described liquid-crystalline polyester composition hot strength and high-temperature heat-resistance stability is had no report.
The present inventor through great many of experiments surprisingly it has been found that, select the weight content gross weight based on liquid-crystalline polyester composition adding metallic sodium element in liquid-crystalline polyester composition formula when being 1ppm-800ppm, the hot strength of the liquid-crystalline polyester composition obtained is obviously improved, and high-temperature heat-resistance stability obtains beyond thought significantly improving.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the primary and foremost purpose of the present invention is to provide a kind of hot strength to be obviously improved, and the liquid-crystalline polyester composition that high-temperature heat-resistance stability significantly improves.
The present invention is achieved through the following technical solutions:
A kind of liquid-crystalline polyester composition, gross weight based on liquid-crystalline polyester composition, the weight content of metallic sodium element is 1ppm-800ppm.
Being preferably based on the gross weight of liquid-crystalline polyester composition, the weight content of metallic sodium element is preferably 5ppm-500ppm, more preferably 10ppm-300ppm.
Wherein, the method for testing of the weight content of metallic sodium element: liquid-crystalline polyester composition is dried 4 hours at 120 DEG C, take the pending sample of 1g, add nitric acid and hydrogen peroxide, heat 2 hours, period is continuously added nitric acid and hydrogen peroxide；After having cleared up of sample, cancelling the sample after solution, the full-automatic inductively coupled plasma atomic emission spectrometer using Agilent company model to be 720ES is analyzed Gold Samples and is belonged to the weight content of sodium element.
Document is not yet had to be reported in liquid-crystalline polyester composition the introducing metallic sodium element impact on composition properties at present, present inventors have unexpectedly found that in liquid-crystalline polyester composition, introduce appropriate sodium element, liquid-crystalline polyester composition hot strength is obviously improved, and shows surprising heat-resistant stability in high temperature environments.And when in liquid-crystalline polyester composition, the weight content of metallic sodium element exceedes particular value, liquid-crystal composition contains higher metal residuals, its dielectric properties as electronic apparatus type component will certainly be affected, be substantially reduced its range, and mobility there will be significantly decline.
nullIntroducing typically by adding what compounds containing sodium realized of metallic sodium element，Compounds containing sodium can be selected from D-ALPHA-Hydroxypropionic acid sodium、Pfansteihl sodium、Sodium acetate、Sodium sulfite、Sodium oxide、Sodamide.、Sodium nitrate、Sodium sulfide、Sodium sulfate、Sodium phosphate、Disodium oxalate.、Sodium tartrate binary dihydrate、Sodium chlorite、Sodium selenite、Sodium metasilicate、Sodium metabisulfite、Sodium hexafluorisilicate、The inorganic compound such as sodium diacetate，It can also be sodium acrylate、Sodium acetylide、Sodium ethylate、Sodium citrate、Enuatrol、Sodium salicylate、Feldalat NM、Biphenyl sodium、Sodium phenate、1-sodium butane sulfonate、1-propane sodium mercaptides、1-dodecane sulfonic acid sodium、1-sodium nonanesulfonate、1-sodium heptanesulfonate、1-decane sulfonate、2-propane sodium mercaptides、2-sodium naphthalene sulfonate、Disodium succinate、Sodium succinate、Sodium Pyruvate、Sodium propionate、Sodium xylene sulfonate、Sodium lauryl sulphate、The organic compound such as sodium tert-butoxide.The source of the metallic sodium element pointed by the present invention is not limited only to the example above, no matter uses the compounds containing sodium of which kind of form, and atomic emission spectrometry can be used to detect.The weight content of metallic sodium element is by metallic sodium element itself rather than on the basis of the compounds containing sodium adding metallic sodium element.The weight content of the metallic sodium element represented by ppm is to calculate on the basis of the gross weight of liquid-crystalline polyester composition.
The liquid-crystalline polyester composition of the present invention can also include Titanium element, gross weight based on liquid-crystalline polyester composition, and the weight content of Titanium element is 1ppm-800ppm, preferably 10ppm-500ppm.
Wherein, the method for testing of the weight content of Titanium element: liquid-crystalline polyester composition is dried 4 hours at 120 DEG C, take the pending sample of 1g, add nitric acid and hydrogen peroxide, heat 2 hours, period is continuously added nitric acid and hydrogen peroxide；After having cleared up of sample, cancelling the sample after solution, the full-automatic inductively coupled plasma atomic emission spectrometer using Agilent company model to be 720ES is analyzed Gold Samples and is belonged to the weight content of titanium elements.
nullIntroducing typically by adding what titanium-containing compound realized of Titanium element，Titanium-containing compound can be selected from Barium metatitanate.、Iron titanate (II)、Aluminium titanates、Lithium titanate、Zinc titanate、Metatitanic acid sodium salt、Titanium oxide (II)、Titanium oxide (IV)、Silicon titanium oxide、Titanium carbide (IV)、Titanium disulfide、Ammonium hexa-fluorotitanate、Ten dichloro Tritanium/Trititanium aluminum、Titanium tetrafluoride、Titanium fluoride (III)、Titanium carbonitride、The inorganic compound such as ammonium titanyl oxalate monohydrate，Titanium ethanolate can also be selected、Titanyl phthalocyanine、Poly(tributoxy titanium)、2-ethyl-1-hexanol titanium、Trichlorine one cyclopentadienyl titanium、Acetylacetone,2,4-pentanedione oxygen titanium (IV)、Double (levulinic ketone group) diisopropyl titanate esters、Double (cyclopentadienyl group) titanium chloride (IV)、Tert-butyl alcohol titanium、Four (dimethyl amido) titanium (IV)、Titanium tetraisopropylate、Four methanol titaniums (IV)、Normal propyl alcohol titanium、Three isopropoxy titanium chlorides、Dichloro two indenyl titanium、Butyl titanate、Four (ethyl-methyl amido) titanium (IV)、The organic compound such as four (diethyl amido) titanium (IV).The source of the Titanium element pointed by the present invention is not limited only to the example above, no matter uses the titanium-containing compound of which kind of form, and atomic emission spectrometry can be used to detect.The weight content of Titanium element is by Titanium element itself rather than on the basis of the titanium-containing compound adding Titanium element.The weight content of the Titanium element represented by ppm is to calculate on the basis of the gross weight of liquid-crystalline polyester composition.
Wherein, described liquid-crystalline polyester composition, by weight, including following component:
Liquid crystal polyester
100 parts；
Filler
5 parts-100 parts.
Wherein, the fusing point of described liquid-crystalline polyester composition is 150 DEG C-400 DEG C；The method of testing of described fusing point is: by NETZSCH company DSC
200 F3 type differential scanning calorimeter DSC, are starting to test with the Elevated Temperature Conditions of 20 DEG C/min from room temperature, are observing endotherm peak temperature Tm1After, than Tm1Keep 5 minutes at a temperature of high 20 DEG C, then under the cooling conditions of 20 DEG C/min, be cooled to room temperature, be the most again measured with the Elevated Temperature Conditions of 20 DEG C/min, the endotherm peak temperature T now observedm2It is the fusing point of liquid-crystalline polyester composition.
Wherein, described liquid crystal polyester, by mole meter, comprise following repetitive:
Repetitive derived from aromatic hydroxy-carboxylic
30mol%-100mol%；
Repetitive derived from aromatic diol
0mol%-35mol%；
Repetitive derived from aromatic dicarboxylic acid
0mol%-35mol%。
Preferably, described liquid crystal polyester, by mole meter, including following repetitive:
Repetitive derived from aromatic hydroxy-carboxylic
50mol%-100mol%；
Repetitive derived from aromatic diol
0mol%-25mol%；
Repetitive derived from aromatic dicarboxylic acid
0mol%-25mol%。
Wherein, the described repetitive derived from aromatic hydroxy-carboxylic is selected from the repetitive derived from 4-HBA and/or the repetitive of 2-hydroxyl-6-naphthoic acid；The described repetitive derived from aromatic diol is selected from repetitive and/or the repetitive of 4,4 '-dihydroxybiphenyl of hydroquinone；The described repetitive derived from aromatic dicarboxylic acid is selected from the repetitive of the repetitive of p-phthalic acid, the repetitive of M-phthalic acid, 2,6-naphthalenedicarboxylic acid one or more.
The preparation method of above-mentioned liquid crystal polyester, can use standard polycondensation techniques method well known to those skilled in the art, comprise the steps:
In the reactor being equipped with agitator, thermometer, nitrogen ingress pipe and reflux condensate device, it is separately added into the repetitive derived from aromatic hydroxy-carboxylic, the repetitive derived from aromatic diol and the repetitive derived from aromatic dicarboxylic acid according to proportioning, and to add a certain proportion of acetic anhydride be acylating agent；Then nitrogen is passed through in reactor and replaces；Start stirring, in nitrogen stream, reactant mixture is heated to 140 DEG C-160 DEG C by room temperature, at this temperature backflow 1 hour-3 hours；Hereafter continue to heat up, mixture was heated to 300 DEG C-350 DEG C through 2 hours-4 hours from 140 DEG C-160 DEG C, steams unreacted acetic anhydride and side reaction product acetic acid in the process；Whole polycondensation phase, reduces pressure to reaction system, and the endpoint terminated as reaction by observing moment of torsion to raise；Now the prepolymer of melt state is discharged through drain hole, and be cooled to room temperature；Prepolymer being transferred to solid phase device further, through 5 hours-7 hours, temperature from ambient is increased to 260 DEG C-280 DEG C, insulation carries out solid-phase polymerization in 9 hours-11 hours at this temperature；Product is derived after terminating by reaction, thus obtains liquid crystal polyester.
Wherein, described filler is selected from fibrous filler and/or tabular filler；One or more in glass fibre, asbestos fibre, silicon dioxide fibre, silica-alumina fiber, potassium titanate fibre, carbon or graphite fibre, metallic fiber of described fibrous filler；It is preferably glass fibre；One or more in Talcum, Muscovitum, graphite, Kaolin of described tabular filler；It is preferably Muscovitum.
Preferably, the equal fibre diameter of number of described glass fibre is 3 microns-30 microns, and the equal draw ratio of number is more than or equal to 5, and number average fiber length is 50 microns-3000 microns；The mean diameter of described Muscovitum is 0.5 micron-200 microns.
When adding filler, relative to liquid crystal polyester 100 weight portion, adding the filler more than more than 100 parts, the mechanical strength of liquid-crystalline polyester composition may reduce.The method adding filler is not particularly limited, and can be set forth in method as known in the art.
Additionally, in addition to the foregoing, not damage, the liquid-crystalline polyester composition that the amount of the object of the invention uses in the present invention can add known various additives；Various additives can be selected from one or more in plasticizer, stabilizer, coloring agent, lubricant, releasing agent, antioxidant.
Suitably plasticizer is phthalic acid ester.
Suitably stabilizer includes organic phosphite, such as triphenyl phosphite, tricresyl phosphite-(2, 6-3,5-dimethylphenyl) ester, tricresyl phosphite-nonyl phenylester, dimethylbenene phosphonate, trimethyl phosphate etc., organic phosphite, alkylating monohydric phenol or polyhydric phenols, polyhydric phenols and the alkylation reaction product of diene, the butylation product of paracresol or bicyclopentadiene, alkylating hydroquinones, hydroxylated thiodiphenvl ethers, alkylidene-bis-phenol, benzyl compounds, polyhydric alcohol esters, benzotriazole, one or more combinations of benzophenone.
Suitably releasing agent includes metallic stearic salt, allcyl stearate class, stearic acid pentaerythritol esters, paraffin, lignite wax etc..
Suitably coloring agent includes various pigment, and dyestuff, such as metal-oxide and the zinc oxide of mixed-metal oxides of inorganic pigment, ferrum oxide, sulfide such as zinc sulfide etc.；Aluminate, silicate, ferrite etc., white carbon black, ultramarine；Organic pigment such as azo, diazonium class, Anthraquinones, phthalocyanine, quinolines, naphthalene, ketone, piperazine class etc..
Proper lubrication agent includes the slaine etc. of higher fatty acids, high-grade fatty ester, higher fatty acids.
Suitably antioxidant includes organic phosphite, alkylating monohydric phenol or polyhydric phenols, polyhydric phenols and the alkylation reaction product of diene, the butylation product of paracresol or bicyclopentadiene, alkylating hydroquinones, hydroxylated thiodiphenvl ethers, alkylidene-bis-phenol, benzyl compounds, polyhydric alcohol esters etc..
Various additives are not limited to above-mentioned several, can optionally contain other material common in the heat stability to liquid crystal polyester and harmless other species components of physical property and thermoplastic compounds, polypropylene, polyamide, polyester, polyphenylene sulfide, polyether-ketone, Merlon, polyether sulfone, polyphenyl ether and modified material thereof such as one or more, thermoplastic resin such as Polyetherimide, thermosetting resin such as phenolic resin, epoxy resin, polyimide resin and cyanide resin.
The method coordinating filler, various additives etc. in the liquid crystal polyester of embodiments of the present invention, the most specifically limits, it is possible to use dry type blending, solution mixing method, the polymerization of liquid crystal polyester are interpolation, melting mixing etc., the most preferably melting mixing.Such as kneader, uniaxially or biaxially extruder, rubber-roller machine etc., biaxial extruder is wherein preferably used.The temperature of melting mixing is more than the fusing point of liquid crystal polyester, fusing point less than+50 DEG C.
As compounding process, it is possible to use put into liquid crystal polyester, filler, various additive in the lump to carry out mixing method from rear dress charger；Liquid crystal polyester and various additive can also be penetrated from rear dress charger, add filler from side charger and carry out mixing method, the liquid-crystalline polyester composition master batch that high concentration comprises liquid crystal polyester and various additive can also be prepared, then liquid-crystalline polyester composition master batch and filler are carried out any one method of the method etc. of the mixing concentration to become regulation.
The liquid-crystalline polyester composition of embodiments of the present invention by carrying out injection moulding, the known melt molding product such as injection compression molding, compression forming, extrusion molding, blow molding, compressing spinning.Products formed described here, can be the various cellosilks etc. such as the various membrane products such as injection-molded article, extrusion molding article, compressing product, sheet, pipe, non-stretched film, single axle drawn membrane, biaxially oriented film, undrawn yarn, super drawing silk.In the case of extrusion molding, can significantly obtain the effect of the present invention, the most preferably.
Wherein, the liquid-crystalline polyester composition obtained by extruding-out process, specifically comprise the following steps that after liquid crystal polyester, filler, compounds containing sodium and/or titanium-containing compound and/or various additive high-speed mixer mix homogeneously according to proportioning, add double screw extruder, melting mixing under the screw speed of 280RPM-320RPM, barrel temperature is 290 DEG C-355 DEG C, extrusion, cooling, pelletizing, obtain liquid-crystalline polyester composition.
nullWherein compounds containing sodium can be selected from D-ALPHA-Hydroxypropionic acid sodium、Pfansteihl sodium、Sodium acetate、Sodium sulfite、Sodium oxide、Sodamide.、Sodium nitrate、Sodium sulfide、Sodium sulfate、Sodium phosphate、Disodium oxalate.、Sodium tartrate binary dihydrate、Sodium chlorite、Sodium selenite、Sodium metasilicate、Sodium metabisulfite、Sodium hexafluorisilicate、The inorganic compound such as sodium diacetate，It can also be sodium acrylate、Sodium acetylide、Sodium ethylate、Sodium citrate、Enuatrol、Sodium salicylate、Feldalat NM、Biphenyl sodium、Sodium phenate、1-sodium butane sulfonate、1-propane sodium mercaptides、1-dodecane sulfonic acid sodium、1-sodium nonanesulfonate、1-sodium heptanesulfonate、1-decane sulfonate、2-propane sodium mercaptides、2-sodium naphthalene sulfonate、Disodium succinate、Sodium succinate、Sodium Pyruvate、Sodium propionate、Sodium xylene sulfonate、Sodium lauryl sulphate、The organic compound such as sodium tert-butoxide.The source of the metallic sodium element pointed by the present invention is not limited only to the example above, no matter uses the compounds containing sodium of which kind of form, and atomic emission spectrometry can be used to detect.The weight content of metallic sodium element is by metallic sodium element itself rather than on the basis of the compounds containing sodium adding metallic sodium element.The weight content of the metallic sodium element represented by ppm is to calculate on the basis of the gross weight of liquid-crystalline polyester composition.
nullWherein titanium-containing compound can be selected from Barium metatitanate.、Iron titanate (II)、Aluminium titanates、Lithium titanate、Zinc titanate、Metatitanic acid sodium salt、Titanium oxide (II)、Titanium oxide (IV)、Silicon titanium oxide、Titanium carbide (IV)、Titanium disulfide、Ammonium hexa-fluorotitanate、Ten dichloro Tritanium/Trititanium aluminum、Titanium tetrafluoride、Titanium fluoride (III)、Titanium carbonitride、The inorganic compound such as ammonium titanyl oxalate monohydrate，Titanium ethanolate can also be selected、Titanyl phthalocyanine、Poly(tributoxy titanium)、2-ethyl-1-hexanol titanium、Trichlorine one cyclopentadienyl titanium、Acetylacetone,2,4-pentanedione oxygen titanium (IV)、Double (levulinic ketone group) diisopropyl titanate esters、Double (cyclopentadienyl group) titanium chloride (IV)、Tert-butyl alcohol titanium、Four (dimethyl amido) titanium (IV)、Titanium tetraisopropylate、Four methanol titaniums (IV)、Normal propyl alcohol titanium、Three isopropoxy titanium chlorides、Dichloro two indenyl titanium、Butyl titanate、Four (ethyl-methyl amido) titanium (IV)、The organic compound such as four (diethyl amido) titanium (IV).The source of the Titanium element pointed by the present invention is not limited only to the example above, no matter uses the titanium-containing compound of which kind of form, and atomic emission spectrometry can be used to detect.The weight content of Titanium element is by Titanium element itself rather than on the basis of the titanium-containing compound adding Titanium element.The weight content of the Titanium element represented by ppm is to calculate on the basis of the gross weight of liquid-crystalline polyester composition.
nullThe products formed that the liquid-crystalline polyester composition that the present invention is obtained is formed can have following application，With various gears、Various housings、Sensor、LED lamp、Adapter、Socket、Resistor、Casing of relay、Relay base、Relay roll、Switch、Coil axle、Capacitor、Variable condenser housing、Optical pickup unit、Resonator、Various terminal boards、Transformator、Plug、Printed wiring board、Tuner、Speaker、Microphone、Head type headphones、Miniature motor、Magnetic head base、Power model、Shell、Quasiconductor、Liquid crystal display component、FDD bracket、FDD chassis、HDD parts、Motor brush holder、Parabola antenna、The electrical and electronic parts that computer associated components etc. are representative、With VTR parts、TV part、Flatiron、Hair dryer、Electric cooker parts、Microwave oven component、Sound part、Audio frequency、Laser disk、The speech ciphering equipment parts such as CD、Illuminace component、Parts of refrigerator、Air supply rate、Typewriter parts、The family that word processor parts etc. are representative、Enterprise's electric product parts、Office computer associated components、Telephone set associated components、Facsimile machine associated components、Photocopier associated components、Washing fixture、Oilless bearing、Stern bearing、The various bearings such as water middle (center) bearing、Motor component、With lighter、The mechanical associated components that typewriter etc. are representative、With microscope、Binoculars、Photographing unit、The optical device that clock and watch etc. are representative、Precision optical machinery associated components；nullAlternating current generator terminal、Alternating current generator adapter、IC actuator、Dimmer potentiometer base、The various valves such as aerofluxus air valve、Fuel associates、Exhaust system、The various pipes of air-breathing system、Inlet jet breather、Inlet manifold、Petrolift、Engine cool water swivel、Carburator main body、Carburator spacer、Exhaust gas sensor、Cooling water sensor、Oil temperature sensor、TPS、Crankshaft position sensor、Mass air flow sensor、Brake pad abrasion sensor、Idle call thermostat base、Air conditioning electricity motivation insulator、The on-vehicle motor insulators such as motorized window、Warmer heated airflow control valve、Radiator fan motor brush carrier、Water pump vane、Turbo blade、Wiper motor associated components、Ignition distributor、Starter switch、Starter relay、Actuating device wire harness、Window cleaning device nozzle、Air-conditioning panel switch substrate、Fuel association electromagnetic valve coil、Electric fuse adapter、Loudspeaker terminal、Parts of electric insulation board、Stepping motor rotor、Lamp ring、Lamp socket、Lamp reflector、Lamp housing、Brake piston、Solenoid bobbin、Engine oil filter、The automobiles such as ignition housings、Vehicle associated components etc.，At printed wiring board，In small-sized thin-walled electronic device etc. particularly useful.
The present invention compared with prior art, has the advantages that
When the present invention is 1ppm-800ppm by selecting the weight content gross weight based on liquid-crystalline polyester composition adding metallic sodium element in liquid-crystalline polyester composition formula, the hot strength of the liquid-crystalline polyester composition obtained is obviously improved, and high-temperature heat-resistance stability obtains beyond thought significantly improving.
Detailed description of the invention
Further illustrating the present invention below by detailed description of the invention, following example are the present invention preferably embodiment, but embodiments of the present invention are not limited by following embodiment.
The method of testing of the weight content of described metallic sodium element: be dried 4 hours at 120 DEG C by liquid-crystalline polyester composition, takes the pending sample of 1g, adds nitric acid and hydrogen peroxide, heats 2 hours, and period is continuously added nitric acid and hydrogen peroxide；After having cleared up of sample, cancelling the sample after solution, the full-automatic inductively coupled plasma atomic emission spectrometer using Agilent company model to be 720ES is analyzed Gold Samples and is belonged to the weight content of sodium element.
The method of testing of the weight content of described Titanium element: be dried 4 hours at 120 DEG C by liquid-crystalline polyester composition, takes the pending sample of 1g, adds nitric acid and hydrogen peroxide, heats 2 hours, and period is continuously added nitric acid and hydrogen peroxide；After having cleared up of sample, cancelling the sample after solution, the full-automatic inductively coupled plasma atomic emission spectrometer using Agilent company model to be 720ES is analyzed Gold Samples and is belonged to the weight content of titanium elements.
The method of testing of the fusing point of described liquid-crystalline polyester composition: by NETZSCH company DSC
200 F3 type differential scanning calorimeter (DSC), are starting to test with the Elevated Temperature Conditions of 20 DEG C/min from room temperature, are observing endotherm peak temperature Tm1After, than Tm1Keep 5 minutes at a temperature of high 20 DEG C, then under the cooling conditions of 20 DEG C/min, be cooled to room temperature, be the most again measured with the Elevated Temperature Conditions of 20 DEG C/min, the endotherm peak temperature T now observedm2Fusing point for liquid-crystalline polyester composition.
The method of testing of the hot strength of described liquid-crystalline polyester composition: liquid-crystal composition is molded into No. 4 dumbbell shape samples of ASTM, then according to the hot strength of ASTM D638 standard testing compositions.
Deflection temperature (HDT) method of testing under described liquid-crystalline polyester composition load: liquid-crystalline polyester composition injection is made long 127
Mm, wide 12.7 mm and thick 6.4
The sample of mm, then according to ASTM D648 measures under the load of 1.82MPa.
Title and the abbreviation of the monomer that the repetitive that contains of liquid crystal polyester that uses in the present invention is corresponding are as follows:
4-HBA (HBA)；
4,4 '-dihydroxybiphenyl (BP)；
P-phthalic acid (TA)；
M-phthalic acid (IA)；
2-hydroxyl-6-naphthoic acid (HNA)；
Hydroquinone (HQ)；
2,6-naphthalenedicarboxylic acid (NDA)；
The compounds containing sodium used in the present invention:
Sodium acetate: Sigma-Aldrich (Shanghai) trade Co., Ltd；
Sodium sulfate: Sigma-Aldrich (Shanghai) trade Co., Ltd；
Sodium tert-butoxide: Sigma-Aldrich (Shanghai) trade Co., Ltd；
Biphenyl sodium: Sigma-Aldrich (Shanghai) trade Co., Ltd；
The titanium-containing compound used in the present invention:
Titanium oxide (IV): Sigma-Aldrich (Shanghai) trade Co., Ltd；
The glass fibre used in the present invention: trade mark CS03JAPX-1, number equal fibre diameter 10 microns, the equal draw ratio 300 of number, number average fiber length 3000 microns, Asahi Fiber
Glass Co., Ltd。
Embodiment
A1-A4:
The preparation of liquid crystal polyester
In the reactor being equipped with agitator, thermometer, nitrogen ingress pipe and reflux condensate device, it is separately added into the repetitive derived from aromatic hydroxy-carboxylic, the repetitive derived from aromatic diol and the repetitive derived from aromatic dicarboxylic acid according to proportioning, and to add a certain proportion of acetic anhydride be acylating agent；Then nitrogen is passed through in reactor and replaces；Start stirring, in nitrogen stream, reactant mixture is heated to 140 DEG C-160 DEG C by room temperature, at this temperature backflow 1 hour-3 hours；Hereafter continue to heat up, mixture was heated to 300 DEG C-350 DEG C through 2 hours-4 hours from 140 DEG C-160 DEG C, steams unreacted acetic anhydride and side reaction product acetic acid in the process；Whole polycondensation phase, reduces pressure to reaction system, and the endpoint terminated as reaction by observing moment of torsion to raise；Now the prepolymer of melt state is discharged through drain hole, and be cooled to room temperature；Prepolymer being transferred to solid phase device further, through 5 hours-7 hours, temperature from ambient is increased to 260 DEG C-280 DEG C, insulation carries out solid-phase polymerization in 9 hours-11 hours at this temperature；Product is derived after terminating by reaction, thus obtains liquid crystal polyester.
The concrete proportioning of table 1 embodiment A1-A4 and test performance result thereof
Embodiment
1-14
And comparative example
1-6
: the preparation of liquid-crystalline polyester composition
After gained liquid crystal polyester, filler, compounds containing sodium and/or titanium-containing compound and/or various additive high-speed mixer mix homogeneously being prepared by embodiment A1-A4 by the proportioning of table 2, add double screw extruder, melting mixing under the screw speed of 280RPM-320RPM, barrel temperature is 290 DEG C-355 DEG C, extrusion, cooling, pelletizing, obtain liquid-crystalline polyester composition.The fusing point of gained liquid-crystalline polyester composition, hot strength and HDT are shown in Table 2；
Wherein, the metallic sodium element in liquid-crystalline polyester composition, Titanium constituent content are to be adjusted by the actual addition of compounds containing sodium, titanium-containing compound and recorded in the preparation process of liquid-crystalline polyester composition.
Table 2
Continued 2
Continued 2
From the embodiment 1 of table 2-14 and comparative example 1-6 relatively can be seen that, when the present invention is 1ppm-800ppm by selecting the weight content gross weight based on liquid-crystalline polyester composition adding metallic sodium element in liquid-crystalline polyester composition formula, the hot strength of the liquid-crystalline polyester composition obtained is obviously improved, and high-temperature heat-resistance stability obtains beyond thought significantly improving.
Claims (13)
1. a liquid-crystalline polyester composition, it is characterised in that gross weight based on liquid-crystalline polyester composition, the weight content of metallic sodium element is 1ppm-800ppm.
Liquid-crystalline polyester composition the most according to claim 1, it is characterised in that the method for testing of the weight content of metallic sodium element: liquid-crystalline polyester composition is dried 4 hours at 120 DEG C, take the pending sample of 1g, adding nitric acid and hydrogen peroxide, heat 2 hours, period is continuously added nitric acid and hydrogen peroxide；After having cleared up of sample, cancelling the sample after solution, the full-automatic inductively coupled plasma atomic emission spectrometer using Agilent company model to be 720ES is analyzed Gold Samples and is belonged to the weight content of sodium element.
Liquid-crystalline polyester composition the most according to claim 1, it is characterised in that gross weight based on liquid-crystalline polyester composition, the weight content of metallic sodium element is preferably 5ppm-500ppm, more preferably 10ppm-300ppm.
Liquid-crystalline polyester composition the most according to claim 1, it is characterised in that also include Titanium element, gross weight based on liquid-crystalline polyester composition, the weight content of Titanium element is 1ppm-800ppm, preferably 10ppm-500ppm.
Liquid-crystalline polyester composition the most according to claim 4, it is characterised in that the method for testing of the weight content of Titanium element: liquid-crystalline polyester composition is dried 4 hours at 120 DEG C, take the pending sample of 1g, adding nitric acid and hydrogen peroxide, heat 2 hours, period is continuously added nitric acid and hydrogen peroxide；After having cleared up of sample, cancelling the sample after solution, the full-automatic inductively coupled plasma atomic emission spectrometer using Agilent company model to be 720ES is analyzed Gold Samples and is belonged to the weight content of titanium elements.
6. according to the liquid-crystalline polyester composition described in any one of claim 1-5, it is characterised in that described liquid-crystalline polyester composition, by weight, including following component:
Liquid crystal polyester 100 parts；
Filler 5 parts-100 parts.
Liquid-crystalline polyester composition the most according to claim 6, it is characterised in that the fusing point of described liquid-crystalline polyester composition is 150 DEG C-400 DEG C；The method of testing of described fusing point is: by NETZSCH company DSC 200 F3 type differential scanning calorimeter DSC, is starting to test with the Elevated Temperature Conditions of 20 DEG C/min from room temperature, is observing endotherm peak temperature Tm1After, than Tm1Keep 5 minutes at a temperature of high 20 DEG C, then under the cooling conditions of 20 DEG C/min, be cooled to room temperature, be the most again measured with the Elevated Temperature Conditions of 20 DEG C/min, the endotherm peak temperature T now observedm2It is the fusing point of liquid-crystalline polyester composition.
Liquid-crystalline polyester composition the most according to claim 6, it is characterised in that described liquid crystal polyester, by mole meter, comprises following repetitive:
Repetitive 30mol%-100mol% derived from aromatic hydroxy-carboxylic；
Repetitive derived from aromatic diol
0mol%-35mol%；
Repetitive 0mol%-35mol% derived from aromatic dicarboxylic acid.
Liquid-crystalline polyester composition the most according to claim 8, it is characterised in that described liquid crystal polyester, by mole meter, including following repetitive:
Repetitive 50mol%-100mol% derived from aromatic hydroxy-carboxylic；
Repetitive 0mol%-25mol% derived from aromatic diol；
Repetitive 0mol%-25mol% derived from aromatic dicarboxylic acid.
Liquid-crystalline polyester composition the most according to claim 8 or claim 9, it is characterised in that the described repetitive derived from aromatic hydroxy-carboxylic is selected from the repetitive derived from 4-HBA and/or the repetitive of 2-hydroxyl-6-naphthoic acid；The described repetitive derived from aromatic diol is selected from repetitive and/or the repetitive of 4,4 '-dihydroxybiphenyl of hydroquinone；The described repetitive derived from aromatic dicarboxylic acid is selected from the repetitive of the repetitive of p-phthalic acid, the repetitive of M-phthalic acid, 2,6-naphthalenedicarboxylic acid one or more.
11. liquid-crystalline polyester compositions according to claim 6, it is characterised in that described filler is selected from fibrous filler and/or tabular filler；One or more in glass fibre, asbestos fibre, silicon dioxide fibre, silica-alumina fiber, potassium titanate fibre, carbon or graphite fibre, metallic fiber of described fibrous filler；It is preferably glass fibre；One or more in Talcum, Muscovitum, graphite, Kaolin of described tabular filler；It is preferably Muscovitum.
12. liquid-crystalline polyester compositions according to claim 11, it is characterised in that the equal fibre diameter of number of described glass fibre is 3 microns-30 microns, the equal draw ratio of number is more than or equal to 5, and number average fiber length is 50 microns-3000 microns；The mean diameter of described Muscovitum is 0.5 micron-200 microns.
13. liquid-crystalline polyester compositions according to claim 6, it is characterised in that also comprise various additive；One or more in plasticizer, stabilizer, coloring agent, lubricant, releasing agent, antioxidant of described various additive.
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Application publication date: 20160810 |