CN116102723A - 一种液晶聚酯及其制备方法和一种液晶聚酯组合物 - Google Patents
一种液晶聚酯及其制备方法和一种液晶聚酯组合物 Download PDFInfo
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- CN116102723A CN116102723A CN202211671685.3A CN202211671685A CN116102723A CN 116102723 A CN116102723 A CN 116102723A CN 202211671685 A CN202211671685 A CN 202211671685A CN 116102723 A CN116102723 A CN 116102723A
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- 229920000728 polyester Polymers 0.000 title claims abstract description 65
- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 35
- 239000000203 mixture Substances 0.000 title claims description 21
- 238000002360 preparation method Methods 0.000 title description 9
- 230000014759 maintenance of location Effects 0.000 claims abstract description 31
- 239000000178 monomer Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000000835 fiber Substances 0.000 claims description 20
- 238000006068 polycondensation reaction Methods 0.000 claims description 15
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 239000012763 reinforcing filler Substances 0.000 claims description 8
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 125000004957 naphthylene group Chemical group 0.000 claims description 6
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
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- IJFXRHURBJZNAO-UHFFFAOYSA-N 3-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC(O)=C1 IJFXRHURBJZNAO-UHFFFAOYSA-N 0.000 claims description 4
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000010425 asbestos Substances 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
- 239000011324 bead Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 4
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 4
- 239000010440 gypsum Substances 0.000 claims description 4
- 229910052602 gypsum Inorganic materials 0.000 claims description 4
- 239000012779 reinforcing material Substances 0.000 claims description 4
- 229910052895 riebeckite Inorganic materials 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 3
- 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
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000021736 acetylation Effects 0.000 claims description 3
- 238000006640 acetylation reaction Methods 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
- 125000002529 biphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C12)* 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
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- 229910052751 metal Inorganic materials 0.000 claims description 3
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- 229960005489 paracetamol Drugs 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- SJJCQDRGABAVBB-UHFFFAOYSA-N 1-hydroxy-2-naphthoic acid Chemical compound C1=CC=CC2=C(O)C(C(=O)O)=CC=C21 SJJCQDRGABAVBB-UHFFFAOYSA-N 0.000 claims description 2
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 claims description 2
- LODHFNUFVRVKTH-ZHACJKMWSA-N 2-hydroxy-n'-[(e)-3-phenylprop-2-enoyl]benzohydrazide Chemical compound OC1=CC=CC=C1C(=O)NNC(=O)\C=C\C1=CC=CC=C1 LODHFNUFVRVKTH-ZHACJKMWSA-N 0.000 claims description 2
- ALKYHXVLJMQRLQ-UHFFFAOYSA-N 3-Hydroxy-2-naphthoate Chemical compound C1=CC=C2C=C(O)C(C(=O)O)=CC2=C1 ALKYHXVLJMQRLQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N Salicylic acid Natural products OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910052570 clay Inorganic materials 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 2
- 239000010459 dolomite Substances 0.000 claims description 2
- 229910000514 dolomite Inorganic materials 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 claims description 2
- 229910000271 hectorite Inorganic materials 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
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 2
- FCQGSMZDIIILCP-UHFFFAOYSA-N n-(6-hydroxynaphthalen-2-yl)acetamide Chemical compound C1=C(O)C=CC2=CC(NC(=O)C)=CC=C21 FCQGSMZDIIILCP-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 2
- NEQFBGHQPUXOFH-UHFFFAOYSA-N 4-(4-carboxyphenyl)benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=CC=C(C(O)=O)C=C1 NEQFBGHQPUXOFH-UHFFFAOYSA-N 0.000 claims 1
- 239000000454 talc Substances 0.000 claims 1
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- 239000000463 material Substances 0.000 abstract description 17
- 229920000106 Liquid crystal polymer Polymers 0.000 abstract description 12
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 abstract description 12
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 8
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- PQAMFDRRWURCFQ-UHFFFAOYSA-N 2-ethyl-1h-imidazole Chemical compound CCC1=NC=CN1 PQAMFDRRWURCFQ-UHFFFAOYSA-N 0.000 description 1
- TVPCUVQDVRZTAL-UHFFFAOYSA-N 2-ethylhexanoyl 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OC(=O)C(CC)CCCC TVPCUVQDVRZTAL-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- NJQHZENQKNIRSY-UHFFFAOYSA-N 5-ethyl-1h-imidazole Chemical compound CCC1=CNC=N1 NJQHZENQKNIRSY-UHFFFAOYSA-N 0.000 description 1
- 108010053481 Antifreeze Proteins Proteins 0.000 description 1
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHASWHZGWUONAO-UHFFFAOYSA-N butanoyl butanoate Chemical compound CCCC(=O)OC(=O)CCC YHASWHZGWUONAO-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- DUCKXCGALKOSJF-UHFFFAOYSA-N pentanoyl pentanoate Chemical compound CCCCC(=O)OC(=O)CCCC DUCKXCGALKOSJF-UHFFFAOYSA-N 0.000 description 1
- 229940094537 polyester-10 Drugs 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- WYVAMUWZEOHJOQ-UHFFFAOYSA-N propionic anhydride Chemical compound CCC(=O)OC(=O)CC WYVAMUWZEOHJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000012797 qualification Methods 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
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/685—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
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Abstract
本发明公开了一种液晶聚酯,以摩尔含量计,包括以下重复单元构成:‑O‑Ar1‑CO‑单元45‑56mol%;‑O‑Ar2‑CO‑单元9‑20mol%;‑CO‑Ar3‑CO‑单元10‑19 mol%;‑O‑Ar4‑O‑单元10‑19mol%;‑Y‑Ar5‑O‑单元0.5‑8mol%。本发明的液晶聚酯具有独特的重复单元结构,使其能够在聚合成为分子链段规整性良好且晶格堆砌紧密的液晶聚合物,其热滞留重量保持率>97.5%,表现出优异的回流焊后尺寸稳定性。热滞留重量保持率能够表征液晶聚合物材料加工与成型过程材料热稳定性能,反映出晶体活动与链间酯交换难易程度,热滞留重量保持率高的材料表现出较低的收缩率,制件经回流焊后的尺寸稳定性优异。
Description
技术领域
本发明涉及高分子材料技术领域,特别是涉及一种液晶聚酯及其制备方法和一种液晶聚酯组合物。
背景技术
近年来,电子元件不断往密集化、微型化以及高密度化的发展,行业对薄壁制件需求量大。液晶聚合物(LCP)是一种各向异性的、由刚性分子链段构成、且分子链段规整取向排布的芳香族高分子材料,这种微观结构决定材料具有高流动性、高耐热、优良的机械性能、自阻燃性等性能。因此,行业内在成型薄壁制件上,大多数通过采用高流动性的液晶聚合物(LCP)材料的技术方案。
在电子材料应用中,需将电子元件直接安装到印刷电路板表面,行业普遍采用表面贴装技术(SMT),为适应环保要求,SMT技术发展成为采用的无铅回流焊,焊接工艺中温度进一步提高至回流焊加工温度下,材料容易出现形变进而引起基材表面不均匀,导致出现虚焊异常,造成接触不良与运行通电通断状态不稳定。虚焊问题导致应用制件合格率降低,制件厂需在产品质量监控方面需投入大量人力资源,导致生产效率与产品质量下降。虚焊是导致电路可靠性下降的主要原因,一旦漏检或未检测出不合格制件并流出,将给下游电子整机产品的调试、使用和维护带来重大使用甚至安全隐患。因此,行业迫切需要提高表面贴装技术,并要求材料必须在回流焊高温条件下具备良好的尺寸稳定性,改善产品的高温变形问题,解决电路虚焊问题。
液晶聚合物材料的热稳定性能受分子链段断裂难易程度、晶体堆砌紧密情况影响,可以通过恒温热滞留下的重量保持率来反映。
发明内容
本发明的目的在于,提供一种恒温热滞留下的重量保持率大于97.5%的液晶聚酯,及其制备方法和一种液晶聚酯组合物。
本发明是通过以下技术方案实现的:
一种液晶聚酯,以摩尔含量计,包括以下重复单元构成:
其中,Ar1表示亚苯基;Ar2表示亚萘基;Ar3和Ar4分别独立表示亚苯基、亚萘基或亚联苯基中的至少一种;Ar5表示亚苯基、亚萘基或亚联苯基中的至少一种,Y为-NH-或-NR,其中R为芳基基团或包含1-6个碳的烷基基团中的至少一种;
所述的液晶聚酯的热滞留重量保持率≥97.5%。
优选的,以摩尔含量计,包括以下重复单元构成:
其中,-O-Ar1-CO-单元衍生自4-羟基苯甲酸、3-羟基苯甲酸、2-羟基苯甲酸中的至少一种;-O-Ar2-CO-单元衍生自2-羟基-6-萘甲酸、3-羟基-2-萘甲酸、1-羟基-2萘甲酸中的至少一种;-CO-Ar3-CO-单元衍生自对苯二甲酸、间苯二甲酸、2,6萘二甲酸、4,4’-联苯二甲酸中的至少一种;-O-Ar4-O-单元衍生自4,4’-二羟基联苯、对苯二酚、2,6-萘二酚中的至少一种;-Y-Ar5-O-单元衍生自4-乙酰氨基酚、对氨基苯酚、4’-氨基-4-联苯酚、6-乙酰氨基-2-萘酚中的至少一种。
所述的液晶聚酯的熔融粘度为10-50Pa.s。
优选的,所述的液晶聚酯的热滞留重量保持率≥98.5%。
热滞留重量保持率通常用于表征液晶聚合物材料加工与成型过程材料热稳定性能,反映出晶体活动与链间酯交换难易程度,热滞留重量保持率高的材料表现出优异的抗起泡性。
本发明液晶聚酯的制备方法,包括以下步骤:
(1)乙酰化工段:-O-Ar1-CO-单元的单体、-O-Ar2-CO-单元的单体、-O-Ar4-O-单元的单体和-Y-Ar5-O-单元分别对应的单体同时投入第一反应器中,在100-160℃温度下反应0.5-5h;
优选的制备工艺为,将-O-Ar2-CO-单元、-O-Ar4-O-单元和-Y-Ar5-O-单元分别对应的单体、酰化剂、催化剂、30-60wt%的-O-Ar1-CO-单元的单体同时投入第一反应器中,在100-160℃温度下反应0.5-5h,其中反应2-4h后开始补加剩余的-O-Ar1-CO-单元单体;
酰化剂可以是乙酸酐、丙酸酐、丁酸酐、戊酸酐、2-乙基己酸酐、二氯乙酸酐或二氟乙酸酐中的至少一种。
催化剂可以是离子液体作为催化剂。离子液体催化剂是由阳离子化合物与阴离子化合物反应得到。阳离子化合物可以是含有两个或两个以上氮原子的杂环有机碱类化合物为咪唑化合物、三唑化合物或二吡啶基化合物,所述咪唑化合物为1-甲基咪唑、2-甲基咪唑、4-甲基咪唑、1-乙基咪唑、2-乙基咪唑、4-乙基咪唑、1,2-二甲基咪唑、1,4-二甲基咪唑或2,4-二甲基咪唑,优选为1-甲基咪唑。阴离子化合物可以是乙酸、丙酸或丁酸等有机羧酸,优选为乙酸。
离子液体催化剂的制备方法为:阳离子化合物与阴离子化合物在80℃搅拌反应24小时。
(2)缩聚工段:把乙酰化后的反应物转入第二反应器中,与-CO-Ar3-CO-单元对应的单体进行熔融缩聚,以0.3-1.5℃/min升温速率升温至275-285℃后,特别地,为确保分子链段有序性,需促进对称单体充分参与反应,控制升温速率使在280-300℃升温段的升温时间保持在1-3h,最后继续采用0.3-1.5℃/min升温速率升温至熔点以上10~30℃,升温期间不断馏出醋酸及其副产物;
(3)减压缩聚工段:通过对第二反应器进行减压缩聚,目标真空度为0.1kPa~40kPa,减压缩聚时间控制在3小时以内,最终控制排出时预聚物熔体的温度为至熔点以上10~30℃;达到目标搅拌功率后,在熔融状态下排出熔体,冷却后进行切割或粉碎,得到的液晶聚酯。
一种液晶聚酯组合物,按重量份计,包括以下组分:
本发明的液晶聚酯45-78份;
增强材料22-55份;
所述的增强材料选自纤维状增强填料、颗粒状增强填料中的至少一种;
所述的液晶聚酯组合物的热滞留重量保持率≥98.5%。
所述的纤维状增强填料选自玻璃纤维、钛酸钾纤维、陶瓷纤维、硅灰石纤维、金属碳化物纤维、金属固化纤维、石棉纤维、氧化铝纤维、碳化硅纤维、石膏纤维、硼纤维中的至少一种。
所述的颗粒状增强填料选自钛酸钾晶须、硼酸铝晶须、滑石粉、炭黑、石膏、石棉、沸石、高岭土、蒙脱土、粘土、锂蒙脱土、合成云母、硅铝酸盐、二氧化硅、氧化钛、氧化铝、氧化锌、氧化锆、氧化铁、碳酸钙、钛酸镁、白云石、硫酸铝、硫酸钡、硫酸镁、云母、石英粉、氢氧化镁、氢氧化钙、氢氧化铝、玻璃珠、陶瓷珠、氮化硼、碳化硅中的至少一种。
本发明具有如下有益效果
本发明的液晶聚酯具有独特的重复单元结构,使其能够在聚合成为分子链段规整性良好且晶格堆砌紧密的液晶聚合物,其热滞留重量保持率>97.5%,液晶聚酯组合物的热滞留重量保持率>98.5%,在高温加工下表现出优异的高温加工下的尺寸稳定性。进一步通过在酰基化反应中分批次加入-O-Ar1-CO-单元单体,降低芳香族羟基羧酸的自聚引发的高温易分解,实现热滞留重量保持率的进一步提升。
热滞留重量保持率能够表征液晶聚合物材料加工与成型过程材料热稳定性能,反映出晶体活动与链间酯交换难易程度,热滞留重量保持率高的材料表现出优异的经回流焊后尺寸稳定性。在本领域各厂家的要求中,适用于制备SMT封装的制件的液晶聚酯组合物。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
本发明所用原料来源如下:
本发明所用单体来源于市售产品。
4-羟基苯甲酸,Sigma-Aldrich公司,纯度>99%;
6-羟基-2-萘甲酸,Sigma-Aldrich公司,纯度>99%;
对苯二甲酸,Sigma-Aldrich公司,纯度>99%;
4,4'-二羟基联苯,Sigma-Aldrich公司,纯度>99%;
间苯二甲酸,Sigma-Aldrich公司,纯度>99%;
乙酰氨基酚,Sigma-Aldrich公司,纯度>99%;
玻璃纤维:欧文斯科宁;
滑石粉:青岛凯威尔粉体工程科技公司。
实施例和对比例液晶聚酯的制备方法:乙酰化工段:将重复单元Ar1、Ar2、Ar4、Ar5的单体(其中,-O-Ar1-CO-的单体的添加量与补充量见表1)、酰化剂(乙酸酐)、催化剂(1-甲基咪唑/乙酸离子液体)同时投入第一反应器中,在100-160℃温度下反应0.5-5h,其中反应2-4h后开始补加剩余的-O-Ar1-CO-单元单体(如-O-Ar1-CO-单体的初始添加量为100%,则无需补加),让单体充分乙酰化;缩聚工段:把乙酰化后的反应物转入第二反应器中,与对苯二甲酸和/或间苯二甲酸单体进行熔融缩聚,以0.3-1.5℃/min升温速率升温至275-285℃后,控制升温速率使在280-300℃升温段的升温时间保持在1-3h,最后继续采用0.3-1.5℃/min升温速率升温至熔点以上10~30℃,升温期间不断馏出醋酸及其副产物;减压缩聚工段:通过对第二反应器进行减压缩聚,目标真空度为0.1kPa~40kPa,减压缩聚时间控制在3小时以内,最终控制排出时预聚物熔体的温度为至熔点以上10~30℃;达到目标搅拌功率后,在熔融状态下排出熔体,冷却后进行切割或粉碎,得到的液晶聚酯。
其中,离子液体催化剂的制备方法为:咪唑化合物与乙酸在80℃搅拌反应24小时。所述咪唑化合物优选为1-甲基咪唑,反应制备得到1-甲基咪唑乙酸盐离子液体。
实施例和对比例液晶聚酯组合物的制备方法:将液晶聚合物、玻璃纤维或滑石粉混合均匀,通过双螺杆挤出机挤出造粒螺杆最高温度设置比树脂熔点高5~30℃,转速为100-500rpm,得到液晶聚酯组合物。
各项测试方法:
(1)熔融粘度通过以下方法测得:采用Dynisco LCR7000型毛细管流变仪测试,测试温度在熔融温度以上20℃,剪切速率1000S-1,使用内径1mm、长度40mm的口模,预热4min测得数据。
(2)热滞留重量保持率:用(热失重分析仪)TGA测定,测试气氛为氮气,将试样以20℃/min升温至150℃,并在150℃恒温保持10min,再以20℃/min升温至400℃,在400℃恒温保持30min,测试温度达到400℃开始计时,计时0min记录重量G0,计时30min记录重量G30。滞留重量保持率=G30/G0*100%。
(3)高温尺寸稳定性:将液晶聚酯组合物注塑成型直径为100mm、厚度为1.5mm的圆板。将圆板放置在水平桌面上,测量圆板表面离桌面之间的距离,选取两个距离最大点(A,B)和两个最小点(C,D),翘曲变形(w)按如下公式计算:w=(A+B)/2-(C+D)/2。取5次测试结果的平均值为形变尺寸,然后将该5个样品其通过260℃等级的回流焊炉工艺,再次重复此测试过程,取结果平均值。以经过回流焊工艺前后的结果之差为材料高温后变形量,变形量越小,表示测试片条的抗翘曲性能越好高温尺寸稳定性越好。
表1:液晶聚酯1(实施例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯2(实施例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯3(实施例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯4(实施例),其中其初始-O-Ar1-CO-单元单体添加量为50wt%:
续表1:液晶聚酯5(实施例),其中其初始-O-Ar1-CO-单元单体添加量为45wt%:
续表1:液晶聚酯6(实施例),其中其初始-O-Ar1-CO-单元单体添加量为40wt%:
续表1:液晶聚酯7(实施例),其中其初始-O-Ar1-CO-单元单体添加量为60wt%:
续表1:液晶聚酯8(实施例),其中其初始-O-Ar1-CO-单元单体添加量为100wt%:
续表1:液晶聚酯9(实施例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯10(实施例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯11(实施例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯12(对比例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯13(对比例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯14(对比例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯15(对比例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
续表1:液晶聚酯16(对比例),其中其初始-O-Ar1-CO-单元单体添加量为30wt%:
由表1可知,优选重复单元的液晶聚酯的热滞留重量保持率更高。
表2:实施例和对比例液晶聚酯组合物各组分含量(重量份)及测试结果
由实施例8可知,优选通过在酰化反应前加入30-60wt%的-Y-Ar5-O-单体反应2-4小时后再补加剩余的单体,能够降低芳香族羟基羧酸的自聚引发的高温易分解,实现热滞留重量保持率的进一步提升
表2:实施例和对比例液晶聚酯组合物各组分含量(重量份)及测试结果
由表2可知,采用本发明申请的液晶聚酯形成的组合物的热滞留保持率(>98.5%),明显高于现有的液晶聚酯组合物(对比例1-5),经SMT加工后形变量小,高温下尺寸稳定性更好。
Claims (9)
1.一种液晶聚酯,其特征在于,以摩尔含量计,包括以下重复单元构成:
-O-Ar1-CO-单元 45-56mol%;
-O-Ar2-CO-单元 9-20mol%;
-CO-Ar3-CO-单元 10-19 mol%;
-O-Ar4-O-单元 10-19mol%;
-Y-Ar5-O-单元 0.5-8mol%;
其中,Ar1表示亚苯基;Ar2表示亚萘基;Ar3和Ar4分别独立表示亚苯基、亚萘基或亚联苯基中的至少一种;Ar5表示亚苯基、亚萘基或亚联苯基中的至少一种,Y为 -NH-或-NR,其中R为芳基基团或包含1-6个碳的烷基基团中的至少一种;
所述的液晶聚酯的热滞留重量保持率>97.5%。
2.根据权利要求1所述的液晶聚酯,其特征在于,以摩尔含量计,包括以下重复单元构成:
-O-Ar1-CO-单元 48-56mol%;
-O-Ar2-CO-单元 11-18mol%;
-CO-Ar3-CO-单元 13-18mol%;
-O-Ar4-O-单元 13-18mol%;
-Y-Ar5-O-单元 0.5-6mol%。
3.根据权利要求1或2所述的液晶聚酯,其特征在于,-O-Ar1-CO-单元衍生自4-羟基苯甲酸、3-羟基苯甲酸或2-羟基苯甲酸中的至少一种;-O-Ar2-CO-单元衍生自2-羟基-6-萘甲酸、3-羟基-2-萘甲酸或1-羟基-2萘甲酸中的至少一种;-CO-Ar3-CO-单元衍生自对苯二甲酸、间苯二甲酸、2,6萘二甲酸或4,4’-联苯二甲酸中的至少一种;-O-Ar4-O-单元衍生自4,4’-二羟基联苯、对苯二酚或2,6-萘二酚中的至少一种;-Y-Ar5-O-单元衍生自4-乙酰氨基酚、对氨基苯酚、4’-氨基-4-联苯酚或6-乙酰氨基-2-萘酚中的至少一种。
4.根据权利要求1所述的液晶聚酯,其特征在于,所述的液晶聚酯的热滞留重量保持率≥98.5%。
5.根据权利要求1所述的液晶聚酯,其特征在于,所述的液晶聚酯的熔融粘度为10-50Pa.s。
6.权利要求1-5任一项所述液晶聚酯的制备方法,其特征在于,包括以下步骤:
(1)乙酰化工段:将-O-Ar2-CO-单元、-O-Ar4-O-单元和-Y-Ar5-O-单元分别对应的单体、酰化剂、催化剂、30-60wt%的-O-Ar1-CO-单元的单体同时投入第一反应器中,在100-160℃温度下反应0.5-5h,其中反应2-4h后开始补加剩余的-O-Ar1-CO-单元单体;
(2)缩聚工段:把乙酰化后的反应物转入第二反应器中,与-CO-Ar3-CO-单元对应的单体进行熔融缩聚,以0.3-1.5℃/min升温速率升温至275-285℃后;控制升温速率使在280-300℃升温段的升温时间保持在1-3h,最后继续采用0.3-1.5℃/min升温速率升温至熔点以上10~30℃,升温期间不断馏出醋酸及其副产物;
(3)减压缩聚工段:通过对第二反应器进行减压缩聚,目标真空度为0.1kPa~40kPa,减压缩聚时间控制在3小时以内,最终控制排出时预聚物熔体的温度为至熔点以上10~30℃;达到目标搅拌功率后,在熔融状态下排出熔体,冷却后进行切割或粉碎,得到的液晶聚酯。
7.一种液晶聚酯组合物,其特征在于,按重量份计,包括以下组分:
权利要求1-6任一项所述的液晶聚酯 45-78份;
增强材料 22-55份;
所述的增强材料选自纤维状增强填料、颗粒状增强填料中的至少一种;
所述的液晶聚酯组合物的热滞留重量保持率≥98.5%。
8.根据权利要求7所述的液晶聚酯组合物,其特征在于,所述的纤维状增强填料选自玻璃纤维、钛酸钾纤维、陶瓷纤维、硅灰石纤维、金属碳化物纤维、金属固化纤维、石棉纤维、氧化铝纤维、碳化硅纤维、石膏纤维、硼纤维中的至少一种。
9.根据权利要求7所述的液晶聚酯组合物,其特征在于,所述的颗粒状增强填料选自钛酸钾晶须、硼酸铝晶须、滑石粉、炭黑、石膏、石棉、沸石、高岭土、蒙脱土、粘土、锂蒙脱土、硅铝酸盐、二氧化硅、氧化钛、氧化铝、氧化锌、氧化锆、氧化铁、钛酸镁、白云石、硫酸铝、硫酸钡、硫酸镁、碳酸钙、云母、石英粉、氢氧化镁、氢氧化钙、氢氧化铝、玻璃珠、陶瓷珠、氮化硼、碳化硅中的至少一种。
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CN112250846A (zh) * | 2020-10-30 | 2021-01-22 | 金发科技股份有限公司 | 一种液晶聚酯、液晶聚酯组合物及应用 |
CN112724381A (zh) * | 2020-12-29 | 2021-04-30 | 上海普利特化工新材料有限公司 | 一种高机械强度热致型液晶聚合物树脂 |
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US20080286510A1 (en) * | 2004-10-29 | 2008-11-20 | Polyplastics Co., Ltd. | Resin Composition for Extrusion Molding and Extrusion-Molded Article |
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