KR100364218B1 - Improved polybutylene terephthalate resin composition - Google Patents
Improved polybutylene terephthalate resin composition Download PDFInfo
- Publication number
- KR100364218B1 KR100364218B1 KR1019970063463A KR19970063463A KR100364218B1 KR 100364218 B1 KR100364218 B1 KR 100364218B1 KR 1019970063463 A KR1019970063463 A KR 1019970063463A KR 19970063463 A KR19970063463 A KR 19970063463A KR 100364218 B1 KR100364218 B1 KR 100364218B1
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- South Korea
- Prior art keywords
- epoxy
- epoxy compound
- weight
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- polybutylene terephthalate
- Prior art date
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- 229920001707 polybutylene terephthalate Polymers 0.000 title claims abstract description 55
- -1 polybutylene terephthalate Polymers 0.000 title claims abstract description 27
- 239000011342 resin composition Substances 0.000 title claims abstract description 19
- 239000004593 Epoxy Substances 0.000 claims abstract description 64
- 150000001875 compounds Chemical class 0.000 claims abstract description 49
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 28
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 17
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003365 glass fiber Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000004417 polycarbonate Substances 0.000 claims abstract description 7
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 7
- 239000007809 chemical reaction catalyst Substances 0.000 claims abstract description 5
- 239000011256 inorganic filler Substances 0.000 claims abstract description 5
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims description 3
- 229930003836 cresol Natural products 0.000 claims description 3
- 229930185605 Bisphenol Natural products 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 2
- 150000007824 aliphatic compounds Chemical class 0.000 claims description 2
- 125000005907 alkyl ester group Chemical group 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 150000001491 aromatic compounds Chemical class 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- 150000002460 imidazoles Chemical class 0.000 claims description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 2
- 150000004714 phosphonium salts Chemical class 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- 150000004985 diamines Chemical class 0.000 claims 1
- 230000007774 longterm Effects 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 238000001746 injection moulding Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000003063 flame retardant Substances 0.000 description 7
- 238000001879 gelation Methods 0.000 description 7
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 2
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 1
- AQKDMKKMCVJJTC-UHFFFAOYSA-N 2-(2-methylpropoxymethyl)oxirane Chemical compound CC(C)COCC1CO1 AQKDMKKMCVJJTC-UHFFFAOYSA-N 0.000 description 1
- NPKKFQUHBHQTSH-UHFFFAOYSA-N 2-(decoxymethyl)oxirane Chemical compound CCCCCCCCCCOCC1CO1 NPKKFQUHBHQTSH-UHFFFAOYSA-N 0.000 description 1
- VMSIYTPWZLSMOH-UHFFFAOYSA-N 2-(dodecoxymethyl)oxirane Chemical compound CCCCCCCCCCCCOCC1CO1 VMSIYTPWZLSMOH-UHFFFAOYSA-N 0.000 description 1
- LKMJVFRMDSNFRT-UHFFFAOYSA-N 2-(methoxymethyl)oxirane Chemical compound COCC1CO1 LKMJVFRMDSNFRT-UHFFFAOYSA-N 0.000 description 1
- QYYCPWLLBSSFBW-UHFFFAOYSA-N 2-(naphthalen-1-yloxymethyl)oxirane Chemical compound C=1C=CC2=CC=CC=C2C=1OCC1CO1 QYYCPWLLBSSFBW-UHFFFAOYSA-N 0.000 description 1
- ZXJBWUAALADCRI-UHFFFAOYSA-N 2-(octadecoxymethyl)oxirane Chemical compound CCCCCCCCCCCCCCCCCCOCC1CO1 ZXJBWUAALADCRI-UHFFFAOYSA-N 0.000 description 1
- HJEORQYOUWYAMR-UHFFFAOYSA-N 2-[(2-butylphenoxy)methyl]oxirane Chemical compound CCCCC1=CC=CC=C1OCC1OC1 HJEORQYOUWYAMR-UHFFFAOYSA-N 0.000 description 1
- KSLSZOOZWRMSAP-UHFFFAOYSA-N 2-[(4-chlorophenoxy)methyl]oxirane Chemical compound C1=CC(Cl)=CC=C1OCC1OC1 KSLSZOOZWRMSAP-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- WORJEOGGNQDSOE-UHFFFAOYSA-N chloroform;methanol Chemical compound OC.ClC(Cl)Cl WORJEOGGNQDSOE-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- ZFTFAPZRGNKQPU-UHFFFAOYSA-N dicarbonic acid Chemical compound OC(=O)OC(O)=O ZFTFAPZRGNKQPU-UHFFFAOYSA-N 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical class C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- XRQKARZTFMEBBY-UHFFFAOYSA-N oxiran-2-ylmethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1CO1 XRQKARZTFMEBBY-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
- C08L67/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl- and the hydroxy groups directly linked to aromatic rings
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
-
- 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
- C08K7/14—Glass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
본 발명은 다음과 같은 조성을 갖는 개량된 폴리부틸렌테레프탈레이트 수지 조성물을 제공하는 것으로, 본 발명의 개량된 폴리부틸렌테레프탈레이트 수지 조성물은 장기내열성 및 내습열성이 우수하여 주변 환경의 열에 의하여 분해되거나 수분에 의해 가수분해되어 기계적 성질이 저하되지 않고 유동성 및 충격강도가 향상되어 두께가 얇은 성형품들을 사출성형할 수 있는 이점을 갖는다:The present invention provides an improved polybutylene terephthalate resin composition having the following composition, wherein the improved polybutylene terephthalate resin composition of the present invention is excellent in long-term heat resistance and heat-and-moisture resistance, and is decomposed by heat of the surrounding environment. Hydrolysis by moisture does not degrade the mechanical properties, improves fluidity and impact strength, and has the advantage of injection molding thin-walled moldings:
(A) PBT 수지 40∼90 중량%;(A) 40 to 90% by weight of PBT resin;
(B) 에폭시기가 1개인 에폭시 화합물 0.1∼10.0 중량%;(B) 0.1 to 10.0 wt% of an epoxy compound having one epoxy group;
(C) 에폭시기가 2개 이상인 에폭시 화합물 0.1∼10.0 중량%;(C) 0.1 to 10.0% by weight of an epoxy compound having two or more epoxy groups;
(D) 에폭시와 PBT 카르복실말단기 반응 촉매 0.01∼5.0 중량%;(D) 0.01 to 5.0% by weight of epoxy and PBT carboxyl terminal reaction catalyst;
(E) 브롬화 폴리카보네이트 올리고머 1.0∼30 중량%;(E) 1.0-30 wt% brominated polycarbonate oligomer;
(F) 삼산화안티몬 1.0∼10 중량%; 및(F) 1.0-10% by weight of antimony trioxide; And
(G) 유리섬유 및 무기충전제 상기 (A), (B), (C), (D), (E), 및 (F) 전체에 대하여 3-50 중량%.(G) Glass fiber and inorganic filler 3-50% by weight based on the entirety of (A), (B), (C), (D), (E), and (F).
Description
본 발명은 폴리부틸렌테레프탈레이트(이하 PBT로 칭함) 수지 조성물에 관한 것으로, 더욱 상세하게는 폴리부틸렌테레프탈레이트에 강화제, 및 난연제, 난연조제, 에폭시 화합물 등을 첨가하여 장기내열성, 내습열성이 우수하며, 유동성 및 충격강도를 향상시킨 개량된 폴리부틸렌테레프탈레이트 수지 조성물에 관한 것이다.The present invention relates to a polybutylene terephthalate (hereinafter referred to as PBT) resin composition, and more particularly, to a polybutylene terephthalate by adding a reinforcing agent, a flame retardant, a flame retardant aid, an epoxy compound, etc. It relates to an improved polybutylene terephthalate resin composition which is excellent and has improved flowability and impact strength.
일반적으로 PBT 수지는 결정화속도가 빠르고 유동성이 높으며, 내후성, 전기절연성, 내약품성 및 내마모성이 우수한 엔지니어링 플라스틱으로 전기, 전자, 자동차 기계 부품에 널리 사용되고 있다. 특히 PBT 수지는 유리섬유를 강화할 경우 인장강도, 굴곡강도, 충격강도 등의 기계적 성질과 내열성 등의 기초적인 제반 물성이 향상되는 효과를 나타낸다. 유리섬유 강화 PBT 수지는 유리섬유 강화 나이론 수지에 비하여 흡습에 의한 물성 변화가 적고, 유리섬유 강화 PET 수지 보다 결정화속도가 빨라 조핵제를 필요로 하지 않고 120℃ 이하의 낮은 금형온도에서도 충분한 결정화 거동을 시현한다.In general, PBT resin is an engineering plastic that has high crystallization rate and high flowability, and has excellent weather resistance, electrical insulation, chemical resistance, and abrasion resistance, and is widely used in electrical, electronic, and automotive mechanical parts. In particular, PBT resin has the effect of improving the mechanical properties such as tensile strength, flexural strength, impact strength, and basic physical properties such as heat resistance when glass fiber is reinforced. Compared with glass fiber reinforced nylon resin, glass fiber reinforced PBT resin has less physical property change due to moisture absorption, and crystallization rate is faster than glass fiber reinforced PET resin, so it does not require nucleating agent and shows sufficient crystallization behavior even at low mold temperature below 120 ℃. To demonstrate.
그러나, PBT는 두께가 얇은 성형품에서는 잘 깨지는 단점이 있을 뿐만 아니라, 고온에서는 소량의 수분에 의해서도 에스테르의 가수분해가 일어나고, 이로 인해 PBT의 분자량이 감소되어 기계적 성질이 급격하게 감소하는 현상을 나타내는 결점이 있었다. 이 때 가수분해는 말단의 카르복실(carboxyl)기에 의해 매우 빠르게 촉진되기 때문에, 이를 방지하기 위해서 PBT에 특수한 첨가제를 채용함으로써 말단기를 감소시키는 방법이 제안되었다. 그러나, 상기한 방법들은 PBT의 말단기를 감소시켜 장기내열성 및 내습열성을 향상시키기는 하였으나, PBT 수지의 유동성을 저하시켜 성형을 어렵게 하는 단점이 있었다.However, PBT has a disadvantage in that it is not only broken well in a thin molded article, but also hydrolysis of the ester occurs by a small amount of water at a high temperature, which results in a decrease in the molecular weight of the PBT and a rapid decrease in mechanical properties. There was this. At this time, since hydrolysis is accelerated very quickly by the terminal carboxyl group, a method of reducing the terminal group by employing a special additive to PBT has been proposed to prevent this. However, the above methods, although reducing the end group of the PBT to improve the long-term heat resistance and heat-and-moisture resistance, there was a disadvantage in that the molding of the PBT resin by reducing the fluidity.
상술한 PBT 수지의 단점을 보완하기 위하여, 일본특개소 51-91958호, 동51-5865호 등에서는, 한 분자내에 1-2개의 에폭시기를 가지고 있는 화합물을 사용하는 방법을 제안하였고, 일본특개평 3-9257호에서는 옥사졸린 화합물을 사용하여 PBT 수지의 장기내열성 및 내습열성을 향상시키는 방법을 제안하였다. 그러나, 에폭시기가 1개인 에폭시 화합물은 유동성은 우수하나 장기내열성 및 내습열성의 대폭적인 향상이 어렵고, 에폭시기가 2개인 에폭시 화합물 및 옥사졸린 화합물은 장기내열성 및 내습열성은 우수하나 수지의 겔화를 촉진하여 성형성을 저하시키는 문제점을 갖는다.In order to make up for the disadvantages of the above-described PBT resin, Japanese Patent Laid-Open Nos. 51-91958 and 51-5865 have proposed a method of using a compound having 1-2 epoxy groups in one molecule. In 3-9257, an oxazoline compound is used to propose a method for improving the long-term heat resistance and heat and humidity resistance of PBT resin. However, the epoxy compound having one epoxy group has excellent fluidity, but it is difficult to significantly improve long-term heat resistance and moist heat resistance. The epoxy compound and oxazoline compound having two epoxy groups have excellent long-term heat resistance and heat-and-moisture resistance but promote gelation of the resin. There is a problem of lowering moldability.
본 발명의 목적은 상술한 바와 같은 종래 기술의 문제점을 극복하는 것으로, 분자내에 1개의 에폭시기를 갖는 에폭시 화합물과 2개 이상의 에폭시 반응기가 있는 에폭시 화합물을 혼합사용하여 적절하게 반응성을 조절함으로써 PBT 수지의 겔화를 방지하고 우수한 장기내열성 및 내습열성을 갖는 PBT 수지 조성물을 제공하는 것이다.SUMMARY OF THE INVENTION An object of the present invention is to overcome the problems of the prior art as described above, and to adjust the reactivity appropriately by mixing and using an epoxy compound having one epoxy group and an epoxy compound having two or more epoxy reactors in a molecule thereof. It is to provide a PBT resin composition that prevents gelation and has excellent long-term heat resistance and heat-and-moisture resistance.
즉, 본 발명은That is, the present invention
(A) PBT 수지 40∼90 중량%;(A) 40 to 90% by weight of PBT resin;
(B) 에폭시기가 1개인 에폭시 화합물 0.1∼10.0 중량%;(B) 0.1 to 10.0 wt% of an epoxy compound having one epoxy group;
(C) 에폭시기가 2개 이상인 에폭시 화합물 0.1∼10.0 중량%;(C) 0.1 to 10.0% by weight of an epoxy compound having two or more epoxy groups;
(D) 에폭시와 PBT 카르복실말단기 반응 촉매 0.01∼5.0 중량%;(D) 0.01 to 5.0% by weight of epoxy and PBT carboxyl terminal reaction catalyst;
(E) 브롬화 폴리카보네이트 올리고머 1.0∼30 중량%;(E) 1.0-30 wt% brominated polycarbonate oligomer;
(F) 삼산화안티몬 1.0∼10 중량%; 및(F) 1.0-10% by weight of antimony trioxide; And
(G) 유리섬유 및 무기충전제 상기 (A), (B), (C), (D), (E), 및 (F) 전체에 대하여 3-50 중량%로 조성된 것을 특징으로 하는 개량 된 폴리부틸렌테레프탈레이트 수지 조성물을 제공하는 것이다.(G) Glass fiber and inorganic fillers, characterized in that 3-50% by weight relative to the total (A), (B), (C), (D), (E), and (F) It is providing a polybutylene terephthalate resin composition.
이하에서 본 발명을 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.
본 발명은 충격강도, 장기내열성, 내습열성 및 유동성이 우수한 개량된 폴리부틸렌테레프탈레이트 수지 조성물을 제공하고자 하는 것으로, 본 발명의 폴리부틸렌테레프탈레이트 수지 조성물은 PBT 수지, 에폭시기가 1개인 에폭시 화합물, 에폭시기가 2개 이상인 에폭시 화합물, 에폭시 화합물과 PBT 수지의 카르복실 말단기와의 반응성을 향상시켜주는 촉매를 포함하고, 난연제로서 브롬화 폴리카보네이트 올리고머를, 난연조제로 삼산화안티몬을 포함하며, 이 밖에 유리섬유 및 기타 무기충전제를 포함한다.The present invention is to provide an improved polybutylene terephthalate resin composition excellent in impact strength, long-term heat resistance, moist heat resistance and fluidity, the polybutylene terephthalate resin composition of the present invention is a PBT resin, epoxy group having one epoxy group And epoxy resins having two or more epoxy groups, catalysts for improving the reactivity of epoxy compounds with carboxyl end groups of PBT resin, brominated polycarbonate oligomers as flame retardants, and antimony trioxide as flame retardant aids. Fiber and other inorganic fillers.
본 발명에 사용된 PBT 수지(A)는 디카르본산(dicarbonic acid)과 디올(diol)의 중합으로 얻을 수 있다. 이 때 사용가능한 디카르본산 성분의 예로는 테레프탈산, 이소프탈산, 나프탈렌 디카르본산, 디페닐에테르 디카르복실산, 디페닐 디카르복실산, 디페닐설폰 디카르복실산 등을 들 수 있으며, 디올 성분으로는 폴리에틸렌, α,ω-디올, 예컨대 에틸렌글리콜, 트리메틸렌글리콜, 테트라메틸렌글리콜, 헥사메틸렌글리콜, 네오펜틸글리콜, 시클로헥산 디메틸올, 2,2-비스(4-β-하이드록시 페닐-페닐)-프로판, 4,4-비스(β-하이드록시 에폭시)-디페닐 설폰, 디에틸렌글리콜 등을 들 수 있다.PBT resin (A) used in the present invention can be obtained by polymerization of dicarbonic acid and diol. Examples of the dicarboxylic acid component usable here include terephthalic acid, isophthalic acid, naphthalene dicarboxylic acid, diphenyl ether dicarboxylic acid, diphenyl dicarboxylic acid, diphenyl sulfone dicarboxylic acid, and the like. Components include polyethylene, α, ω-diol such as ethylene glycol, trimethylene glycol, tetramethylene glycol, hexamethylene glycol, neopentyl glycol, cyclohexane dimethylol, 2,2-bis (4-β-hydroxy phenyl- Phenyl) -propane, 4, 4-bis ((beta) -hydroxy epoxy)-diphenyl sulfone, diethylene glycol, etc. are mentioned.
본 발명의 조성물에 포함되는 에폭시기를 1개 갖는 에폭시 화합물은 하기 화학식 1의 구조를 갖는다:The epoxy compound having one epoxy group included in the composition of the present invention has a structure of Formula 1 below:
상기 식에서,Where
R1은 지방족 또는 방향족 화합물 또는 이 두가지가 결합된 형태의 화합물이다.R 1 is an aliphatic or aromatic compound or a compound of the two combined forms.
이러한 그리시딜 에테르계 화합물의 예들은 라우릴 그리시딜에테르, 부틸페닐그리시딜에테르, 알릴그리시딜에테르, 스테아릴그리시딜에테르, 메틸그리시딜에테르, 이소부틸글리시딜에테르, 페닐그리시딜에테르, 파라클로로페닐그리시딜에테르, 나프틸그리시딜에테르, 데실그리시딜에테르, 그리시딜벤조에이트, 그리시딜부틸레이트, 페놀그리시딜에테르 등을 포함한다.Examples of such glycidyl ether compounds include lauryl glycidyl ether, butylphenyl glycidyl ether, allyl glycidyl ether, stearyl glycidyl ether, methyl glycidyl ether, isobutyl glycidyl ether, phenyl glycidyl ether, and para. Chlorophenylglycidyl ether, naphthylglycidyl ether, decylglycidyl ether, glycidyl benzoate, glycidyl butylate, phenol glycidyl ether and the like.
상기 에폭시기를 1개 갖는 에폭시 화합물(B)은 일반적인 2관능기 이상의 에폭시 수지가 성형가공시 그 화학구조상 수지내 카르복실 말단기와 반응하여 겔화를 촉진시키는 것에 반하여, 1개의 반응 관능기만을 갖기 때문에, 겔화를 촉진하지 않으면서 수지내 카르복실 말단기와 반응하여 말단기 함량을 감소시켜 수지 조성물의 장기내열성 및 내습열성을 향상시킨다.Since the epoxy compound (B) having one epoxy group has only one reactive functional group, whereas the epoxy resin having at least one bifunctional group reacts with the carboxyl terminal group in the resin during the molding process to promote gelation, the epoxy compound (B) has only one reactive functional group. It does not promote to react with the carboxyl end groups in the resin to reduce the end group content to improve the long-term heat resistance and moist heat resistance of the resin composition.
본 발명의 조성물 중의 상기 에폭시기를 1개 갖는 에폭시 화합물(B)의 함량은 0.1∼10 중량%이며, 바람직하게는 0.1∼2 중량%이다. 본 발명의 조성물 중 상기 화합물(B)의 함량이 0.1 중량% 미만이면 그 성능이 나타나지 않으며, 10 중량%를 초과하는 경우에는 과도한 함량으로 인하여 수지가 제 물성을 나타내지 않는 등 부작용이 발생할 가능성이 있다.The content of the epoxy compound (B) having one epoxy group in the composition of the present invention is 0.1 to 10% by weight, preferably 0.1 to 2% by weight. When the content of the compound (B) in the composition of the present invention is less than 0.1% by weight, its performance does not appear, and when it exceeds 10% by weight, there is a possibility that side effects may occur such that the resin does not exhibit physical properties due to excessive content. .
본 발명에서 에폭시기가 2개 이상인 에폭시 화합물(C)의 예는 폴리그리시딜 에테르 화합물, 폴리그리시딜아민에폭시 화합물, 비스페놀 A형 에폭시 화합물, 비스페놀 F형 에폭시 화합물, 레조르신올형 에폭시 화합물, 테트라히드록시 비스페놀 F형 에폭시 화합물, 크레졸노볼락형 에폭시 화합물, 페놀노볼락형의 에폭시 화합물 등을 포함한다.Examples of the epoxy compound (C) having two or more epoxy groups in the present invention include a polyglycidyl ether compound, a polyglycidylamine epoxy compound, a bisphenol A epoxy compound, a bisphenol F type epoxy compound, a resorcinol type epoxy compound, and tetrahydroxy Bisphenol F-type epoxy compound, a cresol novolak-type epoxy compound, a phenol novolak-type epoxy compound, etc. are contained.
본 발명에서 에폭시기가 2개 이상인 에폭시 화합물(C)은 에폭시기가 1개인 에폭시 화합물(B)과 같이 PBT의 말단 카르복실기(-COOH)와 반응하여 말단 카르복실기를 줄여 PBT 수지의 장기내열성 및 내습열성을 향상시키고 분해억제능력으로 내충격성을 향상시키는 작용을 하지만, 그 자체로는 PBT 겔화를 촉진시키는 부작용을 갖는데, 이러한 부작용은 에폭시기를 1개 갖는 에폭시 화합물(B)과 혼합사용함으로써 예방될 수 있다.In the present invention, the epoxy compound (C) having two or more epoxy groups reacts with the terminal carboxyl group (-COOH) of the PBT like the epoxy compound (B) having one epoxy group to reduce the terminal carboxyl group to improve the long-term heat resistance and heat and moisture resistance of the PBT resin. It has a side effect of promoting PBT gelation by itself, but the side effect can be prevented by mixing with an epoxy compound (B) having one epoxy group.
본 발명에서 에폭시기가 2개 이상인 에폭시 화합물(C)의 적절한 함량은 0.1∼10 중량%이고, 바람직하게는 0.1∼5 중량%이며, 성분 (C)의 함량이 0.1 중량% 미만이면 장기내열성 및 내습열성 향상 효과가 부족하게 되고, 이와 반대로 10 중량%를 초과하는 경우에는 수지의 성형성이 불량해지는 문제점이 발생하므로, 본 발명에서 에폭시기가 2개 이상인 에폭시 화합물(C)의 함량은 상기 범위내인 것이 필수적이다.In the present invention, the appropriate content of the epoxy compound (C) having two or more epoxy groups is 0.1 to 10% by weight, preferably 0.1 to 5% by weight, and if the content of component (C) is less than 0.1% by weight, long term heat resistance and moisture resistance. When the thermally improving effect is insufficient, on the contrary, when the content exceeds 10% by weight, a problem arises in that the moldability of the resin is poor. In the present invention, the content of the epoxy compound (C) having two or more epoxy groups is within the above range. It is essential.
본 발명에서 상기 에폭시기가 1개인 에폭시 화합물과 에폭시기가 2개 이상인 에폭시 화합물의 혼합비율은 0.01∼99.99이다.In the present invention, the mixing ratio of the epoxy compound having one epoxy group and the epoxy compound having two or more epoxy groups is 0.01 to 99.99.
본 발명의 개량된 폴리부틸렌테레프탈레이트 수지 조성물에는 에폭시와 PBT 카르복실 말단기 반응 촉매가 포함되는데, 이와 같이 촉매를 사용하면 에폭시의 반응성을 향상시킬 수 있을 뿐만 아니라, PBT 수지 내에서의 카르복실 말단기와 선택적 반응을 진행함으로써 에폭시의 효율을 극대화할 수 있어 소량의 에폭시 화합물로도 우수한 목표 수준에 도달할 수 있기 때문에 PBT 수지의 겔화를 억제할 수 있다. 더욱이, 압출 등 1차 가공공정에서 대부분의 에폭시가 반응을 진행하므로 사출 성형 등 2차 가공 과정에서 수지 겔화를 촉진하지 않는다.The improved polybutylene terephthalate resin composition of the present invention includes an epoxy and a PBT carboxyl end group reaction catalyst, and the use of such a catalyst not only improves the reactivity of the epoxy, but also the carboxyl in the PBT resin. By proceeding with a selective reaction with the end group it is possible to maximize the efficiency of the epoxy to reach a good target level even with a small amount of epoxy compound can suppress the gelation of the PBT resin. Furthermore, since most of the epoxy proceeds in the primary processing process such as extrusion, the resin gelation is not promoted during the secondary processing such as injection molding.
본 발명에서 성분 (B),(C) 에폭시와 PBT 수지의 카르복실 말단기와의 반응을 촉진하는 촉매로서 사용되는 촉매(D)의 예로는 인산, 아인산, 포스핀산, 포스폰산 등의 저급 알킬에스테르, 포스포늄 화합물, 이미다졸 화합물, 3가 아민, 4가 암모늄염 등을 포함한다. 본 발명에서 상기 촉매(D)의 적절한 사용량은 0.001∼5 중량%이다. 본 발명에서 촉매의 사용량이 상기 범위를 벗어나면 본 발명에서 의도하는 효과를 수득할 수 없게 된다.Examples of the catalyst (D) used in the present invention as a catalyst for promoting the reaction between the component (B) and (C) epoxy and the carboxyl end groups of the PBT resin include lower alkyl esters such as phosphoric acid, phosphorous acid, phosphinic acid and phosphonic acid. , Phosphonium compounds, imidazole compounds, trivalent amines, tetravalent ammonium salts and the like. Suitable amount of the catalyst (D) in the present invention is 0.001 to 5% by weight. When the amount of the catalyst used in the present invention is outside the above range, the effect intended in the present invention cannot be obtained.
본 발명의 폴리부틸렌테레프탈레이트 수지 조성물 중 주난연제로는 브롬화 폴리카보네이트계 난연제가 포함되며, 그 함량은 1.0∼30 중량%, 바람직하게는 5∼20 중량%이다. 본 발명의 조성물중 난연조제로는 삼산화안티몬이 1.0∼10 중량%의 함량으로 포함된다.The main flame retardant in the polybutylene terephthalate resin composition of the present invention includes a brominated polycarbonate-based flame retardant, the content is 1.0 to 30% by weight, preferably 5 to 20% by weight. The flame retardant aid in the composition of the present invention contains antimony trioxide in an amount of 1.0 to 10% by weight.
본 발명에서 폴리부틸렌테레프탈레이트의 기계적 물성을 향상시키기 위해 첨가되는 유리섬유는 통상의 유리로빙 중에서 적당한 길이로 절단한 단섬유(chopped strand)가 사용될 수 있으며, 수지와의 접착력을 높이기 위해 커플링제를 사용할 수 있다. 기타 무기충전제로는 탄소섬유, 세라믹섬유, 붕소섬유, 티탄산칼륨섬유, 아스베스토스, 탄산칼슘, 규산염, 알루미나, 수산화알루미늄, 활석, 점토, 운모, 유리분말, 유리비이드, 황산바륨, 희스커 등이 사용될 수 있다.In the present invention, the glass fiber added to improve the mechanical properties of the polybutylene terephthalate may be used a chopped strand cut to a suitable length in ordinary glass roving, and a coupling agent to increase the adhesive strength with the resin Can be used. Other inorganic fillers include carbon fiber, ceramic fiber, boron fiber, potassium titanate fiber, asbestos, calcium carbonate, silicate, alumina, aluminum hydroxide, talc, clay, mica, glass powder, glass beads, barium sulfate, and heskers. Can be used.
본 발명의 폴리부틸렌테레프탈레이트 수지 조성물에는 상술한 성분 (A), (B), (C), (D), (E), (F) 및 (G) 이외에 물성을 해하지 않는한 통상의 산화방지제, 이형제, 안티-드리핑 에이젼트(anti-dripping agent), 안료, 무기첨가제 등도 첨가될 수 있다. 이 때 각각의 첨가제의 함량은 (A), (B), (C), (D), (E), (F) 및 (G) 전체에 대하여 0.1∼2.0 중량%의 미량인 것이 바람직하다.In the polybutylene terephthalate resin composition of the present invention, in addition to the components (A), (B), (C), (D), (E), (F) and (G) described above, normal oxidation is not carried out. Inhibitors, release agents, anti-dripping agents, pigments, inorganic additives and the like may also be added. At this time, the content of each additive is preferably 0.1 to 2.0% by weight based on the total amount of (A), (B), (C), (D), (E), (F) and (G).
이하에서 본 발명을 실시예를 들어 더욱 상세히 설명하나, 이하의 실시예들은 설명의 목적만을 위한 것으로 본 발명의 보호범위를 제한하는 의미로 해석되어서는 안된다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following Examples are for illustrative purposes only and should not be construed as limiting the protection scope of the present invention.
실시예 1∼2Examples 1-2
하기 표 1에 표기된 조성의 조성물들 중 유리섬유를 제외한 나머지 성분들을 헨셀 믹서기에서 3∼10분간 균일하게 혼합한 후 이축압출기에 투입하고, 유리섬유는 사이드 피더를 이용하여 압출기 중간에 투입하여 압출온도 240℃, 250 rpm으로 압출하여 펠렛으로 제조하였다. 이어서 제조된 펠렛을 10 oz 사출기를 이용하여 사출온도 240℃, 금형온도 80℃로 사출하여 물성 시편을 제조하고 상대습도 50%에서 40시간 방치한 후 물성을 측정하여 그 결과를 하기 표 1에 나타내었다.The remaining ingredients except the glass fibers of the compositions shown in Table 1 are uniformly mixed for 3 to 10 minutes in a Henschel mixer, and then introduced into a twin screw extruder, and the glass fibers are fed into the extruder using a side feeder in the middle of the extrusion temperature. Extruded at 240 ℃, 250 rpm to prepare a pellet. Subsequently, the prepared pellets were injected at an injection temperature of 240 ° C. and a mold temperature of 80 ° C. using a 10 oz. Injection machine to prepare a physical specimen, and left at 40% for 50 hours at a relative humidity to measure physical properties. The results are shown in Table 1 below. It was.
〈물성 평가 방법〉<Property evaluation method>
(1) PBT 카르복실 말단기 함량 : 용제로서 벤질알콜, 클로로포름, 클로로포름-메탄올 등을 사용하여 PBT를 용해시킨 후 수산화나트륨으로 적정하는 방법을 사용하여 측정하였다.(1) PBT carboxyl end group content: It was measured using a method of dissolving PBT using benzyl alcohol, chloroform, chloroform-methanol as a solvent and titrating with sodium hydroxide.
(2) 내습열성 : 인장강도 측정 시편을 120℃, 2atm에서 100 시간 동안 가압처리 시험(pressure cooking test)을 실시한 후 인장강도 변화를 측정하여 평가하였으며, 이 때 인장강도는 ASTM D638에 따라 측정하였다.(2) Moisture and heat resistance: Tensile strength measurement specimens were subjected to a pressure cooking test at 120 ° C. and 2 atm for 100 hours, and then the tensile strength was measured and evaluated, and tensile strength was measured according to ASTM D638. .
(3) 장기내열특성 : 180℃에서 200 시간 경과한 후의 인장강도유지율로 평가하였다.(3) Long-term heat resistance: Tensile strength retention was evaluated after 200 hours at 180 ° C.
(4) 유동성 : 스피랄 테스트(두께 1.5 mm)로 측정하였다.(4) Fluidity: It was measured by a spiral test (thickness 1.5 mm).
(5) 충격강도 : ASTM D256에 따라 평가하였다.(5) Impact strength: evaluated according to ASTM D256.
비교예 1∼5Comparative Examples 1 to 5
조성물의 조성을 하기 표 1에 나타낸 바와 같이 변경한 것을 제외하고는 실시예 1과 동일한 방법으로 실시하여 물성 시편을 제조하고 상대습도 50%에서 40시간 방치한 후 물성을 측정하여 그 결과를 하기 표 1에 함께 나타내었다.Except for changing the composition of the composition as shown in Table 1 below, the same procedure as in Example 1 was carried out to prepare a physical specimen and left for 40 hours at 50% relative humidity and then measured for physical properties. Together.
본 발명의 개량된 폴리부틸렌테레프탈레이트 수지 조성물은 장기내열성 및 내습열성이 우수하여 주변 환경의 열에 의하여 분해되거나 수분에 의해 가수분해되어 기계적 성질이 저하되지 않고 유동성 및 충격강도가 향상되어 두께가 얇은 성형품들을 사출성형할 수 있는 이점을 갖는다.The improved polybutylene terephthalate resin composition of the present invention has excellent long-term heat resistance and heat-and-moisture resistance, and is decomposed by heat in the surrounding environment or hydrolyzed by moisture, thereby reducing mechanical properties and improving fluidity and impact strength. It has the advantage of being able to injection molded molded articles.
또한 본 발명의 폴리부틸렌테레프탈레이트 수지 조성물은 에폭시 수지와 PBT 수지에 있는 카르복실 말단기와의 반응성을 향상시켜 주기 위하여 가공성형시 반응을 촉진시켜 줄 수 있는 촉매를 포함하여 사용가능한 에폭시량을 최적화시켜줌으로써 소량의 에폭시 화합물로도 우수한 목표 수준에 도달할 수 있는 장점 때문에 PBT 수지의 겔화를 억제시켜 성형성이 향상된 효과도 갖는다.In addition, the polybutylene terephthalate resin composition of the present invention to optimize the amount of epoxy available, including a catalyst that can promote the reaction during processing in order to improve the reactivity of the epoxy resin and the carboxyl end groups in the PBT resin In addition, because of the advantage of reaching a good target level even with a small amount of epoxy compound, it also has an effect of suppressing the gelation of the PBT resin to improve the moldability.
Claims (5)
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| KR100430193B1 (en) * | 1998-12-31 | 2004-10-12 | 제일모직주식회사 | Polybutylene Terephthalate Resin Composition |
| KR100446474B1 (en) * | 2001-05-30 | 2004-09-01 | 주식회사 삼양사 | Polybutyleneterephthalate having good durability |
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|---|---|---|---|---|
| JPH0395257A (en) * | 1989-05-29 | 1991-04-19 | Polyplastics Co | Flame retardant polyester resin composition |
| US5034439A (en) * | 1988-12-29 | 1991-07-23 | Ciba-Geigy Corporation | Flame-resistant polyester moulding compound |
| JPH05230348A (en) * | 1992-02-19 | 1993-09-07 | Teijin Ltd | Flame-retardant resin composition |
| KR940002316A (en) * | 1992-07-08 | 1994-02-17 | 하기주 | Flame Retardant Polyester Resin Composition |
| JPH0812865A (en) * | 1994-02-28 | 1996-01-16 | Matsushita Electric Works Ltd | Pbt resin molding material |
| KR19990042601A (en) * | 1997-11-27 | 1999-06-15 | 유현식 | Polybutylene Terephthalate Resin Composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5034439A (en) * | 1988-12-29 | 1991-07-23 | Ciba-Geigy Corporation | Flame-resistant polyester moulding compound |
| JPH0395257A (en) * | 1989-05-29 | 1991-04-19 | Polyplastics Co | Flame retardant polyester resin composition |
| JPH05230348A (en) * | 1992-02-19 | 1993-09-07 | Teijin Ltd | Flame-retardant resin composition |
| KR940002316A (en) * | 1992-07-08 | 1994-02-17 | 하기주 | Flame Retardant Polyester Resin Composition |
| JPH0812865A (en) * | 1994-02-28 | 1996-01-16 | Matsushita Electric Works Ltd | Pbt resin molding material |
| KR19990042601A (en) * | 1997-11-27 | 1999-06-15 | 유현식 | Polybutylene Terephthalate Resin Composition |
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