KR19990074107A - Polybutylene Terephthalate Resin Composition - Google Patents
Polybutylene Terephthalate Resin Composition Download PDFInfo
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- KR19990074107A KR19990074107A KR1019980007492A KR19980007492A KR19990074107A KR 19990074107 A KR19990074107 A KR 19990074107A KR 1019980007492 A KR1019980007492 A KR 1019980007492A KR 19980007492 A KR19980007492 A KR 19980007492A KR 19990074107 A KR19990074107 A KR 19990074107A
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Abstract
본 발명은 폴리부틸렌테레프탈레이트; 폴리에틸렌테레프탈레이트; 글리시딜메타크릴레이트-함유 에틸렌 공중합체; 디메틸테레프탈레이트, 1,4-부탄디올 및 폴리테트라메틸렌글리콜의 반응생성물인 열가소성 폴리에스터 에라스토머; 및 유리섬유를 함유하는 폴리부틸렌테레프탈레이트 수지조성물에 관한 것으로서, 본 조성물은 인성과 표면특성이 우수하여 외장용 구조재료로 매우 유용하다.The present invention is polybutylene terephthalate; Polyethylene terephthalate; Glycidyl methacrylate-containing ethylene copolymers; Thermoplastic polyester elastomers which are reaction products of dimethyl terephthalate, 1,4-butanediol and polytetramethylene glycol; And it relates to a polybutylene terephthalate resin composition containing a glass fiber, the composition is excellent in toughness and surface properties is very useful as a exterior structural material.
Description
본 발명은 폴리에스테르 수지조성물에 관한 것으로, 더욱 상세하게는 고도의 인성을 요구하는 외장부품에 적합한 폴리부틸렌테레프탈레이트(이하, "PBT"라 약칭합니다) 수지 조성물에 관한 것이다.The present invention relates to a polyester resin composition, and more particularly, to a polybutylene terephthalate (hereinafter, abbreviated as "PBT") resin composition suitable for exterior parts requiring high toughness.
일반적으로 PBT 수지는 내열성이 우수하고 내약품성 및 기계적 강도가 우수하며 성형가공성이 우수하다. 또한 전기적 특성이 뛰어나 공업용 재료로 널리 쓰인다. 그러나 결정화도가 높기 때문에 재료가 취약하여 급격한 충격이나 외부응력에 대한 내충격성이 작다는 단점이 있다. 종래, 이를 개선하기 위하여 유리섬유를 보강하는 것이 알려져 있다. PBT 수지를 유리섬유로 강화하면 인장 및 충격강도는 모두 증가하나 취약한 특성은 향상되지 못하며, 또한 유리섬유의 증가에 따라 표면에 유리섬유가 돌출되는 등의 표면특성이 매끄럽지 못한 또 다른 문제점이 생겨난다.In general, PBT resin has excellent heat resistance, excellent chemical resistance and mechanical strength, and excellent molding processability. It is also widely used as an industrial material because of its excellent electrical properties. However, due to the high degree of crystallinity, the material is vulnerable and has a disadvantage in that impact resistance against sudden impact or external stress is small. It is conventionally known to reinforce glass fibers in order to improve this. Reinforcing PBT resin with glass fiber increases both tensile and impact strength, but does not improve the fragile properties. Also, as the glass fiber increases, the surface property such as glass fiber protruding from the surface causes another problem. .
따라서 위와 같은 단점들을 보완하기 위하여 여러종류의 충격보강재 및 표면개질을 위한 첨가제 등을 함유하는 방법들이 제안된 바 있다.Therefore, methods to contain various kinds of impact modifiers and additives for surface modification have been proposed to compensate for the above disadvantages.
PBT의 내충격성을 향상시키기 위한 종래 방법들 중 가장 널리 사용되어온 방법중의 하나는 일본 특개소45-26233호 및 소45-26224호에 기술된 것처럼 알파-올레핀 공중합체를 첨가하는 방법이다. 이 방법에 의한 조성물로 제조한 성형품은 초기에는 비교적 우수한 물성을 나타내나 PBT와 알파-올레핀 공중합체 사이의 상용성이 불량하여 시간이 경과할 수록 성형품의 물성이 점차 열화되는 단점이 있다.One of the most widely used methods for improving the impact resistance of PBT is a method of adding an alpha-olefin copolymer as described in Japanese Patent Laid-Open Nos. 45-26233 and 45-26224. The molded article prepared by the composition according to this method initially exhibits relatively excellent physical properties, but has a disadvantage in that the physical properties of the molded article gradually deteriorate with time due to poor compatibility between the PBT and the alpha-olefin copolymer.
다른 선행기술로서 미국특허 제4,485,212호 및 제4,558,096호에는 알파-올레핀 공중합체에 스티렌 및 아크릴로니트릴의 그라프트 공중합체(graft copolymer)를 PBT에 첨가하는 방법이 기술되어 있다. 이 방법에 의하면 충격강도가 향상되고 폴리에스터와 알파-올레핀 사이의 상용성이 다소 개선되나 만족할 만한 수준은 아니다.As another prior art, US Pat. Nos. 4,485,212 and 4,558,096 describe a method for adding a graf copolymer of styrene and acrylonitrile to an PBT in an alpha-olefin copolymer. This method improves impact strength and slightly improves compatibility between polyester and alpha-olefins, but is not satisfactory.
또한 미국 특허 제4,445,719호 및 일본 특개소 50-23448호 및 일본특개소50-23448호에는 에폭시 화합물에 부타디엔계 공중합체를 첨가하여 내충격성과 성형성을 개선시켰으나 내열성이 떨어지고 성형성이 떨어지는 단점이 있다.In addition, US Pat. No. 4,445,719, Japanese Patent Application Laid-Open No. 50-23448 and Japanese Patent Application Laid-open No. 50-23448 improve the impact resistance and formability by adding a butadiene-based copolymer to an epoxy compound, but have the disadvantage of poor heat resistance and poor moldability. .
일본특허공개소63-4566호에는 α-올레핀 및 α,β-불포화산의 글리시딜 에스테르기에서 유도된 글리시딜 함유 공중합체, 에틸렌-1-부텐 공중합체, 에틸렌-1-프로필렌 공중합체를 첨가하여 상온 및 저온 충격온도를 향상시켰으나 내열성이 떨어지는 단점이 있다.Japanese Patent Application Laid-Open No. 63-4566 discloses glycidyl-containing copolymers, ethylene-1-butene copolymers and ethylene-1-propylene copolymers derived from glycidyl ester groups of α-olefins and α, β-unsaturated acids. By adding to improve the impact temperature at room temperature and low temperature, but has a disadvantage of poor heat resistance.
또한 PBT의 표면특성을 향상시키기 위한 선행기술로서, 대한민국 특허공개 94-14265호에는 15-30중량%의 PBT에 황산바륨을 62-70중량% 첨가하고 폴리에틸렌테레프탈레이드(PET)를 8-25 중량% 첨가하여 주방용기등의 성형품에 외장용으로 적합한 조성물에 관한 내용이 있는데 이 경우 표면특성은 상당히 우수하나 인성이 부족하여 급격한 충격에 깨질수 있는 단점이 있다.In addition, as a prior art for improving the surface characteristics of PBT, Korean Patent Publication No. 94-14265 discloses adding 62-70% by weight of barium sulfate to 15-30% by weight of PBT and 8-25% by weight of polyethylene terephthalate (PET). There is a content of a composition suitable for exterior use in molded articles such as kitchen containers by adding%. In this case, the surface properties are quite excellent, but the toughness is insufficient and can be broken in a sudden impact.
따라서 본 발명은 이러한 선행기술의 단점을 감안하여 인성 및 표면특성을 동시에 향상시켜서 인성이 요구되는 외장용 구조재료에 적합한 폴리에스테르 수지조성물을 제공하는 것을 기술적 과제로 한다.Accordingly, the present invention provides a polyester resin composition suitable for exterior structural materials that require toughness by simultaneously improving toughness and surface properties in view of the disadvantages of the prior art.
상기한 과제를 해결한 본 발명에 의하면 다음의 성분들을 함유하는 폴리부틸렌테레프탈레이트 수지조성물이 제공된다:According to the present invention, which solves the above problems, a polybutylene terephthalate resin composition containing the following components is provided:
(a) 고유점도 0.8-1.4 ㎗/gr의 폴리부틸렌테레프탈레이트 30-65 중량%,(a) 30-65% by weight of polybutylene terephthalate having an intrinsic viscosity of 0.8-1.4 dl / gr,
(b) 고유점도 0.6-0.9 ㎗/gr의 폴리에틸렌테레프탈레이트 5-20 중량%;(b) 5-20% by weight polyethylene terephthalate with an intrinsic viscosity of 0.6-0.9 dl / gr;
(c) 글리시딜메타크릴레이트-함유 에틸렌 공중합체 2-10 중량%;(c) 2-10% by weight glycidyl methacrylate-containing ethylene copolymer;
(d) 디메틸테레프탈레이트, 1,4-부탄디올 및 폴리테트라메틸렌글리콜의 반응생성물인 열가소성 폴리에스터 에라스토머(thermoplastic polyester elastomer) 5-20 중량%; 및(d) 5-20% by weight of thermoplastic polyester elastomer which is a reaction product of dimethyl terephthalate, 1,4-butanediol and polytetramethylene glycol; And
(e) 유리섬유 5-40 중량%.(e) 5-40% glass fibers.
이하 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
본 조성물에 있어서, 주성분이 되는 폴리부틸렌테레프탈레이트(PBT)는 테레프탈산과 1,4-부탄디올의 중합생성물로서 그 고유점도는 0.8-1.4 ㎗/gr인 것이 적합하며, 상기 조성성분들 (a) 내지 (e)의 합계량을 기준으로 할 때, 그 함량비율은 30-65중량%가 적당하다. PBT 함량은 광택을 발현시키는 폴리에틸렌테레프탈레이트(b)의 최소함량 및 인성에 관여하는 열가소성 폴리에스터 에라스토머(d)의 함량을 고려하여 결정하는 것이 바람직하다.In the present composition, polybutylene terephthalate (PBT) as a main component is a polymerization product of terephthalic acid and 1,4-butanediol, and its intrinsic viscosity is suitably 0.8-1.4 dl / gr, and the composition components (a) Based on the total amount of (e) to (e), the content ratio is suitably 30 to 65% by weight. The PBT content is preferably determined in consideration of the minimum content of polyethylene terephthalate (b) expressing the gloss and the content of the thermoplastic polyester elastomer (d) involved in toughness.
폴리에틸렌테레프탈레이트는 표면특성을 개선하기 위하여 배합되는 것으로서 폴리부틸렌테레프탈레이트와 같은 폴리에스테르수지와 상용성이 우수하다. 일반적으로 폴리에틸렌테레프탈레이트는 폴리부틸렌테레프탈레이트에 비하여 결정화 속도가 느리기 때문에 단독으로 구조용 재료로 사용하지 못하는데, 그 이유는 사출성형성이 떨어져 대량 생산에 문제가 있고 재료의 강도도 현저히 낮기 때문이다. 본 조성물에 사용하기에 적합한 폴리에틸렌테레프탈레이트의 고유점도는 0.6-0.9 ㎗/gr가 적당하며, 이와 같이 높은 고유점도의 PET는 고상중합공정을 거쳐 제조할 수 있다. 고상중합을 하지 않은 저점도의 폴리에틸렌테레프탈레이트는 건조과정에서 펠렛 등이 융착될 수 있어 부적합하다. 본 조성물중 PET의 함량이 너무 높으면 성형 싸이클 타임(사출성형시간)이 길어져서 금형에서 이형이 안되고 대량생산이 곤란하게 되는 데, 그 이유는 PET의 결정화시간이 PBT 보다 현저하게 느리기 때문이다. 반대로 PET의 함량이 너무 낮으면 원하는 광택도를 얻는 것이 곤란하게 된다.Polyethylene terephthalate is blended to improve surface properties and is excellent in compatibility with polyester resins such as polybutylene terephthalate. In general, polyethylene terephthalate is not used alone as a structural material because of its slower crystallization rate than polybutylene terephthalate, because injection molding is poor, which causes problems in mass production and significantly lower strength of the material. Polyethylene terephthalate suitable for use in the present composition is suitable for intrinsic viscosity of 0.6-0.9 dl / gr, PET of such a high intrinsic viscosity can be prepared through a solid state polymerization process. Low-viscosity polyethylene terephthalate without solid phase polymerization is not suitable because pellets may be fused during drying. If the content of PET in the present composition is too high, the molding cycle time (injection molding time) becomes long, which does not mold release and makes mass production difficult, because the crystallization time of PET is significantly slower than PBT. On the contrary, if the content of PET is too low, it is difficult to obtain the desired glossiness.
하기 구조식으로 표시되는 글리시딜메타크릴레이트를 함유하는 에틸렌 공중합체는 말단에 에폭시기를 가지고 있어서 조성물을 압출기에서 컴파운딩할 때에 열에 의하여 폴리에스테르와 반응하여 조성물에 우수한 인성을 부여한다.The ethylene copolymer containing glycidyl methacrylate represented by the following structural formula has an epoxy group at the terminal, and when reacted with the polyester by heat when compounding the composition in an extruder, imparts excellent toughness to the composition.
본 조성물에 사용되는 글리시딜메타크릴레이트-함유 에틸렌 공중합체는 유리전이온도(glass transition temperature: Tg)가 낮으며 가공성이 우수한 등의 특징이 있다. 글리시딜메타크릴레이트-함유 에틸렌 공중합체의 시중구입가능한 예로는 일본 스미토모(Sumitomo)사에서 제조판매되는 이게타본드 이(Igetabond E)가 있다. Igetabond E는 에틸렌공중합체에 글리시딜메타크릴레이트가 약 12중량% 함유된 것으로 비중이 0.94이고, 유리전이온도가 -26℃이다.Glycidyl methacrylate-containing ethylene copolymer used in the composition is characterized by low glass transition temperature (Tg) and excellent processability. A commercially available example of glycidyl methacrylate-containing ethylene copolymer is Igetabond E manufactured and sold by Sumitomo, Japan. Igetabond E contains about 12% by weight of glycidyl methacrylate in the ethylene copolymer and has a specific gravity of 0.94 and a glass transition temperature of -26 ° C.
본 조성물중의 열가소성 폴리에스터 에라스토머는 디메틸테레프탈레이트, 1,4-부탄디올 및 폴리테트라메틸렌글리콜의 반응생성물이며, 폴리부틸렌테레프탈레이트와 같은 폴리에스테르에 대한 상용성이 우수하고 용융중에 가교가 없으므로 가공성을 우수하게 하며 인성보강효과를 제공한다.The thermoplastic polyester elastomer in the composition is a reaction product of dimethyl terephthalate, 1,4-butanediol and polytetramethylene glycol, and has excellent compatibility with polyesters such as polybutylene terephthalate and no crosslinking during melting. Excellent workability and toughness reinforcement effect.
본 조성물은 예를 들어 각 조성성분들을 상기한 조성비로 압출기 혹은 컴파운더에 투입하고 실린더 온도 230-270℃에서 혼련하고, 냉각조에서 냉각하여 펠렛상태로 제품화할 수 있다.For example, the composition may be introduced into an extruder or compounder at the composition ratio described above, kneaded at a cylinder temperature of 230 to 270 ° C., cooled in a cooling bath, and commercialized in pellet form.
본 발명 조성물의 특성 및 장점은 후술되는 실시예로부터 보다 명백하게 될 것이다. 물론, 하기 실시예는 본 발명을 예시하기 위한 것일 뿐 제한하기 위한 것은 아니다.The properties and advantages of the composition of the present invention will become more apparent from the examples described below. Of course, the following examples are intended to illustrate the invention but not to limit it.
[실시예 1]Example 1
컴파운더에 고유점도가 0.82 ㎗/gr인 폴리부틸렌테레프탈레이트(PBR) 수지 47중량%, 고유점도가 0.77 ㎗/gr인 폴리에틸렌테레프탈레이트(PET) 15 중량%를 투입하였다. 이때 폴리에틸렌테레프탈레이트는 고상중합공정을 거쳐 준비한 것을 사용하였다. 여기에 글리시딜메타크릴레이트-함유 에틸렌 공중합체로서 Igetabond E 3중량%; 디메틸테레프탈레이트, 1,4-부탄디올 및 폴리테트라메틸렌글리콜로 이루어진 열가소성 폴리에스터 에라스토머(TPE) 5 중량% 및 강성을 발현하기 위하여 유리섬유 30 중량%를 투입하였다. 또한 열안정성을 발현하기 위한 첨가제로서 힌더드(hindered) 페놀 계통의 1차안정제 0.3phr(백에 대한 중량부)와 인계의 2차안정제 0.35phr 투입하였다. 이와 같이 투입한 후 실린더온도 250℃에서 혼련하고 냉각조에서 냉각하여 펠렛으로 제조하였다. 제조된 펠렛을 건조기에서 120℃에서 4시간동안 건조하여 수분율이 0.01% 이하가 되도록 건조하고, 건조된 펠렛을 사출기에서 실린더 온도 250℃, 금형온도 80℃, 사출보압시간 10초, 냉각시간 12초 및 사출압력 120-140 bar의 조건하에 가공하여 시험편을 제조하였다.47 wt% of polybutylene terephthalate (PBR) resin having an intrinsic viscosity of 0.82 dl / gr and 15 wt% of polyethylene terephthalate (PET) having an intrinsic viscosity of 0.77 dl / gr were added to the compounder. In this case, polyethylene terephthalate was prepared by a solid phase polymerization process. 3% by weight of Igetabond E as glycidyl methacrylate-containing ethylene copolymer; 5 wt% of thermoplastic polyester elastomer (TPE) consisting of dimethyl terephthalate, 1,4-butanediol and polytetramethylene glycol and 30 wt% of glass fiber were added to express rigidity. In addition, 0.3 phr of the primary stabilizer of the hindered phenol (in parts by weight) and 0.35 phr of the phosphorus-based secondary stabilizer were added as an additive for expressing thermal stability. After the addition, the mixture was kneaded at a cylinder temperature of 250 ° C. and cooled in a cooling bath to prepare pellets. The prepared pellets were dried in a drier at 120 ° C. for 4 hours and dried to a moisture content of 0.01% or less, and the dried pellets were used in an injection molding machine at a cylinder temperature of 250 ° C., a mold temperature of 80 ° C., an injection holding time of 10 seconds, and a cooling time of 12 seconds. And a specimen was processed under the conditions of injection pressure 120-140 bar.
제조된 시험편을 사용하여 인장강도, 신율, 충격강도, 유동성평가를 위한 용융흐름지수(Melt Index: MI)를 측정하였다. 또한 표면이 연마된 금형을 이용하여 시편을 제작하고 이 시편을 사용하여 표면광택을 측정하였다. 상기한 물성은 다음과 같은 방법으로 측정하였으며, 그 결과는 하기 표 1에 제시된다.Melt Index (MI) was measured for the evaluation of tensile strength, elongation, impact strength, and flowability using the prepared test pieces. In addition, a specimen was fabricated using a mold having a polished surface, and surface gloss was measured using the specimen. The physical properties were measured by the following method, and the results are shown in Table 1 below.
- 인강강도 및 신율 : ASTM D638에 의거하여 TYPE 1 시편을 이용하여 온도 23±2 ℃, 상대습도 50±5%, 대기압의 조건에서 5mm/min의 속도로 측정한다. 신율은 항복점에서의 값을 기록하되, 최소 5회이상 측정하여 평균값으로 나타내었다.-Tensile strength and elongation: According to ASTM D638, measure using a Type 1 specimen at a speed of 5mm / min under conditions of temperature 23 ± 2 ℃, relative humidity 50 ± 5%, atmospheric pressure. Elongation was recorded as a value at the yield point, measured at least five times and expressed as an average value.
- 충격강도 : ASTM D256에 의거하여 펜들럼(Pendulum)에 의해 1/4" 두께의 시편이 파단될 때의 에너지를 나타내며, 최소 5회이상 측정하여 평균값으로 나타내었다.-Impact Strength: According to ASTM D256, it represents the energy when a 1/4 "thick specimen is broken by Pendulum. It is measured at least 5 times and expressed as an average value.
- 유동성 : ASTM D1238에 의거하여 용융흐름지수를 측정하였다. MI는 재료의 유동성을 평가하기 위하여 손쉽게 측정할 수 있는 지수로 주로 낮은 전단속도에서의 거동을 측정하므로 사출성형과 같은 높은 전단속도에서의 거동을 예측하기는 쉽지 않다. 그러나 같은 종류의 첨가제의 사용유무 또는 함량의 변화에 의한 유동성의 평가에는 적절하게 사용될 수 있다. 본 실험에서는 250℃의 온도에서 2160g의 하중하에서 측정하였으며, 10분당 토출되는 무게로 나타내되, 최소 5회정도 측정하여 평균값으로 나타내었다.-Flowability: The melt flow index was measured according to ASTM D1238. MI is an easily measurable index for evaluating the fluidity of a material. It is not easy to predict the behavior at high shear rates such as injection molding because it mainly measures the behavior at low shear rates. However, it can be appropriately used for the evaluation of fluidity due to the use or addition of the same kind of additives. In this experiment, measured under a load of 2160g at a temperature of 250 ℃, it is expressed as the weight discharged per 10 minutes, measured at least five times as an average value.
- 표면광택 : 가드너 마이크로 글로스 메터(Gloss Meter)를 이용하여 ASTM D523에 의거하여 60°의 반사율을 측정하되, 최소 5회이상 측정하여 평균값으로 나타내었다.-Surface gloss: Reflectance of 60 ° was measured according to ASTM D523 by using Gardner micro gloss meter, but at least 5 times was expressed as average value.
[실시예 2 내지 3 및 비교예 1 내지 5][Examples 2 to 3 and Comparative Examples 1 to 5]
하기 표 1에 제시되는 바와 같이 조성성분 및 함량을 변화시킨 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다. 각 예에 의한 조성물의 물성은 하기 표 1에 제시된다.The same procedure as in Example 1 was repeated except that the composition components and contents were changed as shown in Table 1 below. Physical properties of the composition according to each example are shown in Table 1 below.
상기 표 1로부터 알 수 있는 바와 같이, PET, TPE 및 Igetabond E를 사용하지 않은 비교예 1의 경우에는 인장신율, 충격강도, 유동성 및 표면특성이 불량하였고, PET와 Igetabond E를 사용하지 않은 비교예 2의 경우에는 인장강도 및 충격강도가 낮고 유동성이 불량하게 나타났으며, TPE와 Igetabond E를 사용하지 않은 비교예 3의 경우에는 인장신율, 충격강도 및 유동성이 부적합하였으며, PET를 사용하지 않은 비교예 4의 경우에는 인성, 유동성 표면특성이 부적합하였고, Igetabond E를 초과사용한 비교예 5의 경우에는 인성, 유동성 표면특성이 부적합하였다. 그러나, 본 발명에 따르는 실시예 1 내지 3의 조성물은 외장용 구조재료에 요구되는 제반물성이 고르게 개선된 효과를 보여준다. 이와 같이, 본 조성물은 외장용 구조재료에 적합한 인성 및 표면특성을 동시에 만족하는 것임을 알 수 있다.As can be seen from Table 1, in the case of Comparative Example 1 without using PET, TPE and Igetabond E, tensile elongation, impact strength, flowability and surface properties were poor, Comparative Example without using PET and Igetabond E In case of 2, the tensile strength and impact strength were low and the fluidity was poor. In Comparative Example 3 without TPE and Igetabond E, the tensile elongation, impact strength and fluidity were inadequate. In the case of Example 4, toughness and fluidity surface properties were inadequate, and in Comparative Example 5 in which Igetabond E was used in excess, the toughness and fluidity surface properties were inadequate. However, the compositions of Examples 1 to 3 according to the present invention show an evenly improved overall physical properties required for the exterior structural material. As such, it can be seen that the present composition simultaneously satisfies toughness and surface properties suitable for exterior structural materials.
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