KR100446473B1 - High Viscosity Poly(butylene terephthalate) for high speed extrusion - Google Patents
High Viscosity Poly(butylene terephthalate) for high speed extrusion Download PDFInfo
- Publication number
- KR100446473B1 KR100446473B1 KR10-2001-0035103A KR20010035103A KR100446473B1 KR 100446473 B1 KR100446473 B1 KR 100446473B1 KR 20010035103 A KR20010035103 A KR 20010035103A KR 100446473 B1 KR100446473 B1 KR 100446473B1
- Authority
- KR
- South Korea
- Prior art keywords
- extrusion
- viscosity
- speed extrusion
- polybutylene terephthalate
- lubricant
- Prior art date
Links
Classifications
-
- 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
- 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
- C08G63/80—Solid-state polycondensation
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
Landscapes
- 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 고속압출용 고점도 폴리부틸렌테레프탈레이트 수지의 제조방법에 관한 것으로서, 더욱 상세하게는 용융중합으로 얻은 PBT 수지에 윤활제 0.1 내지 2.0 중량%를 첨가하고 핵제 1.0 내지 5.0 중량%를 첨가하여 압출가공 후 고상중합을 수행함으로써, 고점도이면서도 빠른 전단속도에서 낮은 전단점도를 가지며 결정화 속도가 빨라 고속압출이 가능한 폴리부틸렌테레프탈레이트(PBT) 수지를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a high viscosity polybutylene terephthalate resin for high-speed extrusion, and more specifically, to the PBT resin obtained by melt polymerization, by adding 0.1 to 2.0% by weight of the lubricant and 1.0 to 5.0% by weight of the nucleating agent is extruded The present invention relates to a method for preparing a polybutylene terephthalate (PBT) resin having a high viscosity and a low shear viscosity at a high shear rate and a fast crystallization rate to enable high-speed extrusion by performing solid phase polymerization after processing.
Description
본 발명은 고속압출용 고점도 폴리부틸렌테레프탈레이트 수지의 제조방법에 관한 것으로서, 더욱 상세하게는 용융중합으로 얻은 PBT 수지에 윤활제 0.1 내지 2.0 중량%를 첨가하고 핵제 1.0 내지 5.0 중량%를 첨가하여 압출가공 후 고상중합을 수행함으로써, 고점도이면서도 빠른 전단속도에서 낮은 전단점도를 가지며 결정화 속도가 빨라 고속압출이 가능한 폴리부틸렌테레프탈레이트(PBT) 수지를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a high viscosity polybutylene terephthalate resin for high-speed extrusion, and more specifically, to the PBT resin obtained by melt polymerization, by adding 0.1 to 2.0% by weight of the lubricant and 1.0 to 5.0% by weight of the nucleating agent is extruded The present invention relates to a method for preparing a polybutylene terephthalate (PBT) resin having a high viscosity and a low shear viscosity at a high shear rate and a fast crystallization rate to enable high-speed extrusion by performing solid phase polymerization after processing.
일반적으로 PBT는 폴리에틸렌테레프탈레이트와 비슷한 특성을 가지며, 한때 유리전이온도가 너무 낮아서 합성섬유로는 실용성이 떨어졌으나, 현재 엔지니어링용으로 개발되면서 본격적으로 사용되고 있다.In general, PBT has properties similar to polyethylene terephthalate, and at one time the glass transition temperature is so low that it is not practical as a synthetic fiber, but is currently being used in earnest as it is developed for engineering.
이와 같은 PBT는 현재 흡수성, 치수 안정성, 내마모성 등의 기계적 특성과 가공성이 우수하기 때문에 아라미드계와 함께 광섬유 자케팅용으로 사용되고 있으며, 전자 통신망의 확충 및 교체의 증가와 더불어 그 사용량도 매우 빠르게 증가하고 있는 실정이다. 광섬유 자케팅용으로 사용되고 있는 PBT 수지는 용융중합 후 고상중합을 통해 고유점도가 1.15 ∼ 1.35 ㎗/g 정도의 고점도를 가지는 것을 사용하여야 한다. 그러나, 현재까지의 문헌을 살펴보면 고점도의 PBT 수지를 제조하는 고상중합 방법이나 고상중합을 빠르게 하는 방법 등의 연구는 보고된 바가 많지만, 아직까지 고점도이면서 고속압출용 PBT 수지는 알려진 바가 없다.Such PBT is currently used for optical fiber jacketing with aramid system because of its excellent mechanical properties such as absorbency, dimensional stability, abrasion resistance, etc., and its usage increases very rapidly with the expansion and replacement of electronic communication networks. There is a situation. PBT resin, which is used for optical fiber jacketing, should have high viscosity of 1.15 ~ 1.35 ㎗ / g through solid phase polymerization after melt polymerization. However, looking at the literature to date, studies on a solid phase polymerization method for producing a high viscosity PBT resin or a method for speeding up the solid phase polymerization have been reported, but a high viscosity and high speed extrusion PBT resin is not known yet.
상기 문헌의 예로써 미국 특허 제 4,917,845호와 제 5,536,810호 등에서는 빠른 고상중합으로 고분자량을 얻는 방법이나 가장 적당한 고상중합 온도를 구하는 방법 등에 대해서 개시되어 있으며, 미국 특허 제 5,334,343호에는 결정화 속도를 향상시켜 압출에 응용하는 방법에 대해 개시되어 있으나 PBT 수지의 고속압출에 관해서는 알려진 바가 없다.As examples of such documents, US Pat. Nos. 4,917,845, 5,536,810, and the like disclose methods for obtaining high molecular weight by fast solid-state polymerization, and methods for obtaining the most suitable solid-phase polymerization temperature. US Pat. No. 5,334,343 improves the crystallization rate It is disclosed a method for application to extrusion, but is not known for the high-speed extrusion of PBT resin.
상기와 같이, 기존의 PBT 수지를 고속압출 시 사용하게 되면 전단점도가 높고 결정화 속도가 느려서 가공 후 수축이 많이 일어나므로 광섬유가 휘거나 꺾이게 되는 문제점이 있으므로, 고점도이면서 고속압출이 가능한 PBT 수지의 개발이 시급한 실정이다.As described above, when the existing PBT resin is used for high-speed extrusion, the shear viscosity is high and the crystallization rate is slow, so that a lot of shrinkage occurs after processing, so that the optical fiber is bent or bent. Thus, the development of high viscosity and high-speed extrusion is possible. This is urgent.
이에, 본 발명자들은 상기와 같은 점을 감안하여 연구한 결과, 용융 중합으로 얻은 PBT 수지에 윤활제와 핵제를 첨가하여 압출가공한 후 고상중합을 수행하여 고속압출 시 전단점도가 낮으며 결정화 속도가 빠른 고속압출용 고점도 PBT 수지를 제조함으로써 본 발명을 완성하게 되었다.Therefore, the present inventors have studied in view of the above, as a result of the extrusion process by adding a lubricant and a nucleating agent to the PBT resin obtained by melt polymerization after performing solid-phase polymerization, the shear viscosity is low at high-speed extrusion and the crystallization rate is fast The present invention has been completed by producing a high viscosity PBT resin for high-speed extrusion.
따라서, 본 발명은 고속압출이 가능한 PBT 수지를 제조하는 방법을 제공하는데 그 목적이 있다.Accordingly, an object of the present invention is to provide a method for producing a PBT resin capable of high-speed extrusion.
본 발명은 용융중합으로 얻은 PBT 수지에 윤활제 0.1 내지 2.0 중량%, 핵제를 1.0 내지 5.0 중량% 첨가하여 압출가공한 후 고상중합을 수행함으로써 고속압출이 가능한 고점도 PBT 수지를 제조하는 방법을 그 특징으로 한다.The present invention is characterized by a method of producing a high viscosity PBT resin capable of high-speed extrusion by performing solid phase polymerization after extrusion processing by adding 0.1 to 2.0% by weight of lubricant, 1.0 to 5.0% by weight of nucleating agent to the PBT resin obtained by melt polymerization do.
이와 같은 본 발명을 더욱 상세하게 설명하면 다음과 같다.The present invention will be described in more detail as follows.
일반적으로 PBT 수지는 디메틸테레프탈레이트(DMT) 또는 테레프탈릭에시드(TPA)와 부탄디올(1,4-BD)을 사용하여 용융중합 후 고상중합을 하여 제조된다.In general, PBT resin is prepared by solid phase polymerization after melt polymerization using dimethyl terephthalate (DMT) or terephthalic acid (TPA) and butanediol (1,4-BD).
본 발명에 사용되는 용융중합에 의해 얻어진 PBT 수지는 용융유동지수(250 ℃, 2.16 kg, 이하 동일 조건)가 30 내지 80 g/10 min인 것을 사용할 수 있다.As the PBT resin obtained by melt polymerization used in the present invention, a melt flow index (250 ° C., 2.16 kg, or the same conditions below) may be used in a range of 30 to 80 g / 10 min.
본 발명에서 광케이블 고속 압출시 압출 부하를 낮추기 위해 전단 점도를 낮추는 역할을 하는 윤활제로는 칼슘 스테아레이트(Ca(C17H35COO)2), 마그네슘 스테아레이트(Mg(C17H35COO)2) 또는 바륨 스테아레이트(Ba(C17H35COO)2) 등을 사용한다. 그리고, 상기 윤활제는 PBT 수지에 대하여 0.1 내지 2.0 중량% 첨가하는 것이 바람직하며, 더욱 바람직하게는 0.2 내지 1.0 중량%가 좋다. 만일 윤활제를 0.1 중량% 미만으로 사용하면 전단점도를 낮추는 효과가 없으며, 2.0 중량%를 초과하여사용하면 더 이상 전단점도가 낮아지는 효과가 없다.In the present invention, lubricants that lower shear viscosity in order to reduce extrusion load in high speed optical cable extrusion include calcium stearate (Ca (C 17 H 35 COO) 2 ) and magnesium stearate (Mg (C 17 H 35 COO) 2 ) Or barium stearate (Ba (C 17 H 35 COO) 2 ), or the like. The lubricant is preferably added in an amount of 0.1 to 2.0 wt% based on the PBT resin, and more preferably 0.2 to 1.0 wt%. If the lubricant is used in less than 0.1% by weight, there is no effect of lowering the shear viscosity, and when used in excess of 2.0% by weight, the shear viscosity is no longer lowered.
또한, 본 발명에서 광케이블 고속압출시 압출 부하를 낮추기 위해 결정화 속도를 빠르게 하는 역할을 하는 핵제로는 다음 화학식 1로 표시되는 화합물로, 바람직하게는 디메틸테레프탈로일디옥시디벤조에이트 또는 디메틸테레프탈로일디옥시나프토에이트 등을 사용한다. 그리고, 상기 핵제는 PBT 수지에 대하여 1.0 내지 5.0 중량%로 첨가하는 것이 바람직하며, 더욱 바람직하게는 2.0 내지 3.0 중량%가 좋다. 만일 핵제를 1.0 중량% 미만 사용하면 결정화 속도가 빨라지는 효과가 없으며, 5.0 중량%를 초과하여 사용하면 결정화 속도가 너무 빨라져서 가공하는 동안에 수축이 많이 일어나는 문제점이 있다.In addition, in the present invention, the nucleating agent that plays a role of increasing the crystallization rate in order to lower the extrusion load during high-speed extrusion of the optical cable is a compound represented by the following formula (1), preferably dimethyl terephthaloyldioxydibenzoate or dimethyl terephthaloyl Oxynaphthoate etc. are used. In addition, the nucleating agent is preferably added in an amount of 1.0 to 5.0 wt% with respect to the PBT resin, and more preferably 2.0 to 3.0 wt%. If the nucleating agent is used less than 1.0% by weight, there is no effect of increasing the crystallization rate, and when it is used in excess of 5.0% by weight, the crystallization rate is too fast, causing a lot of shrinkage during processing.
상기 화학식 1에서; R은 수소원자 또는 알킬기이며, Ar과 Ar'는 방향족이다.In Chemical Formula 1; R is a hydrogen atom or an alkyl group, and Ar and Ar 'are aromatic.
본 발명에 따른 PBT 수지는 상기한 윤활제와 핵제를 용융중합으로 얻은 PBT 수지에 첨가하여 압출가공한 후 고상중합을 수행함으로써 제조할 수 있다.The PBT resin according to the present invention can be prepared by adding the lubricant and the nucleating agent to the PBT resin obtained by melt polymerization and performing solid phase polymerization after extrusion processing.
또한, 본 발명은 상기한 방법에 의해 제조된 용융유동지수가 7 내지 15 g/10 min이고, 고유점도가 1.15 내지 1.35 ㎗/g인 고속압출용 고점도 PBT 수지를 포함한다.In addition, the present invention includes a high viscosity PBT resin for high-speed extrusion having a melt flow index of 7 to 15 g / 10 min and an intrinsic viscosity of 1.15 to 1.35 dl / g.
한편, 광케이블의 압출가공 후 수축이 발생하면 수축되지 않는 광섬유가 휘거나 꺾이게 되므로 광손실의 우려가 있다. 따라서, 압출가공 후 광케이블의수축 발생을 방지하기 위해서 짧은 시간 내에 결정화할 수 있어야 하므로 PBT의 결정화 속도가 중요하다.On the other hand, if the shrinkage occurs after the extrusion processing of the optical cable, the optical fiber is not shrunk or bent, there is a risk of optical loss. Therefore, the crystallization rate of PBT is important because it must be able to crystallize within a short time to prevent shrinkage of the optical cable after extrusion processing.
이와 같이 본 발명에 따른 PBT는 기존의 고점도 PBT에 비해 동일조건에서 압출부하는 낮고 결정화 속도가 빠르며, 용융유동지수가 7 내지 15 g/10 min이므로 종래에 비해 압출속도가 약 30% 향상되며, 빠른 결정화 속도로 인해 광케이블 압출가공 후 수축을 줄일 수 있다.As described above, the PBT according to the present invention has a lower extrusion load and faster crystallization rate under the same conditions as the conventional high viscosity PBT, and has a melt flow index of 7 to 15 g / 10 min, thereby improving the extrusion rate by about 30% compared to the conventional method. The fast crystallization rate can reduce shrinkage after fiber optic extrusion.
이하, 본 발명을 실시예에 의거하여 상세하게 설명하겠는바, 본 발명이 다음 실시예에 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited to the following Examples.
실시예 1 ∼ 3Examples 1-3
중합 초기에 원부 원료로 디메틸 테레프탈레이트(DMT)와 부탄디올(1,4-BD)을 투입하여 용융유동지수가 60 ∼ 70 g/10 min, 고유점도가 0.84 ∼ 0.85㎗/g인 PBT를 제조한 후 다음 표 1에서와 같이 윤활제로 칼슘 스테아레이트를 투입하고 핵제로 디메틸테레프탈로일디옥시디벤조에이트를 첨가하여 이축 용융 혼련압축기(twin screw extruder)[W&P사의 ZSK25]로 마스터 배치를 제조하였다. 제조된 마스터 뱃치를 원료로 회전식 증발건조기(Rotary evaporator)[자체 제작]를 사용하여 185 ℃에서 12시간 동안 고상중합을 수행함으로써 다음 표 1과 같은 용융유동지수와 고유점도를 갖는 고점도의 PBT 수지를 제조하였다.Dimethyl terephthalate (DMT) and butanediol (1,4-BD) were added as raw materials at the beginning of the polymerization to prepare PBT having a melt flow index of 60 to 70 g / 10 min and an intrinsic viscosity of 0.84 to 0.85 dl / g. Next, calcium stearate was added as a lubricant as shown in Table 1, and dimethyl terephthaloyldioxydibenzoate was added as a nucleating agent to prepare a master batch using a twin screw extruder (ZSK25 by W & P). By using a rotary evaporator (self-produced) as a raw material, the prepared master batch was subjected to solid phase polymerization at 185 ° C for 12 hours to obtain a high viscosity PBT resin having a melt flow index and intrinsic viscosity as shown in Table 1 below. Prepared.
실시예 4 ∼ 6Examples 4-6
다음 표 1에서와 같이 윤활제로 칼슘 스테아레이트를 투입하고 핵제로 디메틸테레프탈로일디옥시디벤조에이트를 첨가하여 상기 실시예 1과 동일한 방법으로 고점도 PBT 수지를 제조하였다. 이때, 고상중합 수행 후 용융유동지수와 고유점도는 다음 표 1과 같이 나타났다.Next, calcium stearate was added as a lubricant and dimethyl terephthaloyldioxydibenzoate was added as a nucleating agent to prepare a high viscosity PBT resin in the same manner as in Example 1. At this time, the melt flow index and intrinsic viscosity after the solid state polymerization was shown in Table 1.
비교예 1Comparative Example 1
용융중합 후 윤활제와 핵제를 첨가하기 위한 압출공정을 거치지 않고 고상중합을 수행하여 용융유동지수가 11.1 g/10 min, 고유점도가 1.25 ㎗/g인 것을 제외하고는 상기 실시예 1과 동일한 방법으로 고점도 PBT 수지를 제조하였다.After melt polymerization, solid phase polymerization was carried out without the addition of a lubricant and a nucleating agent, and the melt flow index was 11.1 g / 10 min, and the inherent viscosity was 1.25 ㎗ / g. High viscosity PBT resins were prepared.
비교예 2Comparative Example 2
용융중합 후 압출공정을 통해 윤활제로 칼슘 스테아레이트를 0.5 중량% 투입한 것과 고상중합 수행 후 용융유동지수가 10.5 g/10 min, 고유점도가 1.26 ㎗/g인 것을 제외하고는 상기 비교예 1과 동일한 방법으로 고점도 PBT 수지를 제조하였다.Comparative Examples 1 and 1 except that 0.5 wt% of calcium stearate was added as a lubricant through the extrusion process after melt polymerization, the melt flow index was 10.5 g / 10 min, and the intrinsic viscosity was 1.26 ㎗ / g after solid phase polymerization. In the same manner, a high viscosity PBT resin was prepared.
시험예 1Test Example 1
상기 실시예와 비교예에서 제조한 고점도 PBT 수지를 사용하여 광섬유의 자케팅을 하는 압출공정에서 압출부하의 기준이 될 수 있도록 전단 속도에 따른 전단 점도를 모세관 점도계(Capillary Rheometer)[ROSAND사의 RH7]를 사용하여 측정하였다. 상기 실시예 1 ∼ 3과 비교예 1에서 제조한 PBT 수지의 전단속도에 따른 전단점도를 260 ℃에서 전단속도에 따라 측정하여 다음 표 2에 나타내었다.Shear viscosity according to shear rate is capillary rheometer (Capillary Rheometer) [ROSH RH7] so as to become the reference of the extrusion load in the extrusion process of the optical fiber jacketing using the high viscosity PBT resin prepared in Examples and Comparative Examples Measured using. The shear viscosity of the PBT resins prepared in Examples 1 to 3 and Comparative Example 1 was measured according to the shear rate at 260 ° C., and is shown in Table 2 below.
상기 표 2에서 알 수 있듯이, 실시예 1 ∼ 3과 같이 윤활제를 투입했을 경우에는 동일 온도에서 각 전단속도에서의 전단점도가 낮은 것을 볼 수 있지만, 비교예 1과 같이 윤활제를 투입하지 않은 경우 전단점도가 높게 나타남을 확인할 수 있었다. 따라서, 적당량의 윤활제를 첨가하여 제조할 경우, 고속압출 가공시 전단점도를 낮춤으로써 생산성을 향상시킬 수 있다.As shown in Table 2, when the lubricant is added as in Examples 1 to 3, it can be seen that the shear viscosity at each shear rate at the same temperature is low, but when the lubricant is not added as in Comparative Example 1 It was confirmed that the viscosity is high. Therefore, when manufacturing by adding an appropriate amount of lubricant, it is possible to improve the productivity by lowering the shear viscosity during high-speed extrusion processing.
시험예 2Test Example 2
상기 실시예 4 ∼ 6과 비교예 1, 2에서 제조한 고점도 PBT의 결정화 속도상수를 측정하기 위해 테스트 시료를 샘플링한 후 시차열분석기[Perkin-Elmer사의DSC7]에 넣고 상온에서 250 ℃까지 가열하여 충분히 용융한 후 195 ℃로 급속히 냉각하여 등온 상태에서 결정화하여 측정하였으며, 그 결과를 다음 표 3 에 나타내었다.In order to measure the crystallization rate constants of the high viscosity PBT prepared in Examples 4 to 6 and Comparative Examples 1 and 2, the test samples were sampled and placed in a differential thermal analyzer [DSC7 from Perkin-Elmer] and heated to 250 ° C. at room temperature. After melting sufficiently, the mixture was rapidly cooled to 195 ° C. and crystallized in an isothermal state, and the results are shown in Table 3 below.
상기 표 3에서 보는 바와 같이, 핵제로 디메틸테레프탈로일디옥시디벤조에이트를 첨가할 경우 첨가하는 양에 따라 첨가하지 않았을 경우 보다 결정화 속도가 빨라짐을 확인할 수 있었다. 따라서, 고점도 PBT 수지에 윤활제와 함께 적당량의 핵제를 첨가하여 제조할 경우, 빠른 결정화 속도를 가지고 압출부하가 낮아짐으로써 고속압출이 가능해져 가공생산성을 향상시킬 수 있다.As shown in Table 3 above, when dimethyl terephthaloyldioxydibenzoate was added as a nucleating agent, it could be confirmed that the crystallization rate was faster than that when the dimethyl terephthaloyldioxydibenzoate was not added. Therefore, when a suitable amount of nucleating agent is added to the high-viscosity PBT resin together with a lubricant, the extrusion load is lowered with a fast crystallization rate and high-speed extrusion is possible, thereby improving processing productivity.
이상에서 상술한 바와 같이, 본 발명은 PBT 수지의 제조시 적당량의 윤활제와 핵제를 첨가함으로써 고속압출 시 전단점도를 낮추고 결정화 속도를 빠르게 하여 고속압출이 가능하다.As described above, in the present invention, by adding an appropriate amount of lubricant and nucleating agent in the production of PBT resin, high-speed extrusion can be achieved by lowering the shear viscosity and increasing the crystallization rate during the high-speed extrusion.
따라서, 본 발명은 고점도이면서도 빠른 전단속도에서 낮은 전단점도를 가지며 결정화 속도가 빨라 고속압출이 가능한 PBT 수지를 제조함으로써 광섬유 자케팅의 고속압출 생산시 문제가 되는 가공 후 수축과 높은 압출부하를 해결할 수 있다.Therefore, the present invention can solve the post-shrinkage and high extrusion load which are a problem in high-speed extrusion production of optical fiber jacketing by manufacturing PBT resin which has high viscosity and low shear viscosity at high shear rate and fast crystallization rate and thus enables high-speed extrusion. have.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2001-0035103A KR100446473B1 (en) | 2001-06-20 | 2001-06-20 | High Viscosity Poly(butylene terephthalate) for high speed extrusion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2001-0035103A KR100446473B1 (en) | 2001-06-20 | 2001-06-20 | High Viscosity Poly(butylene terephthalate) for high speed extrusion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20020096543A KR20020096543A (en) | 2002-12-31 |
| KR100446473B1 true KR100446473B1 (en) | 2004-09-01 |
Family
ID=27710161
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR10-2001-0035103A KR100446473B1 (en) | 2001-06-20 | 2001-06-20 | High Viscosity Poly(butylene terephthalate) for high speed extrusion |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR100446473B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20220056346A (en) | 2020-10-28 | 2022-05-06 | 코오롱플라스틱 주식회사 | Polybutyleneterephthalate resin composition and method for preparing thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06145632A (en) * | 1992-11-02 | 1994-05-27 | Okura Ind Co Ltd | Polyester hot melt resin composition for inflation molding |
| JPH0716920A (en) * | 1993-07-06 | 1995-01-20 | Toray Ind Inc | Method for successively biaxial orientation of crystalline polymer film |
| JPH07126496A (en) * | 1993-10-28 | 1995-05-16 | Polyplastics Co | Polyester resin composition and molded product therefrom |
| JPH08188643A (en) * | 1995-01-11 | 1996-07-23 | Mitsubishi Chem Corp | Preparation of high viscosity polyester |
| JP2000345014A (en) * | 1999-06-08 | 2000-12-12 | Nippon Shokubai Co Ltd | Polyester resin composition |
| KR20010031150A (en) * | 1997-10-17 | 2001-04-16 | 스타르크, 카르크 | Use of High-Molecular Polyester Moulding Materials |
-
2001
- 2001-06-20 KR KR10-2001-0035103A patent/KR100446473B1/en active IP Right Grant
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06145632A (en) * | 1992-11-02 | 1994-05-27 | Okura Ind Co Ltd | Polyester hot melt resin composition for inflation molding |
| JPH0716920A (en) * | 1993-07-06 | 1995-01-20 | Toray Ind Inc | Method for successively biaxial orientation of crystalline polymer film |
| JPH07126496A (en) * | 1993-10-28 | 1995-05-16 | Polyplastics Co | Polyester resin composition and molded product therefrom |
| JPH08188643A (en) * | 1995-01-11 | 1996-07-23 | Mitsubishi Chem Corp | Preparation of high viscosity polyester |
| KR20010031150A (en) * | 1997-10-17 | 2001-04-16 | 스타르크, 카르크 | Use of High-Molecular Polyester Moulding Materials |
| JP2000345014A (en) * | 1999-06-08 | 2000-12-12 | Nippon Shokubai Co Ltd | Polyester resin composition |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20220056346A (en) | 2020-10-28 | 2022-05-06 | 코오롱플라스틱 주식회사 | Polybutyleneterephthalate resin composition and method for preparing thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20020096543A (en) | 2002-12-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4408022A (en) | Blend of polyalkylene terephthalate and wholly aromatic polyester and process for producing the same | |
| EP0044177A2 (en) | Blend of sulfone polymer and wholly aromatic polyester | |
| EP0154065B1 (en) | Blend of polyalkylene terephthalate and high molecular weight wholly aromatic polyester and process for producing the same | |
| KR940007858B1 (en) | Styrene resin oriented molded product and manufacturing method thereof | |
| JPH01225660A (en) | Polyarylene sulfide resin composition | |
| CN105542135A (en) | Liquid crystal polyester and liquid crystal polyester composition consisting of same | |
| KR100446473B1 (en) | High Viscosity Poly(butylene terephthalate) for high speed extrusion | |
| CN112662139B (en) | High-melt-strength liquid crystal polyester resin composition for film and preparation method thereof | |
| CN113999456A (en) | High-performance weather-proof wear-resistant glass fiber reinforced polypropylene material with low dielectric constant and preparation method thereof | |
| EP0192262B1 (en) | Polycyanoaryl ether films | |
| EP0358135B1 (en) | Polyarylene sulfide resin composition | |
| KR100310911B1 (en) | Polyimide Resin Composition | |
| CN113004663A (en) | Low-dielectric alloy material and preparation method and application thereof | |
| US5340861A (en) | Polyphenylene sulfide composition with improved crystallizing characteristic | |
| JP3034335B2 (en) | Polyarylene sulfide resin composition | |
| CN108219427B (en) | Biological-grade transparent flame-retardant polycarbonate compound and preparation method thereof | |
| KR950001643B1 (en) | Mold and its manufacturing composition in situ composite | |
| US4351751A (en) | Glass fiber reinforced polyethylene terephthalate resin composition | |
| KR100435510B1 (en) | A process for preparing poly(butylene terephthalate) resin | |
| CN115028983A (en) | Low-cost POK/PP alloy with good chemical resistance and preparation method and application thereof | |
| JP2009506144A (en) | Polycarbonate molding composition with improved rheological properties | |
| KR20010036052A (en) | A process for preparing polybutylene terephthalate resin | |
| KR100325442B1 (en) | Polybuthyleneterephthalate resin and optical fiber coating tube | |
| KR100323611B1 (en) | Manufacturing method of high shrinkage polyester bland | |
| JPH0665705B2 (en) | Blend of polyalkylene terephthalate and high molecular weight wholly aromatic polyester and process for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant | ||
| FPAY | Annual fee payment |
Payment date: 20130531 Year of fee payment: 10 |
|
| FPAY | Annual fee payment |
Payment date: 20140609 Year of fee payment: 11 |
|
| FPAY | Annual fee payment |
Payment date: 20150603 Year of fee payment: 12 |
|
| FPAY | Annual fee payment |
Payment date: 20160601 Year of fee payment: 13 |
|
| FPAY | Annual fee payment |
Payment date: 20170605 Year of fee payment: 14 |
|
| FPAY | Annual fee payment |
Payment date: 20180605 Year of fee payment: 15 |