KR0157182B1 - The method of manufacturing polyester master batch - Google Patents
The method of manufacturing polyester master batch Download PDFInfo
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- KR0157182B1 KR0157182B1 KR1019950021482A KR19950021482A KR0157182B1 KR 0157182 B1 KR0157182 B1 KR 0157182B1 KR 1019950021482 A KR1019950021482 A KR 1019950021482A KR 19950021482 A KR19950021482 A KR 19950021482A KR 0157182 B1 KR0157182 B1 KR 0157182B1
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- 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
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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
- C08G63/02—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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- 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
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2310/00—Masterbatches
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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)
- Polyesters Or Polycarbonates (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
본 발명에서는 테레프탈산(TPA)과 에틸렌글리콜(EG)을 촉매 존재하에서 에스테르화 반응을 시키고 인화합물의 존재하에서 중축합 시킨 후 다시 고상중합하여 극한 점도가 0.72∼0.78인 에틸렌테레프탈레이트를 주 반복단위로 하는 폴리에스테르를 제조하여 입경이 1㎜ 이하가 되도록 형상 변경하여 하기 일반식 (Ⅰ)로 표현되는 스카이블루 색상의 안료와 혼련함으로써 스카이블루 색상의 착색용 폴리에스테르 입상물을 제조하였다.In the present invention, terephthalic acid (TPA) and ethylene glycol (EG) are esterified in the presence of a catalyst, and polycondensation is carried out in the presence of a phosphorus compound. To prepare a polyester to change the shape so that the particle diameter is 1mm or less and kneaded with the pigment of the sky blue color represented by the following general formula (I) to prepare a polyester granules for coloring of the sky blue color.
Description
본 발명은 생수를 포함하는 음료수용 착색 폴리에스테르 중공 성형체를 제조하기 위한 착색 폴리에스테르 입상물(master batch)의 제조방법에 관한 것으로, 좀 더 구체적으로는 주 반복 단위가 에틸렌테레프탈레이트인 열가소성 성형 폴리에스테르에 하기 일반식(Ⅰ)로 표현되는 스카이블루 생삭의 안료와 혼합하여 용융 혼련시킨 착색용 폴리에스테르 입상물(master batch)의 제조방법에 관한 것이다.The present invention relates to a method for producing a colored polyester master batch for producing a colored polyester hollow molded article for drinking water containing bottled water, and more particularly, a thermoplastic molded poly with a main repeating unit of ethylene terephthalate. The present invention relates to a method for producing a colored polyester masterbatch (master batch) obtained by mixing and mixing and kneading a pigment of SkyBlue raw green represented by the following general formula (I) to an ester.
폴리에틸렌테레프탈레이트 및 이것을 주체로 하는 폴리에스테르는 기계적, 화학적 성질이 우수하기 때문에 섬유, 필름, 중공용기 등의 성형물에 광범위하게 이용되어 왔고, 특히, 블로잉(Blowing) 성형 기술의 진전에 따라 여러가지 착색방법에 따른 착색 중공 성형물이 개발되어 왔다.Polyethylene terephthalate and its main polyester have been widely used in moldings such as fibers, films and hollow containers because of their excellent mechanical and chemical properties, and in particular, various coloring methods according to the development of blowing molding technology. Colored hollow moldings have been developed.
종래, 착색 폴리에스테르 성형품의 제조방법으로는 영국특허 제610,137호 일본특공 소43-13475호, 일본특공 소47-10861호, 일본 특개 소55-149344호 등에 폴리에스테르의 중합공정에서 에틸렌글리콜 등의 다가 알콜계 용매의 분산액에 안료를 분산 첨가하는 방법이 알려져 있으나, 안료는 슬러리(slurry)의 분산성 때문에 균일성을 기하기 어렵고, 제품 성형시 큰 입자를 제거하기 위하여 폴리머 여과를 실시하여야 하며 여과제의 교환빈도가 높고 폴리머의 수율을 저하시켜 생산원가의 상승을 초래하게 되며 큰 입자가 성형품중에 포함되어 있으면 불량품이 발생하고 제품 착색도에 얼룩이가 발생하여 상품가치를 저하시키는 결점이 있다.Conventionally, methods for producing colored polyester molded articles include ethylene glycol and the like in the polymerization process of polyester in British Patent No. 610,137, Japanese Patent Application No. 43-13475, Japanese Patent Application No. 47-10861, and Japanese Patent Application No. 55-149344. Although a method of dispersing a pigment in a dispersion of a polyhydric alcohol-based solvent is known, it is difficult to achieve uniformity due to the dispersion of a slurry, and a polymer filtration must be performed to remove large particles when forming a product. The exchange rate of the problem is high and the yield of the polymer is lowered, which leads to an increase in the production cost. If large particles are included in the molded article, defective products are generated and staining occurs in the product coloration, thereby lowering the product value.
착색제를 중합관에 투입하여 착색 폴리에스테르를 제조하는 방법은 반응물의 오염과 반응제어면에서 어려움이 있다.The method of preparing a colored polyester by adding a colorant to a polymerization tube is difficult in terms of contamination of the reactants and reaction control.
또한 테레프탈산(TPA)을 원료로 하는 폴리에스테르 제조시 착색제를 에틸렌글리콜에 충분히 분산시켜 반응관에 주입하면 착색제가 재응집하여 성형공정에서 작업성이 크게 떨어지고 불량품의 발생이 많아지는 결점이 있다.In addition, when preparing a polyester using terephthalic acid (TPA) as a raw material, if the colorant is sufficiently dispersed in ethylene glycol and injected into the reaction tube, the colorant is reaggregated and the workability is greatly reduced in the molding process, and defects occur more frequently.
또한 착색 성형물의 미적감각을 향상시키기 위해 첨가한 착색제가 비위생적이거나 사용도중 착색제의 일부가 밖으로 용출되어 비위생적인 문제를 자아낸다.In addition, the colorant added to improve the aesthetics of the colored molding is unsanitary or some of the colorant elutes out during use, causing unsanitary problems.
따라서, 본 발명의 목적은 폴리에스테르 원착 입상물(master batch)을 제조하고, 이를 일반 폴리에스테르 칩과 혼합 사용함으로써 착색된 폴리에스테르 성형품을 제공함에 있다.Accordingly, it is an object of the present invention to provide a colored polyester molded article by preparing a polyester master batch and mixing the same with a general polyester chip.
이에 본 발명자들은 연구를 거듭한 결과 특정의 착색제를 고분산화 하여 착색 폴리에스테르 입상물을 제조하고 위생적으로 제조된 미착색 폴리에스테르와 일정 비율로 혼합하여 블로잉(Blowing) 성형기로 성형하면 이러한 제반 문제점을 해결하는 스카이블루 색상의 중공 송형물을 얻을 수 있게 되었다.Therefore, the inventors of the present invention have repeatedly studied to prepare a colored polyester granules by highly dispersing a specific colorant, and to mix them with a hygienically manufactured uncolored polyester in a proportion to form a blow molding machine to solve these problems. It is now possible to obtain a sky blue colored hollow pine tree.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명에서는 테레프탈산(TPA)과 에틸렌글리콜(EG)을 촉매 존재하에서 에스테르화 반응을 시키고 인화합물의 존재하에서 중축합 시킨 후 다시 고상중합하여 극한 점도가 0.72∼0.78인 에틸렌테레프탈레이트를 주 반복단위로 하는 폴리에스테르(이하 폴리에스테르[A]라고 한다)를 사용하여 입경이 1㎜ 이하가 되도록 형상 변경하고 하기 일반식 (Ⅰ)의 구조를 갖는 스카이블루 색상의 안료 0.1∼3중량%를 첨가하여 혼련함으로써 스카이블루 색상의 폴리에스테르 원착 입상물을 얻게 된다.In the present invention, terephthalic acid (TPA) and ethylene glycol (EG) are esterified in the presence of a catalyst, and polycondensation is carried out in the presence of a phosphorus compound. Using a polyester (hereinafter referred to as polyester [A]) to change the shape so that the particle diameter is 1mm or less, kneading by adding 0.1 to 3% by weight of a pigment of sky blue color having a structure of the following general formula (I) This resulted in a sky blue polyester native granular material.
만일, 상기 일반식 (Ⅰ)로 표현되는 안료의 사용량이 0.1중량% 미만이면 분산성은 양호하지만 성형성이 불량하고, 3중량% 초과이면 성형성은 양호하지만 분산성이 취약하게 된다.If the amount of the pigment represented by the general formula (I) is less than 0.1% by weight, the dispersibility is good, but the moldability is poor, and if it is more than 3% by weight, the moldability is good but the dispersibility becomes weak.
또한 본 발명에서 사용하는 일반식(Ⅰ)의 구조를 갖는 안료로는 일본 다이이찌가세이고교의 군청(群靑, Ultramarine) No.8000을 사용하는 것이 바람직하다.In addition, it is preferable to use the ultramarine No. 8000 of Daiichi Chemical Co., Ltd. of Japan as a pigment which has a structure of General formula (I) used by this invention.
폴리에스테르와 안료의 혼합성을 높이기 위해 혼련기내에서 일정수준 이상의 분산도를 얻는 시간을 최대한 짧게 하여 폴리에스테르의 열분해를 방지하고, 폴리에스테르에 쉽게 습윤 분산되는 착색제를 선택 사용함으로써 고분산화 된 본 발명 폴리에스테르 원착 입상물을 제조할 수 있다.The present invention is highly dispersed by using a colorant which is easily wet-dispersed in polyester by preventing the thermal decomposition of the polyester by shortening the time for obtaining a certain level of dispersion in the kneader to increase the blendability of the polyester and the pigment as much as possible. Polyester native granules can be produced.
상기와 같은 고분산화된 폴리에스테르 원착 입상물(master batch)을 제조시 고분산성을 얻기 위하여 트윈 익스투르더(Twin-Extruder)를 사용한다.Twin-Extruder is used to obtain high dispersibility when preparing the highly dispersed polyester master granules (master batch) as described above.
이와같이 하여 제조한 본 발명 착색 폴리에스테르 입상물과 미착색 폴리에스테르[A]를 일정비율로 혼합하고 블로잉 성형기로 성형하여 원하는 색상의 중공성형체를 제조할 수 있다.The colored polyester granules of the present invention thus prepared and the uncolored polyester [A] may be mixed at a predetermined ratio and molded by a blow molding machine to produce a hollow molded product of a desired color.
이하 실시예를 들어 본 발명을 상세히 설명한다.The present invention will be described in detail with reference to the following Examples.
[실시예 1]Example 1
극한점도가 0.78인 폴리에스테르[A]를 입경이 1㎜이하가 되도록 형상 변경시킨 입상(粒狀) 변경분 99.65wt%에 스카이블루 색상의 안료로서 일본 다이이찌가세히고교 제품중 일반식 Na6Al6Si6O24S4인 군청(群靑, Ultramarine) No.8000 0.35wt%를 첨가하고 충분히 혼합하고 이 혼합물을 용융혼련기에서 270℃ 부근에서 50초간 처리하여 착색용 폴리에스테르 입상물 칩을 제조하였다.99.65wt% of the granular change obtained by changing the shape of polyester [A] having an intrinsic viscosity so as to have a particle diameter of 1 mm or less as a pigment of sky blue color as general formula Na 6 in Daiichi Kasehigyo Co., Ltd. 0.35wt% of Ultramarine No. 8000 Al 6 Si 6 O 24 S 4 was added and thoroughly mixed, and the mixture was treated in a melt kneader at about 270 ° C. for 50 seconds to color polyester granule chips. Was prepared.
이 입상물 칩 5중량부와 폴리에스테르[A] 150중량부를 혼합하여 블로잉 성형기로 성형하여 분산성이 우수하고 스카이블루 색상의 중공성형 용기를 제조하고 물성을 평가하여 그 결과를 표 2에 나타내었다.5 parts by weight of this granular material chip and 150 parts by weight of polyester [A] were mixed and molded by a blow molding machine to prepare a hollow molded container having excellent dispersibility and sky blue color, and evaluated the physical properties thereof. The results are shown in Table 2. .
[실시예 2∼3, 비교예 1∼2][Examples 2-3 and Comparative Examples 1-2]
표 1에 기재한 바와 같이 폴리에스테르 입상변경분, 스카이블루 색상의 안료로서 일본 다이이찌가세이고교 제품인 일반식 Na6Al6Si6O24S4인 군청(群靑, Ultramarine) No.80000의 혼합비율을 변경한 것을 제외하고는 실시예 1과 동일하게 실시하여 그 결과를 표 2에 나타내었다.As shown in Table 1, the ultramarine No.80000 which is a general formula Na 6 Al 6 Si 6 O 24 S 4 manufactured by Daiichigase Kogyo Co., Ltd. as a pigment of polyester granular change and sky blue color Except for changing the mixing ratio was carried out in the same manner as in Example 1 and the results are shown in Table 2.
물성평가Property evaluation
1) 용출시험 : 제조된 중공성형 용기에 증류수, n-헵단, 50% 에탄올을 각각 250℉에서 2시간, 150℉에서 2시간, 120℉에서 24시간 동안 담아 놓은 뒤 클로로포름 추출량을 나타냈다.1) Dissolution test: Distilled water, n-heptane, and 50% ethanol were placed in a prepared hollow molded container for 2 hours at 250 ° F, 2 hours at 150 ° F, and 24 hours at 120 ° F, respectively.
2) 분산성 : SEM으로 용기 표면을 관찰하여 2㎛ 이상의 안료 응집체가 나타나면 불량, 2㎛ 미만의 안료 응집체가 발견되면 양호.2) Dispersibility: When the surface of the container is observed by SEM and the pigment aggregate of 2 µm or more appears, it is poor.
3) 성형성 : 외관상 평가3) Formability: Appearance Evaluation
4) 아세트 알데히드 함량 : 성형병(Bottle) 내부에 질소가스로 충진한 후 24시간 동안 220℃ 이하에서 방치한 후 병(Bottle) 내부의 질소가스 속에 포함되어 있는 아세트 알데히드 함량을 시마주 지이시-9에이(SHIMADZU GC-9A)로 측정.4) Acetaldehyde content: After filling the bottle with nitrogen gas and leaving it at 220 ℃ or lower for 24 hours, the amount of acetaldehyde contained in the nitrogen gas inside the bottle is made by Shimaju Jishi. Measured with 9 A (SHIMADZU GC-9A).
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| KR970006397A (en) | 1997-02-19 |
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