KR20060035001A - Thermoplastic resin composition - Google Patents
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- KR20060035001A KR20060035001A KR1020040084065A KR20040084065A KR20060035001A KR 20060035001 A KR20060035001 A KR 20060035001A KR 1020040084065 A KR1020040084065 A KR 1020040084065A KR 20040084065 A KR20040084065 A KR 20040084065A KR 20060035001 A KR20060035001 A KR 20060035001A
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- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/06—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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Abstract
본 발명은 이형성이 우수한 ABS계 열가소성 수지 조성물에 관한 것으로, 보다 상세하게는 a) ABS계 그라프트 공중합체 20 ~ 60 중량부; b) 방향족 비닐화합물, 시안화 비닐화합물, 아크릴산의 알킬 에스테르 단량체 및 메타크릴산의 알킬 에스테르 단량체로 이루어진 군에서 선택되는 2종 이상 단량체의 공중합체 40 ~ 80 중량부; 및 c) a)및 b)의 합 100중량부에 대해, 부틸화 하이드록시톨루엔 0.2 ~ 1.5 중량부를 포함하여 이루어지는 열가소성 수지 조성물에 관한 것이다. The present invention relates to an ABS-based thermoplastic resin composition excellent in releasability, and more specifically, a) 20 to 60 parts by weight of an ABS-based graft copolymer; b) 40 to 80 parts by weight of a copolymer of two or more monomers selected from the group consisting of aromatic vinyl compounds, vinyl cyanide compounds, alkyl ester monomers of acrylic acid and alkyl ester monomers of methacrylic acid; And c) 0.2 to 1.5 parts by weight of butylated hydroxytoluene, relative to 100 parts by weight of the total of a) and b).
본 발명에 따른 열가소성 수지 조성물은 0.5중량부 이상의 이형제를 첨가하여 배합시에도 기존의 이형제보다도 수지의 열안정성 및 이형성이 우수하다.The thermoplastic resin composition according to the present invention is more excellent in thermal stability and mold release property of the resin than the conventional mold release agent even when added by adding 0.5 parts by weight or more of a release agent.
이형성, 이형제, 부틸화 하이드록시톨루엔, 열가소성 수지, 사출압Release property, release agent, butylated hydroxytoluene, thermoplastic resin, injection pressure
Description
본 발명은 이형성이 우수한 ABS계 열가소성 수지 조성물에 관한 것으로, 보다 상세하게는 이형제로서 부틸화 하이드록시톨루엔(BHT)을 포함하여 이루어지는 ABS계 열가소성 수지 조성물에 관한 것이다. The present invention relates to an ABS thermoplastic resin composition having excellent release properties, and more particularly, to an ABS thermoplastic resin composition comprising butylated hydroxytoluene (BHT) as a release agent.
아크릴로니트릴-부타디엔-스티렌(이하 ABS라 함) 공중합체 수지는 내충격성, 강성한 정도의 물성 밸런스, 내약품성, 성형가공성, 광택 등이 우수한 것으로 OA기기, 가전제품, 일반 잡화 등의 용도로 사출 성형용 수지로서 폭넓게 이용되고 있고, 장난감의 재료로도 널리 사용되어지고 있다. 이들 분야에서 사용된 성형품은 일반적으로 사출성형, 압축 성형 등에 의해 얻을 수 있지만, 높은 치수 정밀도가 요구된 성형품이나 복잡한 형상을 갖는 성형품을 성형한 경우, 성형품이 금형 등에 부착되어 생산성의 저하, 성형품의 변형 등 외관 불량이 생길 수가 있다.Acrylonitrile-butadiene-styrene (hereinafter referred to as ABS) copolymer resin is excellent in impact resistance, rigid balance of physical properties, chemical resistance, molding processability, gloss, etc. and is used for OA devices, home appliances, general goods, etc. It is widely used as an injection molding resin, and is also widely used as a toy material. Molded articles used in these fields can generally be obtained by injection molding, compression molding, etc., but when molded articles having high dimensional accuracy or molded articles having complex shapes are molded, the molded articles are attached to a mold or the like to reduce productivity, Appearance defects such as deformation may occur.
이러한 이형성의 불량은 적절한 가공 조건의 변경에 의하여 해결되어질 수 있기는 하지만 대부분 성형조건의 변경 만으로는 해결하기가 어렵다. 또한 성형조건의 변경으로 해결한 경우에도 성형 사이클의 소요시간이 길어져 생산성이 저하되는 단점을 가지게 된다. Although the defects of the releasability can be solved by changing the appropriate processing conditions, most of them are difficult to solve only by changing the molding conditions. In addition, even if solved by the change of the molding conditions it takes a long time of the molding cycle has the disadvantage that the productivity is lowered.
또 다른 해결방법으로는 일반적으로 금형에 이형제를 도포하는 방법을 사용한다. 하지만 이 경우에 어린이 들이 사용하는 장난감제품을 성형 할 시에는 성형품 외관에 이형제 성분이 남아있어 안전상에 영향을 미칠 수가 있다. Another solution is to apply a release agent to the mold in general. However, in this case, when molding a toy product used by children, the release agent component may remain on the appearance of the molded article, which may affect safety.
또한 수지에 미리 이형제를 배합하여 수지의 이형성을 개선한 것이 행해지고 있다. 이러한 목적으로 사용되는 이형제로는 고급지방산, 고급지방산의 금속염, 폴리 옥시 프로필렌글리콜류, 실리콘 오일 등이 알려져 있다. 하지만 이 경우에 0.5 중량부 이상의 이형제를 첨가하여 배합할 시에 수지 자체의 기본 물성 밸런스를 파괴할 수 있고, 첨가되고 있는 이형제가 수지 표면으로 이행하여 금형 표면 및 성형품 표면을 오염시키거나 수지의 열안정성을 악화시키고 성형품의 착색을 가져올 수 있으며 나아가서는 성형품의 열변형 온도를 저하시키는 등의 문제를 발생시킬 수 있다. Moreover, what improved the mold release property of resin by mix | blending a mold release agent with resin previously is performed. As the release agent used for this purpose, higher fatty acids, metal salts of higher fatty acids, polyoxypropylene glycols, silicone oils and the like are known. However, in this case, when adding 0.5 parts by weight or more of release agent, the basic physical property balance of the resin itself may be destroyed, and the added release agent may migrate to the resin surface to contaminate the mold surface and the molded article surface or to heat the resin. It may deteriorate the stability and bring about the coloring of the molded article, and may cause problems such as lowering the heat deformation temperature of the molded article.
본 발명은 상기 종래의 기술의 문제점을 고려하여, 0.5 중량부 이상의 이형제를 첨가하여 배합시에도 기존의 이형제를 배합할 때 보다 수지의 열안정성 및 이형성이 우수한 ABS계 열가소성 수지 조성물을 제공하는 것을 목적으로 한다. SUMMARY OF THE INVENTION In view of the problems of the prior art, an object of the present invention is to provide an ABS-based thermoplastic resin composition having more excellent thermal stability and mold release property than the conventional release agent when compounding by adding a release agent of 0.5 parts by weight or more. It is done.
상기 목적을 달성하기 위하여, 본 발명은 In order to achieve the above object, the present invention
a) ABS계 그라프트 공중합체 20 내지 60중량부;a) 20 to 60 parts by weight of ABS-based graft copolymer;
b) 방향족 비닐화합물, 시안화 비닐화합물, 아크릴산의 알킬 에스테르 단량체 및 메타크릴산의 알킬 에스테르 단량체로 이루어진 군에서 선택되는 2종 이상 단량체의 공중합체 40 내지 80 중량부; 및b) 40 to 80 parts by weight of a copolymer of two or more monomers selected from the group consisting of aromatic vinyl compounds, vinyl cyanide compounds, alkyl ester monomers of acrylic acid and alkyl ester monomers of methacrylic acid; And
c) 상기 a)및 b)의 합 100중량부에 대해, 부틸화 하이드록시톨루엔 0.2 내지 1.5중량부c) 0.2 to 1.5 parts by weight of butylated hydroxytoluene based on 100 parts by weight of the sum of a) and b)
를 포함하여 이루어지는 것을 특징으로 하는 열가소성 수지 조성물을 제공한다.It provides a thermoplastic resin composition comprising a.
이하, 본 발명에 대해 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
상기 열가소성 수지 조성물에서 ABS계 그라프트 공중합체는 입자경이 2,500 내지 4,000Å이고, 겔함량이 70 내지 85%이며, 팽윤지수가 12 내지 30인 폴리부타디엔 고무라텍스 30 내지 60중량부에 방향족 비닐화합물 및 비닐시안 화합물로 이루어진 군으로부터 2종 이상 선택되는 단량체 혼합물 40 내지 70중량부를 투여하여 통상적인 그라프트 유화중합 방법으로 제조된다. 이때, 상기 단량체 혼합물의 5 내지 30중량%는 일괄투여하고 70 내지 95 중량%는 유화된 상태로 연속 투여하는 단계를 거친다.In the thermoplastic resin composition, the ABS-based graft copolymer has an aromatic vinyl compound having a particle size of 2,500 to 4,000 kPa, a gel content of 70 to 85%, and a polybutadiene rubber latex having a swelling index of 12 to 30 in an amount of 30 to 60 parts by weight. 40 to 70 parts by weight of a monomer mixture selected from the group consisting of vinyl cyan compounds is administered to prepare a conventional graft emulsion polymerization method. At this time, 5 to 30% by weight of the monomer mixture is administered in a batch and 70 to 95% by weight is subjected to continuous administration in an emulsified state.
상기 열가소성 수지 조성물에서 방향족 비닐화합물, 시안화 비닐화합물, 아크릴산의 알킬 에스테르 단량체 및 메타크릴산의 알킬 에스테르 단량체로 이루어진 군에서 선택되는 2종 이상 단량체의 공중합체는 시안화 비닐화합물과 방향족 비닐화합물의 공중합체가 바람직하다. In the thermoplastic resin composition, the copolymer of two or more monomers selected from the group consisting of an aromatic vinyl compound, a vinyl cyanide compound, an alkyl ester monomer of acrylic acid and an alkyl ester monomer of methacrylic acid is a copolymer of a vinyl cyanide compound and an aromatic vinyl compound. Is preferred.
시안화 비닐화합물과 방향족 비닐화합물의 공중합체의 중량평균 분자량은 일반적인 가공조건에서 50,000 내지 150,000가 바람직하다. 중량평균 분자량이 50,000미만일 경우에는 제품에서 요구되는 구조 강성을 유지하기가 어렵고 제품 사 용시 내구성에 문제가 발생하며, 150,000 초과할 경우에는 사출가공성이 낮아지게 되고 소형이나 정밀 제품의 사출에 문제가 발생할 수 있다. 상기 열가소성 수지 조성물에서 이형제로서 사용되는 부틸화 하이드록시톨루엔(Butylated Hydroxy Toluen , BHT)으로는 2,6-디-터셔리-부틸-4메틸페놀, 2,6-디-터셔리-부틸-파라-크레졸, 씨오디에틸렌 비스[3-(3,5- 디-터셔리-부틸-4-히드록시페닐)프로피오네이트] 등을 예로 들 수 있고, 그중에서 2,6-디-터셔리-부틸-파라-크레졸이 바람직하다.The weight average molecular weight of the copolymer of the vinyl cyanide compound and the aromatic vinyl compound is preferably 50,000 to 150,000 under general processing conditions. If the weight average molecular weight is less than 50,000, it is difficult to maintain the structural rigidity required in the product, and there is a problem in durability when using the product. If the weight average molecular weight exceeds 150,000, the injection processability is lowered, and a problem occurs in the injection of small or precision products. Can be. Butylated Hydroxy Toluen (BHT) used as a release agent in the thermoplastic resin composition is 2,6-di-tert-butyl-4methylphenol, 2,6-di-tert-butyl-para -Cresol, ciodiethylene bis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], and the like, among which 2,6-di-tertiary- Preference is given to butyl-para-cresol.
상기 열가소성 수지 조성물은 활제 및 산화방지제로 이루어진 군에서 선택되는 1이상의 첨가제를 포함하여 이루어질 수 있다.
The thermoplastic resin composition may include one or more additives selected from the group consisting of lubricants and antioxidants.
본 발명의 실시예와 비교예에서 실시한 물성 측정은 아래의 방법으로 행하였다.The physical properties measured in Examples and Comparative Examples of the present invention were performed by the following method.
이형성은 사출기의 최소사출압과 최대사출압의 차이(△사출압)로 나타내었다. Releasability was expressed as the difference between the minimum injection pressure and the maximum injection pressure (△ injection pressure) of the injection molding machine.
이형성 실험 전에 앞서서 시료의 수분함량을 0.2%이하로 낮추기 위해서 80~90℃ 고온 오븐에서 최소 2시간 이상 건조하였다. Prior to the release test, the sample was dried at least 2 hours in a high temperature oven at 80-90 ° C. in order to lower the moisture content of the sample to 0.2% or less.
사출기는 ENGEL사의 제품을 사용하였고, 금형사출온도 230℃, 금형온도 26℃, 스크류(screw) RPM은 130인 조건으로 사출압을 60bar부터 시작해서 사출을 시작하였다. 사출시 금형설계상 금형에서 마지막으로 수지가 채워지는 부분에서 나오는 사출성형품의 모양을 살펴보면서 사출성형품의 미성형 여부를 확인하였다. 미성형이 나왔을 경우는 전 사출압에서 0.5bar 올리고 사출을 하였다. 이런 방법을 되풀이 하여 미성형이 나지 않는 최초의 사출압을 기록하였고, 이 때의 사출압이 최소 사출압이다.The injection machine used ENGEL's product, and the injection pressure was started from 60bar with the injection mold temperature 230 ℃, mold temperature 26 ℃ and screw RPM of 130. In the mold design during injection, the shape of the injection molded product coming out of the last resin-filled part of the mold was checked to determine whether the injection molded product was unmolded. In case of unmolding, injection was performed at 0.5 bar at full injection pressure. This method was repeated to record the first injection pressure without any molding, and the injection pressure at this time is the minimum injection pressure.
최소 사출압을 측정한 후 약 40bar의 사출압을 올려서 사출을 하고 사출 후 사출 성형품이 금형에서 이형되어지는 것을 관찰한 후 이형이 확실히 이루어 지면 이 때부터 0.5bar씩 사출압을 올리면서 사출성형품의 이형 여부를 확인하였다. 이형이 이루어지지 않고 사출성형품이 금형에 끼어 있게 될때의 사출압을 측정하였고 이 때의 사출압이 최대사출압이다.After measuring the minimum injection pressure, the injection pressure is increased to about 40 bar, and after injection, the injection molded product is observed to be released from the mold. When the mold release is certain, the injection pressure is increased by 0.5 bar from this time. Check for release. The injection pressure is measured when the injection molded product is stuck in the mold without mold release, and the injection pressure at this time is the maximum injection pressure.
이렇게 측정되어진 최대사출압과 최소사출압의 차이가 이형성을 측정하는 수치가 된다. 즉 사출압에 따라서 사출성형품의 이형 여부가 결정이 되는데 최대 사출압과 최소 사출압의 차이(△사출압)가 클수록 수지의 이형되어지는 사출영역이 넓어지게 되고 따라서 수지의 이형성도 향상되어진다는 것을 의미하게 된다.
The difference between the maximum injection pressure and the minimum injection pressure, which is measured in this way, is a measure of the dysplasia. In other words, it is determined whether or not the injection molded product is released according to the injection pressure. The greater the difference between the maximum injection pressure and the minimum injection pressure (△ injection pressure), the wider the injection zone where the resin is released, and thus the releasability of the resin is improved. Will mean.
체류 열안정성은 230℃에서 사출한 시편과 250℃ 15분 체류 후 사출한 시편의 색차를 비교하였다. 시편의 색차가 작을수록 열안정성이 우수함을 의미하게 된다.
The retention thermal stability was compared with the color difference between the specimen injected at 230 ° C. and the specimen injected after 250 ° C. for 15 minutes. The smaller the color difference of the specimen, the better the thermal stability.
이하, 본 발명을 하기의 실시예 및 비교예를 통하여 보다 상세히 설명한다. 그러나, 이들 예는 본 발명을 예시하기 위한 것일 뿐, 본 발명이 이에 제한되는 것은 아니다.
Hereinafter, the present invention will be described in more detail with reference to the following examples and comparative examples. However, these examples are only for illustrating the present invention, but the present invention is not limited thereto.
[실시예 및 비교예][Examples and Comparative Examples]
실시예 및 비교예에 사용된 1) ABS계 그라프트 공중합체, 2) 시안화 비닐화합물과 방향족 비닐화합물의 공중합체 3) 부틸화 하이드록시톨루엔(BHT)은 다음과 같다.1) ABS graft copolymers used in Examples and Comparative Examples, 2) copolymers of vinyl cyanide compounds and aromatic vinyl compounds 3) Butylated hydroxytoluene (BHT) is as follows.
1) ABS계 그라프트 공중합체 1) ABS Graft Copolymer
질소 치환된 중합반응기에 입자경이 2,900 Å이고 겔함량이 75%이며, 팽윤지수가 12 내지 30인 폴리부타디엔 고무라텍스 45 중량부에 이온교환수 100 중량부, 로진산 칼륨 유화제 0.4 중량부, 스티렌 9.6 중량부, 아크릴로니트릴 4.1 중량부, 덱스트로즈 0.2 중량부, 황화제1철 0.003 중량부 및 큐멘하이드로퍼옥사이드 0.09 중량부를 45 ℃에서 일괄투여하고 반응온도를 70℃까지 1 시간에 걸쳐서 상승시키면서 유화 중합반응을 시켰다.In the nitrogen-substituted polymerization reactor, 45 parts by weight of polybutadiene rubber latex having a particle diameter of 2,900 mm, a gel content of 75%, and a swelling index of 12 to 30, 100 parts by weight of ion-exchanged water, 0.4 part by weight of potassium rosin emulsifier, and styrene 9.6 By weight, 4.1 parts by weight of acrylonitrile, 0.2 parts by weight of dextrose, 0.003 parts by weight of ferrous sulfide and 0.09 parts by weight of cumene hydroperoxide were collectively administered at 45 ° C. while the reaction temperature was raised to 70 ° C. over 1 hour. Emulsion polymerization was carried out.
그리고 여기에 이온교환수 30 중량부, 로진산 칼륨 1.3 중량부, 스티렌 28.9 중량부, 아크릴로니트릴 12.4 중량부, 3급 도데실메르캅탄 0.6 중량부 및 큐멘하이드로퍼옥사이드 0.15 중량부의 혼합 유화 용액을 3 시간 동안 연속 투여한 후 다시 80 ℃로 승온한 후 1 시간 동안 숙성시키고 반응을 종료시켰다. And a mixed emulsion solution of 30 parts by weight of ion-exchanged water, 1.3 parts by weight of potassium rosinate, 28.9 parts by weight of styrene, 12.4 parts by weight of acrylonitrile, 0.6 parts by weight of tertiary dodecyl mercaptan and 0.15 parts by weight of cumene hydroperoxide After continuous administration for 3 hours, the temperature was again raised to 80 ° C., and aged for 1 hour, and the reaction was terminated.
이 라텍스를 황산 수용액으로 응집시키고 세척한 다음 분말을 얻는다.The latex is agglomerated with aqueous sulfuric acid solution, washed and then powdered.
2) 시안화 비닐화합물과 방향족 비닐화합물의 공중합체2) Copolymer of Vinyl Cyanide Compound and Aromatic Vinyl Compound
아크릴로니트릴 함량이 28 중량부이고 중량평균 분자량이 100,000인 아크릴로니트릴- 스티렌(SAN) 공중합체수지를 사용하였다.An acrylonitrile-styrene (SAN) copolymer resin having an acrylonitrile content of 28 parts by weight and a weight average molecular weight of 100,000 was used.
3) 부틸화 하이드록시톨루엔(BHT) 3) Butylated Hydroxytoluene (BHT)
ABS계 그라프트 공중합체 및 SAN 공중합체의 합 100중량부에 대해 0.3에서 1.5 중량부의 2.6-디-터셔리-부틸-파라-크레졸을 사용하였다.
0.3 to 1.5 parts by weight of 2.6-di-tertiary-butyl-para-cresol was used relative to 100 parts by weight of the ABS-based graft copolymer and the SAN copolymer.
상기 구성 성분들을 사용하여 표1에 나타난 조성과 같은 수지 조성물을 제조하였다. 실시예 1 ~3 은 본 발명의 수지 조성물에 따른 실시예이고, 비교예 1 은 본 발명에서 이형제로 사용한 부틸화 하이드록시톨루엔 대신에 마그네슘 스테아레이트를 이형제로 사용한 경우이고, 비교예 2는 이형제로 부틸화 하이드록시톨루엔을 사용하되 그 사용량이 0.2중량부 미만인 경우이며, 비교예 3은 이형제로 부틸화 하이드록시톨루엔을 사용하되 그 사용양이 1.5 중량부를 초과한 경우이다. Using the above components to prepare a resin composition, such as the composition shown in Table 1. Examples 1 to 3 are examples according to the resin composition of the present invention, Comparative Example 1 is a case where magnesium stearate is used as a release agent instead of butylated hydroxytoluene used as a release agent in the present invention, Comparative Example 2 is a release agent Butylated hydroxytoluene is used but the amount is less than 0.2 parts by weight, Comparative Example 3 is when butylated hydroxytoluene is used as a release agent, the amount of use exceeds 1.5 parts by weight.
수지 조성물은 활제 3 중량부, 산화방지제 0.2 중량부를 투여하여 220 ℃의 실린더 온도에서 2축 압출혼련기를 사용하여 펠렛 형태로 제조하였다. The resin composition was prepared in pellet form using a twin screw extruder at a cylinder temperature of 220 ° C. by administering 3 parts by weight of lubricant and 0.2 part by weight of antioxidant.
표 1에 실시예 와 비교예 실험결과를 정리하였다. Table 1 summarizes the results of the Examples and Comparative Examples.
이상에서 설명하는 바와 같이, 본 발명의 열가소성 수지 조성물은 0.5 중량부 이상의 이형제를 첨가하여 배합시에도 수지의 열안정성 및 이형성이 우수하다.As explained above, the thermoplastic resin composition of this invention is excellent in the thermal stability and mold release property of resin, even when mix | blending by adding 0.5 weight part or more of a mold release agent.
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| KR101387969B1 (en) * | 2009-12-31 | 2014-04-22 | 제일모직주식회사 | Weatherable Thermoplastic Resin Having Excellent Low Gloss Characteristic and Method of Preparing the Same |
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| KR101387969B1 (en) * | 2009-12-31 | 2014-04-22 | 제일모직주식회사 | Weatherable Thermoplastic Resin Having Excellent Low Gloss Characteristic and Method of Preparing the Same |
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