KR20040027129A - Composition of liquid dispersion containing polyethylene wax with fine particle size for oil-based paint and preparation thereof - Google Patents
Composition of liquid dispersion containing polyethylene wax with fine particle size for oil-based paint and preparation thereof Download PDFInfo
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Abstract
Description
본 발명은 미립자 폴리에틸렌왁스를 포함하는 유성도료용 액상분산체 조성물 및 이의 제조방법에 관한 것이다. 더욱 상세하게는, 유기관능기를 가진 고분자량의 공중합체 용액과 미립자 폴리에틸렌왁스를 매체로 하고 용제 및 필요에 따라 실리카를 배합하여 제조된 액상분산체 조성물 및 이의 제조방법에 관한 것으로서, 상기 분산성 및 저장안정성이 우수한 조성물을 각종 공업용 유성도료에 이용함으로써 도장표면의 슬립성, 내긁힘성(내스크래치성. scratch resistance), 내마모성 및 소광력을 향상시킬 수 있다.The present invention relates to a liquid dispersion composition for an oil paint comprising a particulate polyethylene wax and a method for producing the same. More specifically, the present invention relates to a liquid dispersion composition prepared by mixing a high molecular weight copolymer solution having an organic functional group and particulate polyethylene wax as a medium, and to mixing silica as necessary, and to a method for preparing the same. By using the composition having excellent storage stability in various industrial oil paints, the slip surface, scratch resistance (scratch resistance, scratch resistance), abrasion resistance and matting power of the coating surface can be improved.
종래에 제조된 유성도료용 분산체 조성물 제품들은 평균입자크기가 약 10 ㎛이고 최대입자크기도 30∼40 ㎛로 크기 때문에, 분산이 어렵고 재응집이 일어나기 쉬워 도장 후 표면에 크레터링(cratering: 도막면에 분화구 형태의 흠이 생기는 현상)과 같은 도막 결함을 발생시키는 원인이 되며, 장시간 저장시 입자간의 응집현상 발생 및 칙소성(실끊어짐)이 커져 안정성이 떨어진다.Since conventional dispersion composition products for oil-based paints have an average particle size of about 10 μm and a maximum particle size of 30 to 40 μm, it is difficult to disperse and re-agglomerate easily. (A phenomenon in which crater-shaped flaws occur on the surface), which is a cause of defects in the coating film, and agglomeration phenomenon and thixotropy (brokenness) between particles when the long-term storage increases, resulting in poor stability.
일단 응집된 입자는 도료에 투입되어 재분산되더라도 그 응집을 와해시키기 어려워 입자가 도료표면에 알갱이 형태의 시드(seed)로 존재하며 적용계와 상용성 및 표면물성을 향상시키는데 미흡하다.Once agglomerated particles are added to the paint and re-dispersed, it is difficult to disintegrate the agglomerates, so that the particles exist as granulated seeds on the paint surface and are insufficient to improve compatibility and surface properties with the application system.
따라서, 입자크기가 커서 분산성이 떨어지고 재응집되기 쉬운 종래의 분산체 조성물을 유성도료에 적용할 경우, 유성도료의 필수적인 특징인 슬립성, 내긁힘성 및 내마모성이 불량한 문제점이 있었다.Therefore, when the conventional dispersion composition having a large particle size, which is inferior in dispersibility and easily reaggregated, is applied to an oil paint, there is a problem in that slip properties, scratch resistance, and abrasion resistance, which are essential characteristics of the oil paint, are poor.
따라서, 본 발명의 목적은 입자크기가 미세하고 분산성 및 저장안정성이 우수하여 공업용 유성도료의 슬립성, 내마모성 및 내긁힘성을 향상시킬 수 있는 유성도료용 액상분산체 조성물을 제공하는 것이다.Accordingly, an object of the present invention is to provide a liquid dispersion composition for an oil paint, which has a fine particle size and excellent dispersibility and storage stability, thereby improving slip, wear resistance, and scratch resistance of an industrial oil paint.
본 발명의 다른 목적은 소광력을 부여한 유성도료용 액상분산체 조성물을 제공하는 것이다.Another object of the present invention is to provide a liquid dispersion composition for oil-based paint imparting matting power.
본 발명의 또 다른 목적은 분산성이 우수하고 유성도료의 슬립성, 내마모성, 내긁힘성 및/또는 소광력을 향상시킬 수 있는 유성도료용 액상분산체 조성물을 제조하는 방법을 제공하는 것이다.Still another object of the present invention is to provide a method for preparing a liquid dispersion composition for an oil paint, which is excellent in dispersibility and can improve slip resistance, wear resistance, scratch resistance, and / or matting power of an oil paint.
상기 목적을 달성하기 위한 본 발명의 유성도료용 액상분산체 조성물은 미립자 폴리에틸렌왁스 1 내지 30 중량%, 유기관능기를 가지는 공중합체 용액 1 내지 20 중량% 및 용제 50 내지 97 중량%를 포함하며, 바람직하게는 폴리에틸렌왁스 1 내지 15 중량%, 유기관능기를 가지는 공중합체 용액 1 내지 10 중량% 및 용제 75내지 97 중량%를 포함한다.The liquid dispersion composition for oil paint according to the present invention for achieving the above object comprises 1 to 30% by weight of particulate polyethylene wax, 1 to 20% by weight of a copolymer solution having an organic functional group, and 50 to 97% by weight of a solvent. Preferably from 1 to 15% by weight polyethylene wax, 1 to 10% by weight of the copolymer solution having an organic functional group and 75 to 97% by weight of the solvent.
본 발명의 특징은 유성도료의 슬립성, 내마모성 및 내긁힘성을 향상시키기 위한 것으로, 이러한 목적을 달성하기 위하여 본 발명에서는 폴리에틸렌왁스의 입자를 용제내에서 안정하게 분산시켜 미립화시키며, 구체적으로 폴리에틸렌왁스의 최대입자크기가 1 내지 30 ㎛, 바람직하게는 1 내지 10 ㎛ 이하가 되도록 미세하게 분산시킨다. 최대입자크기가 30 ㎛보다 클 경우 미립자로 인한 분산효과를 기대할 수 없으며, 분산시간이 길어질수록 입자는 미립자화되지만 왁스는 분산이 많이 되면 점도가 높아져 유동성이 떨어지게 되며 더 이상의 분산이 어려워지고 이로 인해 입자간 재응집이 발생할 위험이 있으므로 1 ㎛보다 작은 최대입자크기를 가지는 폴리에틸렌왁스를 제조하기는 어렵다.A characteristic of the present invention is to improve the slip resistance, abrasion resistance and scratch resistance of the oil paint, in order to achieve the object of the present invention in the present invention to stably disperse the particles of polyethylene wax in a solvent, specifically, polyethylene wax It is finely dispersed so as to have a maximum particle size of 1 to 30 µm, preferably 1 to 10 µm or less. If the maximum particle size is larger than 30 μm, the dispersion effect due to the fine particles cannot be expected. The longer the dispersion time, the finer the particles become, but the more the wax is dispersed, the higher the viscosity, the lower the fluidity and the more difficult the dispersion. It is difficult to produce polyethylene wax having a maximum particle size of less than 1 μm because of the risk of particle reaggregation.
또한, 최적의 배합 및 분산조건에 의해 입자분포가 미세하고 균일하며 분산성 및 저장안정성이 보다 향상된 액상분산체를 제조할 수 있으며, 이러한 액상분산체 조성물을 유성도료에 적용할 경우 미립자 폴리에틸렌왁스들이 도막에 균일하게 분포됨으로써 유성도료의 슬립성, 내마모성 및 내긁힘성와 같은 도막의 표면물성을 향상시킬 수 있는 것이다. 본 발명에 따라 폴리에틸렌왁스를 포함한 액상분산체 조성물을 미세하게 분산시키면 평균입자크기가 0.5 내지 6 ㎛인 조성물을 제조할 수 있다. 상기 평균입자크기는 분산배합 및 분산조건에 의해 조절될 수 있다.In addition, it is possible to produce a liquid dispersion with fine and uniform particle distribution and improved dispersibility and storage stability by optimum mixing and dispersing conditions, and when the liquid dispersion composition is applied to an oil paint, particulate polyethylene waxes By being uniformly distributed in the coating film, it is possible to improve the surface properties of the coating film, such as slip resistance, wear resistance and scratch resistance of the oil paint. By finely dispersing the liquid dispersion composition including polyethylene wax according to the present invention, a composition having an average particle size of 0.5 to 6 μm can be prepared. The average particle size may be adjusted by dispersion blending and dispersion conditions.
본 발명에서 사용되는 폴리에틸렌왁스는 천연가스나 나프타를 분해하여 얻어지는 에틸렌과 극성모노머와의 공중합체로서, 산화분해 등 각종 화학변성에 의해 극성기가 부여된 파우더상의 합성왁스이다. 중합방법과 가공공정에 따라 다양한 입자크기와 특성을 가진 여러 유형의 폴리에틸렌왁스가 사용되고 있으나, 본 발명에서는 최대입자크기가 바람직하게는 10 ㎛ 이하로 분산되도록 미세한 폴리에틸렌왁스를 선택한다. 상기 조건을 충족하는 폴리에틸렌왁스로서, 예를 들면 DEUREX사(DEUREX Wachs-Chemie GmbH, 독일)의 PRINTWAX 시리즈, LUBRIZOL사(미국)의 PINNACLE 시리즈, MICRO POWDERS사(Micro Powders, Inc., 미국)의 MPP 시리즈 및 CRODA사의 제품을 사용할 수 있다. 본 발명의 액상분산체에서 폴리에틸렌왁스의 함량은 1 내지 30 중량%, 바람직하게는 1 내지 15 중량%이다. 폴리에틸렌왁스가 30 중량%보다 많을 경우 과량의 함량으로 인한 유동성 악화로 분산성이 저하(Flow형 분산기를 사용)되며, 1 중량%보다 적을 경우 분산시간이 너무 길어지게 되어 도료적용시 상대적으로 많은 양의 조성물을 첨가해야 한다.Polyethylene wax used in the present invention is a copolymer of ethylene and polar monomer obtained by decomposing natural gas or naphtha, and is a powdery synthetic wax imparted with a polar group by various chemical modifications such as oxidative decomposition. Various types of polyethylene waxes having various particle sizes and characteristics are used according to the polymerization method and processing process, but in the present invention, fine polyethylene waxes are selected such that the maximum particle size is preferably dispersed to 10 μm or less. As polyethylene wax meeting the above conditions, for example, the PRINTWAX series of DEUREX (DEUREX Wachs-Chemie GmbH, Germany), the PINNACLE series of LUBRIZOL (USA), and the MPP of MICRO POWDERS (Micro Powders, Inc., USA) Series and CRODA products are available. The content of polyethylene wax in the liquid dispersion of the present invention is 1 to 30% by weight, preferably 1 to 15% by weight. If the polyethylene wax is more than 30% by weight, the dispersibility is lowered due to the deterioration of the fluidity due to the excessive content (using a flow type disperser) .When the amount of the polyethylene wax is less than 1% by weight, the dispersion time becomes too long. Must be added.
본 발명에서 사용되는 유기관능기를 가지는 공중합체 용액은 분산체 친화그룹을 가지는 고분자량의 공중합체 용액으로, 조성물의 분산능을 향상시키는 역할을 한다. 여기서 유기관능기는 히드록시기, 카르복실기 또는 아민기이다. 구체적으로 상기 공중합체 용액은 아크릴 공중합체, 아크릴 변성우레탄, 폴리에스테르 변성우레탄 또는 이들의 혼합물로서, 예를 들면 BYK사(BYK-Chemie GmbH & Co., 독일)의 DISPERBYK-108, DISPERBYK-116, DISPERBYK-140, DISPERBYK-160, DISPERBYK-161, DISPERBYK-168, DISPERBYK-170, DISPERBYK-171, DISPERBYK-174, ANTITERRA-U, ANTITERRA-U80, ANTITERRA-204, AVECIA사(AVECIA Pigments & Additives, 영국)의 SOLSPERSE-31845, SOLSPERSE-32500, SOLSPERSE-34750, SOLSPERSE-24000SC, SOLSPERSE-24000GR, EFKA사(네덜란드)의 EFKA-4046, EFKA-4047, EFKA-4050, EFKA-4055, EFKA-4080, EFKA-4400을 사용할 수 있다. 본 발명의 액상분산체에서 유기관능기를 가지는 공중합체 용액의 함유량은 1 내지 20 중량%, 바람직하게는 1 내지 10 중량%이다. 도료에 적용하는 경우 일반적으로 고형분을 감안하여 분산체를 첨가하므로, 공중합체 용액의 함량이 많을 경우 상대적으로 폴리에틸렌왁스의 농도가 낮아지므로 목적하는 표면물성을 얻기 힘들며, 적정 함량보다 적을 경우 분산능이 저하되어 효과가 떨어진다.The copolymer solution having an organic functional group used in the present invention is a high molecular weight copolymer solution having a dispersion affinity group, and serves to improve the dispersibility of the composition. The organic functional group is a hydroxyl group, a carboxyl group or an amine group here. Specifically, the copolymer solution may be an acrylic copolymer, an acrylic modified urethane, a polyester modified urethane, or a mixture thereof. For example, DISPERBYK-108, DISPERBYK-116, manufactured by BYK (BYK-Chemie GmbH & Co., Germany), DISPERBYK-140, DISPERBYK-160, DISPERBYK-161, DISPERBYK-168, DISPERBYK-170, DISPERBYK-171, DISPERBYK-174, ANTITERRA-U, ANTITERRA-U80, ANTITERRA-204, AVECIA (AVECIA Pigments & Additives, UK) SOLSPERSE-31845, SOLSPERSE-32500, SOLSPERSE-34750, SOLSPERSE-24000SC, SOLSPERSE-24000GR, EFKA-4046, EFKA-4047, EFKA-4050, EFKA-4055, EFKA-4080, EFKA-4400 from EFKA Corporation (Netherlands) Can be used. The content of the copolymer solution having an organic functional group in the liquid dispersion of the present invention is 1 to 20% by weight, preferably 1 to 10% by weight. When applied to paints, dispersions are generally added in consideration of solid content. Therefore, when the content of the copolymer solution is large, the concentration of polyethylene wax is relatively low, so that it is difficult to obtain the desired surface properties. The effect is reduced.
본 발명에서 사용되는 용제는 분산체 친화그룹을 가진 고분자량의 공중합체 용액과의 상용성, 필요에 따라 건조속도를 제어할 수 있어야 하며, 예를 들면 부틸셀로솔브, 톨루엔, 자일렌과 같은 휘발성 유기용제를 단독 또는 혼합으로 사용할 수 있다. 본 발명의 실시예에 따르면, 고유점도가 높은 부틸셀로솔브를 사용할 경우 우수한 물성의 액상분산체를 제조할 수 있다. 본 발명의 액상분산체의 조성에 있어서 용제가 대부분을 차지하며, 폴리에틸렌왁스 및 유기관능기를 가지는 공중합체 용액의 함유량을 제외한 나머지가 용제이다.The solvent used in the present invention should be compatible with the high molecular weight copolymer solution having a dispersion affinity group, and can control the drying rate if necessary, such as butyl cellosolve, toluene, xylene Volatile organic solvents may be used alone or in combination. According to an embodiment of the present invention, when using a butyl cellosolve having a high intrinsic viscosity can be prepared a liquid dispersion of excellent physical properties. The solvent occupies most of the composition of the liquid dispersion of the present invention, and the rest is the solvent except for the content of the copolymer solution having polyethylene wax and an organic functional group.
본 발명의 다른 특징은 유성도료에 소광효과를 부여하기 위한 것으로, 이러한 목적을 달성하기 위하여 소광제, 바람직하게는 실리카를 더 포함하는 유성도료용 액상분산체 조성물이 제공된다. 이러한 실리카로서, 예를 들면 GRACE Davison사(W.R. Grace & Co., 미국)의 SYLOID 244, 161, ED30, ED50, ED52, C906, C907, 미국의 DEGUSSA사(미국)의 ACEMATT OK412, OK500, TS100, AEROSIL TT600, TT200, LUBRIZOL사(미국)의 LANCO MATT 2000을 사용할 수 있다. 본 발명의 액상분산체에 첨가되는 실리카의 양은 1 내지 10 중량%이며, 상기 실리카가 10 중량%보다많을 경우 메탈 마킹(metal marking: 도막표면에 금속과 마찰이 발생할 경우 마찰이 발생한 자리에 금속성분이 흑색으로 묻어나는 현상)이 발생할 수 있으며, 1 중량%보다 적을 경우 소광효과를 기대할 수 없다. 또한 소광제로서 실리카가 아닌 폴리프로필렌왁스와 같은 유기계 소광제를 사용하여도 무방하다.Another feature of the present invention is to impart a matting effect to the oil paint, in order to achieve this object is provided a liquid dispersion composition for oil paint further comprises a matting agent, preferably silica. As such silica, for example, SYLOID 244, 161, ED30, ED50, ED52, C906, C907 from GRACE Davison (WR Grace & Co., USA), ACEMATT OK412, OK500, TS100, from DEGUSSA (USA) AEROSIL TT600, TT200 and LANCO MATT 2000 from LUBRIZOL (USA) can be used. The amount of silica added to the liquid dispersion of the present invention is 1 to 10% by weight, and when the silica is more than 10% by weight, metal marking (metal marking: a metal component where friction occurs when friction occurs with the metal on the surface of the coating film. This black color may occur. If the amount is less than 1% by weight, no matting effect can be expected. In addition, an organic matting agent such as polypropylene wax may be used as the matting agent.
본 발명의 유성도료용 액상분산체 조성물은 유기관능기를 가지는 고분자량의 공중합체 용액 및 분산시간의 단축과 분산효율을 높이기 위해 용제의 일부를 저속 교반하여 혼합액을 제조한 후, 상기 혼합액에 미립자 폴리에틸렌왁스를 첨가하고 교반한 후 이를 분산기에 투입하여 분산액을 제조한 다음, 충진단계로서 상기 분산액에 나머지 용제를 가하고 저속 교반하여 최종적으로 제조한다. 이때 특수용도로 소광효과를 부여하려면 실리카를 상기 분산액에 투입한다.Liquid dispersion composition for oil-based paints of the present invention is a high molecular weight copolymer solution having an organic functional group and a portion of the solvent to agitate at low speed to increase the dispersion efficiency and dispersion efficiency, after preparing a mixed solution, fine particulate polyethylene in the mixed solution After adding the wax and stirring the mixture, it is added to a disperser to prepare a dispersion. Then, the remaining solvent is added to the dispersion as a filling step, and finally prepared by stirring at a low speed. In this case, to give a matting effect for a special purpose, silica is added to the dispersion.
더욱 구체적으로 설명하면 본 발명의 유성도료용 액상분산체 조성물의 제조방법은 (a) 액상분산체 조성물 100 중량%를 기준으로 유기관능기를 가지는 고분자량의 공중합체 용액 1 내지 20 중량%, 바람직하게는 1 내지 10 중량%와 용제 50 내지 97 중량%, 바람직하게는 75 내지 97 중량%를 용기에 투입하고 혼합교반기로 상온에서 1 내지 10분 동안, 500 내지 2,000 rpm으로 교반하는 단계;More specifically, the method for preparing a liquid dispersion composition for an oil paint according to the present invention may include (a) 1 to 20% by weight of a high molecular weight copolymer solution having an organic functional group, based on 100% by weight of the liquid dispersion composition. 1 to 10% by weight and 50 to 97% by weight of the solvent, preferably 75 to 97% by weight in a container and stirred at 500 to 2,000 rpm for 1 to 10 minutes at room temperature with a mixing stirrer;
(b) 상기 (a) 단계의 혼합물을 교반하면서 액상분산체 조성물 100 중량%를 기준으로 파우더상의 미립자 폴리에틸린왁스 1 내지 30 중량%, 바람직하게는 1 내지 15 주량%를 첨가한 후 10 내지 30분 동안 1,000 내지 2,000 rpm으로 교반하는 단계;(b) 1 to 30% by weight, preferably 1 to 15% by weight, of fine particulate polyethylenwax, preferably 1 to 15% by weight, based on 100% by weight of the liquid dispersion composition while stirring the mixture of step (a). Stirring at 1,000 to 2,000 rpm for 30 minutes;
(c) 상기 (b) 단계의 혼합물을 분산매체를 이용한 혼합분산기에 투입하여 1내지 5시간 동안 2,000 내지 4,000 rpm으로 분산시키는 단계; 및(c) dispersing the mixture of step (b) at 2,000 to 4,000 rpm for 1 to 5 hours by adding it to a mixed dispersion machine using a dispersion medium; And
(d) 상기 (c) 단계의 분산액을 혼합분산기로부터 분리하여 용제 5 내지 20 중량%를 첨가한 후 5 내지 30분 동안 1,000 내지 2,000 rpm으로 교반하는 단계를 포함한다.(d) separating the dispersion of step (c) from the mixed disperser and adding 5 to 20% by weight of the solvent, followed by stirring at 1,000 to 2,000 rpm for 5 to 30 minutes.
유성도료에 소광효과를 부여하기 위한 본 발명의 액상분산체 조성물의 제조방법은 상기 (c) 단계 다음에 혼합분산기로부터 분리한 분산액을 교반하면서 액상분산체 조성물 100 중량%를 기준으로 실리카 1 내지 10 중량%를 첨가한 후 500 내지 3,000 rpm으로 교반하는 단계; 및 상기 혼합물을 분산매체를 이용한 혼합분산기에 투입하여 1분 내지 1시간 동안 2,000 내지 4,000 rpm으로 분산시키는 단계를 더 포함한다.Method for producing a liquid dispersion composition of the present invention for imparting a matting effect to the oil paint is based on (1) silica step 1 to 10 while stirring the dispersion separated from the mixed dispersion after step (c) Stirring at 500 to 3,000 rpm after addition of weight percent; And dispersing the mixture at 2,000 to 4,000 rpm for 1 minute to 1 hour by adding the mixture to a mixed disperser using a dispersion medium.
본 발명의 액상분산체 조성물은 유리비드, 지르코늄비드와 같은 매체를 이용한 혼합분산방법 또는 고압에 의한 분산방법으로 기재에 분산시킬 수 있다. 특히 분산물에 초고압(1,000∼3,500 kgf/㎠)의 에너지를 가하여 분산물을 두 줄기의 흐름으로 나누어 재결합하는 부분에서 대향 충돌시키거나 미세한 틈 사이로 밀어내어 분산시키는 고압에 의한 분산방법을 사용할 경우 종래의 분산시스템에서 문제가 되었던 금속분 및 비드의 마모를 방지할 수 있고 공정시간을 단축할 수 있는 장점이 있다.The liquid dispersion composition of the present invention may be dispersed in the substrate by a mixed dispersion method using a medium such as glass beads or zirconium beads or a dispersion method by high pressure. In particular, when the dispersion is applied by a high pressure method by applying an ultra-high pressure (1,000 to 3,500 kgf / cm 2) to the dispersion and dispersing the dispersion into two streams, it collides with each other in a recombination part or by pushing it through a fine gap to disperse the dispersion. It is possible to prevent wear of metal powder and beads, which have been a problem in the dispersion system, and to shorten the process time.
이하 실시예를 통하여 본 발명을 구체적으로 설명한다. 그러나 하기의 실시예는 오로지 본 발명을 구체적으로 예시하기 위한 것으로, 이들 실시예에 의해 본 발명의 권리범위가 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail through examples. However, the following examples are only to specifically illustrate the present invention, and the scope of the present invention is not limited to these examples.
<실시예 1><Example 1>
DISPERBYK-160 3 g과 톨루엔 70 g을 SUS(Steel special Use Stainless)용기에 투입한 후 혼합교반기(제조사: 화성기공사)를 이용하여 1,000 rpm으로 상온에서 5분간 교반하였다. 상기 혼합물을 교반하면서 최대입자크기가 30 내지 35 ㎛인 파우더상의 폴리에틸렌왁스 8 g을 첨가한 후 20분간 3,000 rpm으로 교반하였다. 교반이 완료된 후 상기 내용물을 분산매체(종류: 이트리아 안정화 비드, 규격: 0.8∼1.0 mm)를 이용한 혼합분산기(종류: Eiger Mill, 제조사: 화성기공사)에 투입하여 2,000 rpm에서 3시간 분산시켰다. 분산이 완료된 후 분산물을 분산기로부터 분리하여 톨루엔 20 g을 첨가하고 10분간 3,000 rpm으로 교반한 다음 여과함으로써 결과물인 액상분산체 조성물을 제조하였다.3 g of DISPERBYK-160 and 70 g of toluene were added to a stainless steel special use stainless (SUS) container, followed by stirring at room temperature at 1,000 rpm for 5 minutes using a mixing stirrer (manufacturer: Hwasung Chemical Co., Ltd.). While stirring the mixture, 8 g of powdery polyethylene wax having a maximum particle size of 30 to 35 μm was added thereto, followed by stirring at 3,000 rpm for 20 minutes. After the stirring was completed, the contents were added to a mixed disperser (type: Eiger Mill, manufacturer: Hwasung) using a dispersion medium (type: yttria stabilized beads, size: 0.8 to 1.0 mm), and dispersed at 2,000 rpm for 3 hours. After the dispersion was completed, the dispersion was separated from the disperser, 20 g of toluene was added thereto, stirred at 3,000 rpm for 10 minutes, and filtered to prepare a resultant liquid dispersion composition.
제조된 조성물의 평균입자크기(Average Particle Size) 및 점도는 다음과 같았다. 본 실시예 및 하기 실시예에서 평균입자크기는 입자분석기(PSA: Particle Size Analyzer, Brookhaven Instruments Corp., 90 Plus)로 측정하였으며, 최종점도는 25℃에서 브룩필드 점도계(Brookfield Viscometer, 모델명: RVDV-1, 제조사: Brookfield사)로 측정하였다.Average particle size and viscosity of the prepared composition were as follows. In this example and the following examples, the average particle size was measured by a particle analyzer (PSA: Particle Size Analyzer, Brookhaven Instruments Corp., 90 Plus), and the final viscosity was Brookfield Viscometer (Model name: RVDV-) at 25 ° C. 1, manufacturer: Brookfield).
평균입자크기(3시간 분산 후): 3.0 ㎛Average particle size (after 3 hours dispersion): 3.0 μm
최종점도(25℃): 350 cpsFinal viscosity (25 ℃): 350 cps
<실시예 2><Example 2>
실시예 1과 동일한 방법으로 실시하되 최대입자크기가 20 내지 25 ㎛인 파우더상의 폴리에틸렌왁스를 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는다음과 같았다.A powdery polyethylene wax having a maximum particle size of 20 to 25 μm was used in the same manner as in Example 1, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 2.5 ㎛Average particle size (after 3 hours dispersion): 2.5 μm
최종점도(25℃): 300 cpsFinal viscosity (25 ℃): 300 cps
<실시예 3><Example 3>
실시예 1과 동일한 방법으로 실시하되 최대입자크기가 10 내지 15 ㎛인 파우더상의 폴리에틸렌왁스를 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.A powdery polyethylene wax having a maximum particle size of 10 to 15 μm was used in the same manner as in Example 1, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 2.5 ㎛Average particle size (after 3 hours dispersion): 2.5 μm
최종점도(25℃): 310 cpsFinal viscosity (25 ℃): 310 cps
<실시예 4><Example 4>
실시예 3에서 제조한 조성물에 실리카를 투입하여 제조한 조성물의 평균입자크기 및 점도는 다음과 같았다.The average particle size and viscosity of the composition prepared by adding silica to the composition prepared in Example 3 were as follows.
평균입자크기(3시간 분산 후): 5 ㎛Average particle size (after 3 hours dispersion): 5 μm
최종점도(25℃): 260 cpsFinal viscosity (25 ℃): 260 cps
<실시예 5>Example 5
실시예 1과 동일한 방법으로 실시하되 용제로서 톨루엔 대신 부틸셀로솔브를 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.Butyl cellosolve was used instead of toluene as a solvent, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 1.0 ㎛Average particle size (after 3 hours dispersion): 1.0 μm
최종점도(25℃): 280 cpsFinal viscosity (25 ℃): 280 cps
<실시예 6><Example 6>
유기관능기를 가지는 고분자량의 블록공중합체가 조성물의 물성에 미치는 영향을 분석하기 위하여 실시예 1과 동일한 방법으로 실시하되 화학식에 아민기(Amine group)만을 포함하는 DISPERBYK-160 대신 화학식에 산기(Acid group)만을 포함하는 DISPERBYK-170을 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.In order to analyze the effect of the high molecular weight block copolymer having an organic functional group on the physical properties of the composition, it was carried out in the same manner as in Example 1, but instead of the DISPERBYK-160 containing only an amine group in the formula, DISPERBYK-170 containing only group) was used, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 3 ㎛Average particle size (after 3 hours dispersion): 3 μm
최종점도(25℃): 200 cpsFinal viscosity (25 ℃): 200 cps
<실시예 7><Example 7>
DISPERBYK-160 2.5 g과 톨루엔 70 g을 SUS용기에 투입한 후 혼합교반기를 이용하여 1,000 rpm으로 상온에서 5분간 저속 교반하였다. 상기 혼합물을 교반하면서 최대입자크기가 30 내지 35 ㎛인 파우더상의 폴리에틸렌왁스 6 g을 첨가한 후 30분간 3,000 rpm으로 교반하였다. 교반이 완료된 후 분산매체를 이용한 혼합분산기에 투입하여 2,000 rpm에서 3시간 분산시켰다. 분산이 완료된 후 분산물을 분산기로부터 분리하여 톨루엔 20 g을 첨가하여 3,000 rpm으로 약 10분간 교반한 다음 여과함으로써 결과물인 액상분산체 조성물을 제조하였다. 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.2.5 g of DISPERBYK-160 and 70 g of toluene were added to a SUS container, and then stirred at low speed for 5 minutes at room temperature at 1,000 rpm using a mixing stirrer. While stirring the mixture, 6 g of powdery polyethylene wax having a maximum particle size of 30 to 35 μm was added thereto, followed by stirring at 3,000 rpm for 30 minutes. After the stirring was completed, the mixture was added to a mixed disperser using a dispersion medium and dispersed at 2,000 rpm for 3 hours. After the dispersion was completed, the dispersion was separated from the disperser, 20 g of toluene was added, stirred for about 10 minutes at 3,000 rpm, and then filtered to prepare a resultant liquid dispersion composition. Average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 3.0 ㎛Average particle size (after 3 hours dispersion): 3.0 μm
최종점도(25℃): 310 cpsFinal viscosity (25 ℃): 310 cps
<실시예 8><Example 8>
실시예 7과 동일한 방법으로 실시하되 최대입자크기가 20 내지 25 ㎛인 파우더상의 폴리에틸렌왁스를 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.A powdery polyethylene wax having a maximum particle size of 20 to 25 μm was used in the same manner as in Example 7, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 2.5 ㎛Average particle size (after 3 hours dispersion): 2.5 μm
최종점도(25℃): 300 cpsFinal viscosity (25 ℃): 300 cps
<실시예 9>Example 9
실시예 7과 동일한 방법으로 실시하되 최대입자크기가 10 내지 15 ㎛인 파우더상의 폴리에틸렌왁스를 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.A powdery polyethylene wax having a maximum particle size of 10 to 15 μm was used in the same manner as in Example 7, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 2.5 ㎛Average particle size (after 3 hours dispersion): 2.5 μm
최종점도(25℃): 320 cpsFinal viscosity (25 ℃): 320 cps
<실시예 10><Example 10>
실시예 7에서 제조한 조성물에 실리카를 투입하여 제조한 조성물의 평균입자크기 및 점도는 다음과 같았다.The average particle size and viscosity of the composition prepared by adding silica to the composition prepared in Example 7 were as follows.
평균입자크기(3시간 분산 후): 6 ㎛Average particle size (after 3 hours dispersion): 6 μm
최종점도(25℃): 280 cpsFinal viscosity (25 ℃): 280 cps
<실시예 11><Example 11>
실시예 7과 동일한 방법으로 실시하되 화학식에 아민기를 포함하는 DISPERBYK-160 대신 화학식에 산기를 포함하는 DISPERBYK-170을 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.In the same manner as in Example 7, except for using DISPERBYK-170 containing an acid group in the formula instead of DISPERBYK-160 containing an amine group, the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 3 ㎛Average particle size (after 3 hours dispersion): 3 μm
최종점도(25℃): 220 cpsFinal viscosity (25 ℃): 220 cps
<실시예 12><Example 12>
실시예 7과 동일한 방법으로 실시하되 용제로 톨루엔 대신 부틸셀로솔브를 사용하였으며, 제조된 조성물의 평균입자크기 및 점도는 다음과 같았다.Butyl cellosolve was used instead of toluene as a solvent, and the average particle size and viscosity of the prepared composition were as follows.
평균입자크기(3시간 분산 후): 900 nmAverage particle size (after 3 hours dispersion): 900 nm
최종점도(25℃): 300 cpsFinal viscosity (25 ℃): 300 cps
<실시예 13: 물성비교시험>Example 13: Physical Property Comparison Test
상기 실시예에서 제조된 각각의 액상분산체 조성물은 다음과 같이 규정된 시험방법에 의하여 물성시험을 하였으며, 그 결과는 표 1과 같다.Each liquid dispersion composition prepared in the above Example was tested for physical properties by the test method specified as follows, and the results are shown in Table 1.
1. 입자분포 분석시험1. Particle Distribution Analysis
입자분석기에 일정량의 희석된 시료를 투입하여 평균입자크기 및 분포를 측정하였으며, 평균입자크기에 따라 다음과 같이 구분하였다.The particle size and distribution were measured by adding a predetermined amount of diluted sample to the particle analyzer, and classified according to the average particle size as follows.
◎: 우수, 평균입자크기 1 ㎛ 이하◎: excellent, average particle size 1 탆 or less
○: 양호, 평균입자크기 2∼3 ㎛(Circle): good, average particle size 2-3 micrometers
△: 보통, 평균입자크기 3 ㎛ 이상(Triangle | delta): Usually, average particle size 3 micrometers or more
2. 분산성 비교시험2. Dispersibility Comparison Test
분산과정에서 1시간 경과 후 소량의 시료를 취하여 입자분석기로 입자크기를 측정하였으며, 입자크기에 따라 다음과 같이 구분하였다.After 1 hour in the dispersion process, a small amount of samples were taken, and the particle size was measured by a particle analyzer, and classified according to the particle size as follows.
◎: 우수, 1시간 분산 후 3 ㎛ 이하(Double-circle): Excellent, 3 micrometers or less after 1 hour dispersion
○: 양호, 1시간 분산 후 5 ㎛ 이하○: good, 5 μm or less after dispersion for 1 hour
△: 보통, 1시간 분산 후 10 ㎛ 이하(Triangle | delta): Usually, 10 micrometers or less after dispersion | distribution for 1 hour
×: 불량, 1시간 분산 후 10 ㎛ 이상X: 10 micrometers or more after failure and dispersion | distribution for 1 hour
3. 저장안정성 비교시험3. Storage stability comparison test
시료를 지름 20 ㎝, 높이 2.5 ㎝의 유리시험관에 일정량을 넣고 5℃ 이하의 저온에서 15일 동안 방치 후 층분리 정도를 측정하였으며, 그 정도에 따라 다음과 같이 구분하였다.The sample was placed in a glass test tube with a diameter of 20 cm and a height of 2.5 cm, and left for 15 days at a low temperature of 5 ° C. and then the degree of layer separation was measured.
◎: 우수, 층분리 0∼0.1 mm◎: excellent, layer separation 0-0.1 mm
○: 양호, 층분리 0.1∼0.2 mm○: good, layer separation 0.1 to 0.2 mm
△: 보통, 층분리 0.2∼0.3 mm(Triangle | delta): Usually, layer separation 0.2-0.3 mm
표 1에 따르면, 사용한 폴리에틸렌왁스의 최대입자크기가 작을수록 분산성이 우수하였으며, 특히 부틸셀로솔브와 같은 고유점도가 높은 용제를 사용한 경우 입자분포, 분산성 및 저장안정성이 모두 우수하였다. 조성물의 평균입자크기에 따라 일정 분산시간이 지나면 분산성에는 큰 차이가 없었다. 유기관능기를 가지는 고분자량의 블록공중합체의 종류가 분산성 및 저장안정성에 크게 영향을 미치지 않았으나, 조성물의 최종점도는 아민기만을 가지는 공중합체를 사용하였을 때 산기만을 가지는 공중합체를 사용한 경우보다 높게 나타나는 경향이 있었다.According to Table 1, the smaller the maximum particle size of the polyethylene wax used, the better the dispersibility, and especially in the case of using a solvent having a high intrinsic viscosity such as butyl cellosolve, the particle distribution, dispersibility, and storage stability were excellent. According to the average particle size of the composition after a certain dispersion time there was no significant difference in dispersibility. Although the type of high molecular weight block copolymers having organic functional groups did not significantly affect the dispersibility and storage stability, the final viscosity of the composition was higher than that of the copolymer having only an acid group when the copolymer having only an amine group was used. There was a tendency to appear.
<실시예 14><Example 14>
본 실시예에서는 상기 실시예에서 제조한 액상분산체 조성물을 이용하여 유성도료를 제조하였다.In this embodiment, the oil paint was prepared using the liquid dispersion composition prepared in the above embodiment.
먼저 아크릴 폴리올과 이소시아네이트 경화제를 혼합하는 2액형 아크릴우레탄 타입의 투명도료를 제조한 후, 상기 실시예에서 제조한 본 발명의 액상분산체 조성물 및 종래분산체를 고형분비에 따라 왁스 중량이 각각 3%가 되도록 첨가하여 유성투명도료를 제조하였다.First, a two-component acrylic urethane-type transparent paint is prepared by mixing an acrylic polyol and an isocyanate curing agent, and the wax weight of the liquid dispersion composition and the conventional dispersion of the present invention prepared in the above-described examples are 3% by weight, respectively. It was added so as to prepare an oily transparent paint.
제조된 유성투명도료의 일정량을 각각 채취하고 Applicator를 이용하여 동시에 도포하여 같은 도막두께를 가지는 도막의 시편을 제조한 후, 제조된 시편으로 도막의 슬립성, 내긁힘성, 내마모성과 같은 표면물성을 측정하였다.After extracting a certain amount of the oil-based transparent paint prepared by each application and using an applicator at the same time to prepare a coating film having the same coating thickness, the prepared specimen with the surface properties such as slip properties, scratch resistance, wear resistance Measured.
시험방법은 당업계에서 보편적으로 사용되는 동전 테스트로서 실시하였으며, 슬립성의 경우 일정한 기울기에서 도막 위에 동전을 올려놓고 동전이 아래로 미끄러져 내려가는 차이로 측정하였고, 내마모성 및 내긁힘성은 동전으로 도막에 같은 힘으로 긁었을 때 흠집이 나는 정도로 측정하였으며, 그 결과는 표 2와 같다.The test method was carried out as a coin test commonly used in the art, and in the case of slip property, the coin was put on the coating film at a constant slope and the coin slipped down, and the abrasion resistance and the scratch resistance were the same on the coating film with the coin. When scratched with force, the degree of scratches was measured, and the results are shown in Table 2.
표 2에서 보는 바와 같이, 본 발명의 미립자 폴리에틸렌왁스를 포함하는 안료분산체 조성물을 이용하여 제조한 유성도료를 도포한 도막의 경우 종래의 분산체를 사용하여 도포한 도막에 비하여 내긁힘성, 내마모성, 특히 슬립성이 우수하였다.As shown in Table 2, the coating film coated with the oil paint prepared using the pigment dispersion composition containing the particulate polyethylene wax of the present invention is scratch-resistant and abrasion resistant compared to the coating film coated with a conventional dispersion. In particular, the slip property was excellent.
본 발명의 액상분산체 조성물은 폴리에틸렌왁스의 입자크기를 미립화하고 입자크기를 미세하게 분산시킴으로써 도막형성 후 왁스의 부상능력을 최대화하고 표면에 고른 박막으로 존재하도록 하여 공업용 유성도료가 필수적으로 요구하는 성질인 도막의 슬립성, 내마모성 및 내긁힘성을 충분히 부여할 뿐 아니라 분산안정성이 우수하다. 또한 필요에 따라 실리카를 첨가함으로써 유성도료의 소광효과를 부여할 수 있다.Liquid dispersion composition of the present invention is a particle size of the polyethylene wax and finely dispersed particle size to maximize the floating capacity of the wax after forming the coating film and to be present as an even thin film on the surface properties essential for industrial oil paint It not only gives sufficient slip resistance, abrasion resistance and scratch resistance of the phosphor coating film but also has excellent dispersion stability. Moreover, the matting effect of an oil-based paint can be provided by adding silica as needed.
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KR100527795B1 (en) * | 2002-11-30 | 2005-11-09 | 한국신발피혁연구소 | UV coating materials having Non-slip characteristics |
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JP2000265111A (en) * | 1999-03-16 | 2000-09-26 | Nippon Parkerizing Co Ltd | Aqueous surface treating agent for metal material and surface treated metal plate |
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