KR100866588B1 - A flame retardant composite - Google Patents
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- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
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Abstract
Description
본 발명은 무독, 무연성 ABS 난연성 수지 조성물에 관한 것으로, 보다 상세하게는 발암물질이 전혀 발생하지 않으며, 프라스틱이 연소시 유독가스가 발생 되지 않는 우수한 난연성 수지 조성물에 관한 것으로서, 아크릴로니트릴-부타디엔-스치렌수지와 난연성을 부여하는 고분자형 염소화 폴리에티렌, 무기계 수산화알루미늄 및 징크 보레이트를 포함하는 무독, 무연성의 우수한 난연성 수지 조성물에 관한 것이다.The present invention relates to a non-toxic, non-flammable ABS flame retardant resin composition, and more particularly to a flame retardant resin composition which does not generate any carcinogens, and does not generate toxic gas when the plastic is burned, acrylonitrile-butadiene It relates to a non-toxic, non-flammable, excellent flame retardant resin composition comprising a polymeric chlorinated polystyrene, inorganic aluminum hydroxide and zinc borate which impart flame retardancy and flame retardancy.
일반적으로 아크릴로니트릴-부타디엔-스티렌( 이하 "ABS" 이라 한다)난연성 수지는 TV, 컴퓨터, DVD, 복사기, 팩시밀리 및 최근 대형 프로젝션 TV 등의 전체가전 제품 분야는 물론, 전기 콘센트, 밧테리, 충전기, 건축분야 소재까지 널리 사용 되고 있으며, 이들 ABS 난연수지는 ABS 수지에 종래의 유기 브롬화 난연제인 테트라브로모비스페놀, 데카브로모디페닐옥사이드, 옥타브로모디페닐옥사이드, 펜타브로모디페닐옥사이드, 폴리디브로모디페닐옥사이드 또는 열경화성수지인 브롬화 에폭시수지 등의 저분자량의 유기 브롬계 난연제를 첨가하는 것이 제안 되어 왔다. 이들 난연제는 미국 안전규격인 UL 연소규격에 합격하기 위해서는 난연상승화제인 Sb203(삼산화안티몬)을 첨가하는 방식으로 현재 까지 사용 되어 왔다.Generally, acrylonitrile-butadiene-styrene (hereinafter referred to as "ABS") flame retardant resins are used in the field of electric appliances, batteries, chargers, It is widely used in construction materials, and these ABS flame retardant resins are conventional organic brominated flame retardants such as tetrabromobisphenol, decabromodiphenyl oxide, octabromodiphenyl oxide, pentabromodiphenyl oxide, and polydibromodie. It has been proposed to add low molecular weight organic bromine flame retardants such as phenyl oxide or brominated epoxy resins which are thermosetting resins. These flame retardants have been used until now to add the flame retardant enhancer Sb203 (antimony trioxide) in order to pass the US safety standards UL combustion standards.
그러나 사용되고 있는 난연제는 최종제품으로 제조된 성형품 외관에서 다이옥신과 다이퓨란이라는 발암물질이 생성되게 하는 문제점이 전 세계적으로 제기되어 세계보건기구에서는 반치사량(LD50)을 규정하였으며 한국에서도 SGS 실험을 통한 난연제 사용 PBBs/PBDEs를 통하여 사용을 금지하고 있다.However, the flame retardant used has a problem that globally produced carcinogens such as dioxin and difuran are produced from the appearance of molded products made of the final product, and the World Health Organization regulates anti-reflective dose (LD50). Use Prohibited use through PBBs / PBDEs.
따라서 현재는 테트라브로모 비스페놀과 브롬화 에폭시수지만을 사용하고 있으며 이들 난연제는 연소시 브롬이라는 성분 때문에 유독가스 발생, 즉 연소시 발암물질생성이 불가피하여 한시적 사용에 제한되고 있는 실정이다.Therefore, only tetrabromo bisphenol and brominated epoxy resin are used at present, and these flame retardants are limited to temporary use because toxic gases are generated due to the composition of bromine during combustion, that is, inevitable generation of carcinogens during combustion.
또한 기존 ABS 수지에 브롬 난연제와 반드시 같이 첨가되는 난연 상승화제인 Sb203(삼산화 안티몬)은 안티몬(Sb)이 인체에 해로운 독극물로 분류되어 ABS 난연성수지 제조시, 제조자의 인체에 치명적 발암 물질과 연소시 발암 물질 생성을 다량 발생하는 물질로 현재까지 대체 품목이 없어서 제한 사용하고 있는 실정이다.In addition, Sb203 (antimony trioxide), a flame retardant synergist that is necessarily added to bromine flame retardants, is classified as a poison that is harmful to humans. It is a substance that generates a large amount of carcinogens and is currently limited because there is no replacement item.
따라서 발암물질의 발생이라는 문제점을 해결하기 위하여, 상기 저 분자량 브롬계난연제 대신에 염소계 난연제와 무기계_난연제의 개발이 활발히 이루어졌으며, 그 예로 인계, 수산화알루미늄, 수산화마그네슘 등이 제안 되어 왔다.Therefore, in order to solve the problem of the occurrence of carcinogens, development of chlorine flame retardants and inorganic flame retardants instead of the low molecular weight bromine flame retardant has been actively made, for example, phosphorus, aluminum hydroxide, magnesium hydroxide and the like have been proposed.
그러나 염소계, 인계, 수산화마그네슘, 수산화알루미늄 난연제는 난연 효과가 브롬 난연제와는 상대가 안 될 만큼 난연성 효과가 미흡하여, ABS 수지에는 현재까지 적용을 못하고 있다.However, chlorine-based, phosphorus-based, magnesium hydroxide and aluminum hydroxide flame retardant has a low flame retardant effect so that the flame retardant effect is not comparable to bromine flame retardant, so it has not been applied to ABS resin until now.
또한, 수산호마그네슈므 수산화알루미늄은 난연제 자체에 수화물을 함유하고 있어서 ABS 수지에 첨가되면 ABS 수지의 흡습성 때문에 불균일성 난연 효과와 프라 스틱 성형물 외관에 치명적 문제점을 야기 시켜서 난연제 사용은 불가능 한 것으로 판명되었고, 이들 난연제는 폴리에틸렌, 폴리프로필렌 수지의 난연성을 부여하는데만 한정 사용되고 있다.In addition, aluminum hydroxide hydroxide has a hydrate in the flame retardant itself, and when added to the ABS resin, the hygroscopicity of the ABS resin caused a non-uniform flame retardant effect and a fatal problem in the appearance of the plastic molding, and thus it was proved impossible to use the flame retardant. Flame retardants are only used to impart flame retardancy of polyethylene and polypropylene resins.
상기 염소계 난연제로는 염소화 폴리에틸렌을 들 수 있으나, 미국 특허 제 4067930호, 5,376,718 및 5,395,875 에는 ABS 수지에 대하여 염소화 폴리에틸렌을 5중량부 또는 10중량부 이상 사용하는 경우 최종 수지 조성물의 내열성, 내광성 및 내후성의 현저한 저하가 초래됨을 기술 하고 있다.The chlorine-based flame retardant may include chlorinated polyethylene, but US Pat. Nos. 4067930, 5,376,718 and 5,395,875 show that when 5 parts by weight or 10 parts by weight or more of chlorinated polyethylene is used with respect to the ABS resin, the heat resistance, light resistance, and weather resistance of the final resin composition. It is described that a significant degradation is caused.
즉, 지금까지 염소화폴리에틸렌 수지는 ABS 수지에 난연성을 부여하기보다는 ABS수지에 브롬 난연제 첨가시 발생되는 프라스틱 강도 저하를 보완하기 위한 충격 보강제로 일부 사용 되어 왔다.In other words, chlorinated polyethylene resins have been used as impact modifiers to compensate for the decrease in plastic strength caused by adding bromine flame retardants to ABS resins, rather than imparting flame retardancy to ABS resins.
따라서 본 발명의 목적은 상기한 바와 같은 종래기술의 문제점을 해결하기 위한 것으로서, 기존의 저분자량 유기화합물 난연제들과 무기계 삼산화안티몬이 인체에 유해한 발암 물질의 생성과 프라스틱이 화재시 연소하는 과정에서 발생하는 발암 물질을 사용하지 않고 인체에 무독한 고분자형 염소계 화합물과 프라스틱이 연소시 발생하는 발암물질 및 연기 발생량을 최소화 하는 무기계 수산화알루미늄 또는 수산화마그네슘을 난연제로 사용하고, 특히 삼산화안티몬을 무기계 징크 보레이트로 대체함으로서, 새로운 조성물이 ABS난연성 수지를 제공함에 있다.Therefore, an object of the present invention is to solve the problems of the prior art as described above, the existing low-molecular-weight organic compound flame retardants and inorganic antimony trioxide occurs in the process of the generation of carcinogenic substances harmful to the human body and the plastic burning in the event of fire. It does not use carcinogenic substances, and inorganic aluminum hydroxide or magnesium hydroxide, which minimizes the amount of carcinogens and smoke generated when burning plastics, which is harmless to humans and plastics, is used as a flame retardant.In particular, antimony trioxide is used as an inorganic zinc borate. As a replacement, a new composition is to provide an ABS flame retardant resin.
본 발명은 또한, 발명에 적용하고 있는 수산화마그네슘, 알루미늄 및 징크보레이트 난연제 자체가 함유하고 있는 수화물(H2O)을 염소화 폴리에틸렌수지에 1차 적으로 혼합, 가공함으로서 수분을 제거한 후, 2차로 수분을 제거한 난연제를 ABS수지와 재혼합하여 압출 가공하는 방식의 무독, 무연성 ABS 난연성 수지 조성물의 제조방법을 제공함에 또 다른 목적이 있다.The present invention also removes moisture by first mixing and processing the hydrate (H2O) contained in the magnesium hydroxide, aluminum and zinc borate flame retardant itself applied to the chlorinated polyethylene resin, and then removing the water secondly. Another object of the present invention is to provide a method for preparing a non-toxic, non-flammable ABS flame retardant resin composition in which a flame retardant is mixed with an ABS resin and extruded.
따라서, 본 발명은 발명에 사용된 난연제들이 그 자체가 가지고 있는 문제점을 1차적 가공 방법을 통하여 해결하고 이를 2차적으로 ABS 수지 100중량부에 난연 첨가제를 혼합하는 방식으로 2차 조성물을 제공하게 된다.Therefore, the present invention solves the problems of the flame retardants used in the invention through a primary processing method and secondly to provide a secondary composition by mixing a flame retardant additive in 100 parts by weight of ABS resin. .
상기와 같은 목적을 달성하기 위하여 본 발명은,The present invention to achieve the above object,
ABS 수지 100중량부에 대하여 난연 첨가제 50-70중량부가 첨가된 무독, 무연성 ABS 난연성 수지 조성물을 제공한다. 여기서 난연첨가제가 50중량부 이하가 되면 플라스틱 난연성이 저하되어 UL94연소 규격을 만족 할 수 없게 되고 70중량부이상이 첨가되면 플라스틱 난연성이 오버되어 의미가 없게 되므로 위와 같이 정한다.It provides a non-toxic, flame-retardant ABS flame retardant resin composition added 50-70 parts by weight of the flame retardant additive to 100 parts by weight of ABS resin. If the flame retardant additive is 50 parts by weight or less, the flame retardancy of the plastic is lowered to meet the UL94 combustion standard, and if more than 70 parts by weight of plastic flame retardancy is added because it is meaningless as above.
상기에서 난연 첨가제는 난연제, 난연상승화제, 열안정제, 윤활제 또는 분산제를 포함하고, 상기 난연제는 염소화폴리에틸렌수지와 ; 수산화알루미늄 또는 수산화마그네슘 중에서 선택되는 1종 이상을 사용함이 바람직하고, 그 함량은 ABS 수지 100중량부에 대하여 0.1∼70중량부로 함이 바람직하다. 보다 바람직하게는 상기염소화폴리에틸렌수지는 미국 듀폰다우엘라스토머(Dupont Dow Elastomer)사의 상품 명 Tyrin3611을, 수산화알루미늄은 일본국 스미토모케미칼(Sumitomer Chemical)사의 상품명 Alumina를, 수산화마그네슘은 일본국 욱소자 제품으로 브롬을 83% 함유 하는 것을 사용할 수 있다. 상기에서의 난연제는 염소화 폴리에틸렌수지 100중량부 에 대하여 50∼70중량부의 수산화알루미늄이나 수산화 마그네슘을 함유함이 바람직한데, 이는 UL-94-V-O 등급을 만족시키기 위함이다.The flame retardant additives include flame retardants, flame retardants, heat stabilizers, lubricants or dispersants, and the flame retardants include chlorinated polyethylene resins; It is preferable to use at least one selected from aluminum hydroxide or magnesium hydroxide, and the content thereof is preferably 0.1 to 70 parts by weight based on 100 parts by weight of the ABS resin. More preferably, the chlorinated polyethylene resin is a commercial name Tyrin3611 manufactured by Dupont Dow Elastomer, aluminum hydroxide is alumina branded by Sumitomer Chemical of Japan, and magnesium hydroxide is bromine as a Japanese diuretic product. It can be used containing 83%. The flame retardant in the above is preferably containing 50 to 70 parts by weight of aluminum hydroxide or magnesium hydroxide relative to 100 parts by weight of chlorinated polyethylene resin, to satisfy the UL-94-V-O grade.
또한, 난연상승화제로는 징크보레이트(ZnO.3B205.5H2O)를 사용할 수 있는데, 미국 보렉스(Borex)사의 상품명 Firebreak ZB를 사용함이 바람직할 수도 있고, 그 함유량은 ABS 수지 100중량부에 대하여 0.1∼30중량부로 함이 바람직하다고, 가장바람직한 함량은 20중량부이다.In addition, as a flame retardant enhancer, zinc borate (ZnO.3B205.5H 2 O) may be used, but it may be preferable to use a trade name Firebreak ZB manufactured by Borex, USA, and the content thereof may be 100 parts by weight of ABS resin. 0.1 to 30 parts by weight with respect to the preferred, the most preferred content is 20 parts by weight.
또한, 플라스틱이 열에 의해 분해 되는 것을 방지하기 위한 열안정제로는 에폭시수지를 사용하는데 그 함량은 ABS 수지 100중량부에 대하여 0.1∼10중량부로하고, 국내의 국도화학(주)의 상품명 YD-012를 사용할 수 있다. 바람직한 함량은 5중량부이다.In addition, epoxy resin is used as a heat stabilizer to prevent plastic from being decomposed by heat, and its content is 0.1 to 10 parts by weight based on 100 parts by weight of ABS resin, and is trade name YD-012 of Kukdo Chemical Co., Ltd. Can be used. The preferred content is 5 parts by weight.
또한, 플라스틱 가공의 이형성과 대기층 산화 방지 및 기타 혼합이 잘되게 하는 분산성을 갖게 해주는 활제로 사용되는 윤활제는 에틸렌 비스 스테아릭 아마이드를 0.1∼5중량부를 사용할 수 있는데, 국내 선구화학(주)의 상품평 EBS Wax를 사용할 수도 있으며, 분산제로는 바륨 스테아린산을 0.1∼5중량부 사용함이 바람직하고 국내 송원산업(주)의 상품명 Ba-st를 사용할 수도 있으며, 상기한 난연첨가제는 예시한 것으로서 동일한 성분 및 기능을 가진 제품을 사용할 수도 있음은 물론이다.In addition, lubricants used as lubricants for releasing plasticity, preventing atmospheric layer oxidation, and other dispersibility to mix well can use 0.1 to 5 parts by weight of ethylene bis stearic amide. EBS Wax may also be used, and as a dispersant, it is preferable to use 0.1-5 parts by weight of barium stearic acid, and the trade name Ba-st of Korea Songwon Industrial Co., Ltd. may be used. Of course, you can also use the product with.
본 발명에서 사용하는 ABS 수지로는 아크릴로니트릴 20%, 부타디엔 20% 및 스티렌 60%를 함유하는 국내 금호석유화학 제품을 사용하였으나 그 외 동일한 성분 및 제품도 사용할 수 있다.As the ABS resin used in the present invention, a domestic Kumho Petrochemical product containing 20% of acrylonitrile, 20% of butadiene and 60% of styrene was used, but other same components and products may be used.
이하에서는 바람직한 실시 예를 통하여 본 발명의 제조방법을 상세히 설명한다.Hereinafter will be described in detail the manufacturing method of the present invention through a preferred embodiment.
하기 표 1은 본 발명의 난연 첨가제의 실시 조성비를 중량부로 나타낸 것이다.Table 1 shows the actual composition ratio of the flame retardant additive of the present invention in parts by weight.
<표 1> 단위 : 중량부Table 1 Unit: parts by weight
상기와 같은 조성의 중량부를 갖는 실시 예1 ∼ 실시 예6에 따른 물질을 각각 믹서기에 넣고 900∼1100rpm, 바람직하게는 1000rpm의 속도로 8∼15분, 바람직하게는 10분간 150∼200℃, 바람직하게는 플라스틱 자체가 열분해 되기 전인 170℃의 온도로 압출 혼합하여 난연 첨가제를 만든다.The materials according to Examples 1 to 6 each having a weight part of the composition as described above are placed in a blender, respectively, at a speed of 900 to 1100 rpm, preferably 1000 rpm, for 8 to 15 minutes, preferably for 10 minutes to 150 to 200 캜, preferably Preferably, the flame retardant additive is prepared by extrusion mixing at a temperature of 170 ° C. before the plastic itself is pyrolyzed.
상기와 같이 제조된 난연 첨가제를 아래의 표2에서와 같은 함량으로 ABS수지 100중량부에 대해 첨가하여 본 발명의 무독, 무연성 ABS난연성 수지 조성물을 만든다.The flame retardant additive prepared as described above is added to 100 parts by weight of the ABS resin in the content as shown in Table 2 below to make the nontoxic, flame retardant ABS flame retardant resin composition of the present invention.
<표 2>TABLE 2
상기 표2에서와 같이 ABS수지 100중량부에 대하여 표1에서의 조성비로 만들어진 실시 예1 ∼ 6의 난연 첨가제를 50 ∼ 70중량부를 각각 헨셀믹서기를 이용하여 1000rpm의 속도로 10분 이상 혼합한 후 직경 40mm 쌍출 압출기를 이용하여 컴파운딩을 실시하는데, 이때 압출기 실린더 내부는 약 200℃로 일정하게 한다. 이렇게 컴파운딩된 수지는 다시 냉각시켜 고화한 후 6온스 사출성형기를 이용하여 물성 시편을 제작한다.As shown in Table 2, 50 to 70 parts by weight of the flame retardant additives of Examples 1 to 6 made of the composition ratio in Table 1 were mixed with 100 parts by weight of ABS resin at a speed of 1000 rpm using a Henschel mixer, respectively, for 10 minutes or more. Compounding is carried out using a 40 mm diameter twin extruder, wherein the inside of the extruder cylinder is kept constant at about 200 ° C. The compounded resin is cooled and solidified again to prepare a physical specimen using a 6-ounce injection molding machine.
물성시편은 23℃에서 48시간 동안 에이징한 후, 물성 시험기기로 난연성은 물론 기계적 물성, 열안정성, 내후성, 광택도, 대전방지 효과 및 다이옥신, 다이퓨란 등 발생여부를 시행하고, 결과를 (표3)에 나타낸다.After aging at 48 ° C. for 48 hours, the test specimens were tested for physical properties, flame retardancy, mechanical properties, thermal stability, weather resistance, gloss, antistatic effect and dioxin, difuran, etc. 3) is shown.
<표 3>TABLE 3
<실험방법>Experimental Method
아이조드 충격강도 : ASTM D-456Izod Impact Strength: ASTM D-456
인장강도 : ASTM D-683Tensile Strength: ASTM D-683
열변형온도 : ASTM D-648Heat Deflection Temperature: ASTM D-648
난연도 : UL-94Flame retardant: UL-94
내후성 : 기기명 AATRAS 사 WEATHER-O-METERWeather Resistance: Device Name AATRAS WEATHER-O-METER
램프 Xenon Lamp 6500 watt Lamp Xenon Lamp 6500 watt
온도 63 ± 2C Temperature 63 ± 2C
시험방법 ; 상기온도에서 102분간 빛 조사를 하거나 또는 18분 동안 Test Methods ; Irradiate for 102 minutes at this temperature or for 18 minutes
빛 조사와 함께 물 분사하는 조건하에 실시 Conducted under water jet conditions with light irradiation
발암물질검출 : Gas chromatography - Mass spetrometerCarcinogen detection: Gas chromatography-Mass spetrometer
상기 결과에서 나타난 바와 같이, 본 발명의 수지 조성물을 이용하여 제작한 성형품은 기계적강도인 아이조드 충격강도, 인장강도와 내열성 및 난연성이 우수하고, 여타 물성도 우수한 것으로 확인되었다. 또한 내후성은 현재까지 개발된 난연성 수지보다 월등히 우수한 것으로 나타났다.As shown in the above results, it was confirmed that the molded article produced using the resin composition of the present invention is excellent in the Izod impact strength, tensile strength and heat resistance and flame retardancy, which is mechanical strength, and other physical properties. In addition, weather resistance was much better than the flame retardant resins developed to date.
상기와 같이 본 발명의 조성물은 제반물성이 뛰어나면서도 미국 UL94 연소규격에서도 각각 V-0의 우수한 난연등급을 나타낸다. 더욱이 최근 발암물질 규제로 인한 인체에 무독한 무독성 난연수지 조성물이라는 점에서 본 발명의 우수성을 나타내고 있다.As described above, the composition of the present invention exhibits excellent flame retardancy of V-0, respectively, even though the physical properties are excellent, even in the US UL94 combustion standard. In addition, the present invention shows the superiority of the present invention in that it is a nontoxic flame retardant resin composition which is harmless to humans due to the regulation of carcinogens.
특히 최근 화재 발생이 유독 가스 다량 발생과 관련 본 발명품은 유독가스 발생이 매우 적어서 발명의 가치를 더하는 바이다.In particular, the recent fire occurrence associated with the generation of a large amount of toxic gas is a very small amount of toxic gas generated by the present invention adds to the value of the invention.
본 발명에 따른 수지 조성물은 인체에 무독하고 화재시 연기 발생이 극도로 저하되어, 현재 기존 사용하고 있는 ABS 난연수지 대체 소재로 사용될 수 있다.The resin composition according to the present invention is toxic to the human body and extremely low smoke generation in the fire, it can be used as an alternative to the ABS flame retardant resin currently used.
따라서 그 사용범위가 난연성을 요구하는 건축자재를 비롯한 전기 콘세트, 배전반을 필두로 TV, 컴퓨터모니터, 노트북, 복사기, 냉장고, 세탁기 등의 폭 넓은 전자제품 분야에 응용되면 그 사용범위가 첨단 분야의 소재 까를 사용이 확대 될 것으로 전망되고 있다.Therefore, if the scope of application is applied to a wide range of electronic products such as TVs, computer monitors, laptops, photocopiers, refrigerators, washing machines, etc., including electrical constructions and switchboards, including construction materials requiring flame retardancy, the scope of use will be The use of material floors is expected to expand.
뿐만 아니라 기존 사용되던 ABS 난연수지는 그 사용되던 난연제의 단가가 매우 높아 난연수지 자체가 고가 있었으나, 본 발명품은 값 싼 무기물 난연제를 사용함으로서 그 사용량이 크게 증대될 것으로 판단된다.In addition, although the ABS flame retardant resin used in the past was very expensive, the flame retardant resin itself was expensive, but the use of the present invention is expected to be greatly increased by using a cheap inorganic flame retardant.
본 발명을 일부 실시 예에 의해 설명 하였으나, 본 발명은 이에 한정 되는 것이 아니며, 본 발명의 기술적 의도 및 범위를 벗어나지 않는 범위 내에서 여러 가지 변형 및 변경이 가능하다.Although the present invention has been described by some embodiments, the present invention is not limited thereto, and various modifications and changes can be made without departing from the technical intent and scope of the present invention.
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| US10196318B2 (en) * | 2014-02-28 | 2019-02-05 | Croda International Plc | Micronutrient compositions |
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| US10196318B2 (en) * | 2014-02-28 | 2019-02-05 | Croda International Plc | Micronutrient compositions |
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