KR100656832B1 - Flame retardant polypropylene resin composition with good weatherability - Google Patents
Flame retardant polypropylene resin composition with good weatherability Download PDFInfo
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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
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0066—Flame-proofing or flame-retarding additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/36—Silica
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C08L2666/00—Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
- C08L2666/66—Substances characterised by their function in the composition
- C08L2666/84—Flame-proofing or flame-retarding additives
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Abstract
본 발명은 내후성이 우수한 난연성 폴리프로필렌 수지 조성물에 관한 것으로서, 좀더 상세하게는 폴리프로필렌 수지, 무기충전제, 난연제, 난연조제 및 UV안정제를 포함하는 내후성이 우수한 난연성 폴리프로필렌 수지 조성물에 관한 것이다. The present invention relates to a flame retardant polypropylene resin composition having excellent weather resistance, and more particularly to a flame retardant polypropylene resin composition having excellent weather resistance including a polypropylene resin, an inorganic filler, a flame retardant, a flame retardant aid and a UV stabilizer.
실리카, 규회석, 폴리프로필렌, 강성, 내후성, 내광성, 난연제, UV안정제 Silica, wollastonite, polypropylene, rigidity, weather resistance, light resistance, flame retardant, UV stabilizer
Description
본 발명은 내후성이 우수한 난연성 폴리프로필렌 수지 조성물에 관한 것으로서, 좀더 상세하게는 폴리프로필렌 수지, 무기충전제, 난연제, 난연조제 및 UV안정제를 포함하는 내후성이 우수한 난연성 폴리프로필렌 수지 조성물에 관한 것이다. The present invention relates to a flame retardant polypropylene resin composition having excellent weather resistance, and more particularly to a flame retardant polypropylene resin composition having excellent weather resistance including a polypropylene resin, an inorganic filler, a flame retardant, a flame retardant aid and a UV stabilizer.
폴리프로필렌 수지는 범용수지임에도 기계적 물성과 성형성이 뛰어나 자동차 내장부품, 가전부품 및 산업자재 등의 공업적 이용범위가 매우 넓은 소재이다. 특히 최근에 와서는 기존에 스틸(steel)을 적용하였던 에어컨 실외기 또는 옥외 스피커 하우징 등이 성형성과 조립이 용이한 폴리프로필렌 사출성형물로 본격적으로 진행되어 왔다. Although polypropylene resin is a general-purpose resin, it has excellent mechanical properties and formability, and thus has a wide range of industrial applications such as automobile interior parts, home appliances parts, and industrial materials. In particular, the air conditioner outdoor unit or outdoor speaker housing, which has recently been applied to steel, has been in full swing as a polypropylene injection molded product that is easy to form and assemble.
그러나, 폴리프로필렌은 화학구조상 화재발생시 기존 스틸에 비하여 자기 소화 능력이 부족하여 안전문제가 대두되고, 난연성을 확보하기 위하여 난연화를 추진한 결과, 내광성 및 내후성이 현저하게 저하되어 옥외에서의 사용에 있어서 문제를 드러내면서 용도의 확대가 둔화되었다. However, due to its chemical structure, polypropylene has less self-extinguishing ability than existing steels, resulting in safety problems, and flame retardancy has been promoted to secure flame retardancy. Increasing use has slowed while revealing problems.
이러한 문제점을 개선하여 위하여 난연성 폴리프로필렌 수지에 내광제 및 내 후안정제를 첨가함으로써, 난연성 폴리프로필렌 수지의 단점인 내광성 및 내후성을 향상시키는 방법이 다양하게 제시되고 있다. In order to improve these problems, various methods for improving the light resistance and weather resistance, which are disadvantages of the flame retardant polypropylene resin, have been proposed by adding a light resistant agent and a post stabilizer to the flame retardant polypropylene resin.
이와 관련하여 일본국 특개평5-214174호, 일본국 특개평8-49282호 및 일본국 특개평6-136188호 등에 폴리프로필렌에 난연제 및 UV안정제를 첨가하여 내후성을 개선시킨 조성물이 상용화되어 있으나, 탈크와 같은 충전제 첨가시 난연성 확보가 어렵고, 품질관리가 까다로우며 내후안정제의 처방량도 매우 많아서 원가가 높게 상승함에 따라 용도확대가 제한적이었다. In this regard, Japanese Patent Laid-Open Publication No. 5-214174, Japanese Patent Laid-Open Publication No. 8-49282, and Japanese Patent Laid-Open Publication No. 6-136188, etc. have been commercialized to improve the weather resistance by adding a flame retardant and UV stabilizer to polypropylene. When fillers such as talc are added, flame retardancy is difficult to secure, quality control is difficult, and the prescription amount of weather stabilizer is very high.
본 발명은 상기와 같은 종래기술들의 문제점을 해결하고자 하는 것으로, 종래의 난연화 폴리프로필렌에 탈크 첨가시 문제로 되었던 난연성의 저하방지가 가능한 무기충전제, 내광성이 우수한 난연제 및 내광성 향상효과가 탁월한 UV안정제를 첨가하여 장기간 사용하여도 산화에 의한 물성저하를 최소화함으로써 우수한 내후성 및 난연성을 획득할 수 있는 내후성이 우수한 난연성 폴리프로필렌 수지 조성물을 제공하는 것이다.The present invention is to solve the problems of the prior art as described above, inorganic fillers that can prevent the reduction of flame retardancy which was a problem when adding talc to the conventional flame retardant polypropylene, flame retardant excellent light resistance and UV stabilizer excellent in light resistance improvement effect It is to provide a flame-retardant polypropylene resin composition excellent in weatherability that can be obtained excellent weatherability and flame retardancy by minimizing the physical property degradation by oxidation even after long-term use by the addition.
본 발명에 따른 내후성이 우수한 난연성 폴리프로필렌 수지 조성물은, 폴리프로필렌 수지 30.0∼96.0중량%, 무기충전제로서 실리카 또는 규회석 1.0∼50.0중량%, 브롬계 난연제 1.0~40.0중량%, 난연조제 1.0~15.0중량% 및 UV안정제 0.01~10.0중량%를 포함하는 것을 특징으로 한다.The flame-retardant polypropylene resin composition excellent in weatherability according to the present invention is 30.0 to 96.0% by weight of polypropylene resin, 1.0 to 50.0% by weight of silica or wollastonite as inorganic filler, 1.0 to 40.0% by weight of brominated flame retardant, 1.0 to 15.0% of flame retardant % And 0.01 to 10.0% by weight UV stabilizer is characterized in that it comprises.
본 발명에서 사용되는 폴리프로필렌 수지는 용융지수(MI)가 1~50g/10분(ASTM D1238, 230℃)인, 결정성을 갖는 프로필렌 단독중합체 및 에틸렌-프로필렌 공중합체가 바람직하다. 상기 용융지수가 1g/10분 미만인 경우에는 부품의 성형성이 양호하지 못하여 성형불량을 초래할 수 있는 반면, 용융지수가 50g/10분을 초과할 경우에는 충격강도가 급격히 저하되어 옥외 사용 등 가혹한 제품 사용조건에 부적합하다. The polypropylene resin used in the present invention is preferably a propylene homopolymer and an ethylene-propylene copolymer having a melt index (MI) of 1 to 50 g / 10 minutes (ASTM D1238, 230 ° C). When the melt index is less than 1g / 10 minutes, the moldability of the parts may not be good, which may result in molding defects. On the other hand, when the melt index exceeds 50g / 10 minutes, the impact strength is sharply lowered, so that the product is harsh for outdoor use. Not suitable for conditions of use
본 발명에서 사용되는 무기충전제로는 실리카 혹은 규회석이 바람직하다. As the inorganic filler used in the present invention, silica or wollastonite is preferable.
상기 실리카의 경우, 외관 및 작업성을 고려하여 평균입경이 1~15㎛인 것을 사용하는 것이 바람직하다. 평균입경이 1㎛ 미만인 경우에는 혼합과정에서 미세분말과 같이 날리게 되어 적정함량 조절 및 분산성이 문제될 수 있으며, 15㎛를 초과하는 경우에는 성형품의 외관 상태가 불량해진다. 또한, 실리카의 함량은 1.0~50.0중량%인 것이 바람직한데, 실리카 함량이 1.0중량% 미만인 경우에는 강성발현 및 수축율 개선의 효과가 미흡하며, 50.0중량%를 초과하는 경우에는 압출 작업성이 떨어지고, 외관상태가 양호하지 못하다. In the case of the silica, it is preferable to use an average particle diameter of 1 ~ 15㎛ in consideration of appearance and workability. If the average particle diameter is less than 1㎛ to fly like fine powder in the mixing process may be a problem of proper content control and dispersibility, if it exceeds 15㎛ the appearance of the molded article is poor. In addition, the content of silica is preferably 1.0 to 50.0% by weight, when the silica content is less than 1.0% by weight, the effects of improving rigidity and shrinkage are inadequate, and when exceeding 50.0% by weight, extrusion workability is inferior. The appearance is not good.
상기 규회석의 경우, 혼련성 작업을 고려하여 평균입경이 5∼15㎛, 길이가 1∼16mm 범위인 스트랜드 형태(chopped strand)를 사용하는 것이 바람직하다. 또한, 규회석의 함량은 1.0~50.0중량%인 것이 바람직한데, 규회석의 함량이 1.0중량% 미만인 경우에는 강성발현의 효과가 미흡하며, 50.0중량%를 초과하는 경우에는 압출 작업성이 떨어지고 외관상태가 양호하지 못하다. In the case of wollastonite, it is preferable to use a chopped strand having an average particle diameter of 5 to 15 µm and a length of 1 to 16 mm in consideration of the kneading operation. In addition, the content of wollastonite is preferably 1.0 to 50.0% by weight, but when the content of wollastonite is less than 1.0% by weight, the effect of stiffness is inadequate, and when it exceeds 50.0% by weight, extrusion workability is inferior and the appearance is poor. Not good
본 발명에서 사용되는 난연제는 폴리프로필렌 수지 조성물의 난연성 부여를 위해 사용되고, 구체적으로는 브롬(Br)계 난연제가 바람직하다. Br계 난연제로서는 트리스(트리브로모펜틸)포스페이트 또는 1,2-비스-펜타브로모페녹시에탄이 사용되는 것이 바람직하다. 사용함량은 1.0~40.0중량%가 바람직한데, 난연제의 함량이 1.0중량% 미만인 경우에는 난연성을 충분히 확보할 수 없으며, 40.0중량%를 초과하는 경우에는 더 이상의 난연성 향상 효과를 기대할 수 없고 물성 저하 및 작업성 저하를 초래할 우려가 있다. The flame retardant used in the present invention is used for imparting flame retardancy of the polypropylene resin composition, and specifically, a bromine (Br) -based flame retardant is preferable. As the Br-based flame retardant, tris (tribromopentyl) phosphate or 1,2-bis-pentabromophenoxy ethane is preferably used. When the content of the flame retardant is less than 1.0% by weight, the flame retardancy cannot be sufficiently secured. When the content of the flame retardant is less than 1.0% by weight, the effect of improving the flame retardancy can not be expected. There is a risk of deterioration of workability.
본 발명에서 사용되는 난연조제로서는 삼산화안티몬을 사용하며, 함량은 1.0~15.0중량%가 바람직하다. 난연조제의 함량이 1.0중량% 미만인 경우에는 Br계 난연제와의 상승효과를 충분히 기대할 수 없으며, 15.0중량%를 초과하는 경우에는 더이상의 난연성 향상 효과를 기대할 수 없다. As the flame retardant aid used in the present invention, antimony trioxide is used, and the content is preferably 1.0 to 15.0% by weight. When the content of the flame retardant aid is less than 1.0% by weight, the synergistic effect with the Br-based flame retardant may not be sufficiently expected, and when the content of the flame retardant exceeds 15.0% by weight, no further flame retardancy improvement effect may be expected.
본 발명에서 사용되는 UV안정제는 폴리프로필렌의 내후성 향상을 위하여 사용되고, 그 예로서는 2-(2'-히드록시-3'-터셔리-부틸-5-메틸페닐)-5-클로로-벤조트리아졸로 대표되는 벤조트리아졸계, 비스-(2,2,6,6-테트라메틸-4-피페리디닐)세바케이트로 대표되는 세바케이트계, 2-히드록시-4-n-옥틸옥시벤조페놀로 대표되는 벤조페논계, 폴리-{[6-(1,1,3,3-테트라메틸부틸-이미노)-1,3,5-트리아지노-2,2-디일][2-(2,2,6,6-테트라메틸피페리디닐)-아미노]-헥사메틸렌-[4-(2,2,6,6-테트라-메틸피페리디닐)이미노]}, 폴리{(6-몰포리노-s-스트라진-2,4-디일)[(2,2,6,6-테트라메틸-4-피페리디닐)이미노]-헥산[(2,2,6,6-테트라메틸-4-피페라디일)이미노]} 중에서 선택된 하나 또는 둘 이상을 혼합하여 사용하는 것이 바람직하다. UV안정제의 함량은 0.01~10.0중량%가 바람직한데, UV안정제의 함량이 0.01중량% 미만인 경우에는 고분자의 산화방지 효과가 부족하여 내후성 개선 효과가 없으며, 10.0중량%를 초과 하는 경우에는 원가 상승으로 인하여 상업성이 결여되고, 물성저하를 초래할 수 있다. UV stabilizers used in the present invention are used to improve the weather resistance of polypropylene, and are represented by, for example, 2- (2'-hydroxy-3'-tertiary-butyl-5-methylphenyl) -5-chloro-benzotriazole. Benzotriazole-based, bis- (2,2,6,6-tetramethyl-4-piperidinyl) sebacate; benzoic, typified by 2-hydroxy-4-n-octyloxybenzophenol Phenone, poly-{[6- (1,1,3,3-tetramethylbutyl-imino) -1,3,5-triazino-2,2-diyl] [2- (2,2,6 , 6-tetramethylpiperidinyl) -amino] -hexamethylene- [4- (2,2,6,6-tetra-methylpiperidinyl) imino]}, poly {(6-morpholino-s- Strazine-2,4-diyl) [(2,2,6,6-tetramethyl-4-piperidinyl) imino] -hexane [(2,2,6,6-tetramethyl-4-piperadi I) imino]} is preferably used by mixing one or two or more selected from. The amount of UV stabilizer is preferably 0.01 to 10.0% by weight. If the content of the UV stabilizer is less than 0.01% by weight, the anti-oxidation effect of the polymer is insufficient, thereby improving the weather resistance, and when it exceeds 10.0% by weight, the cost increases. Due to this lack of commerciality, it can lead to property degradation.
본 발명의 내후성이 우수한 난연성 폴리프로필렌 수지 조성물에는 보강재, 충전제, 내열안정제, 내후안정제, 대전방지제, 활제, 슬립제, 안료, 염료 등과 같은 통상의 각종 첨가제가 본 발명의 특징에 어긋나지 않는 범위 내에서 첨가될 수 있으며, 그 구체적인 예로는 탄소섬유, 탄산칼슘, 클레이, 알루미나, 카본블랙, 수산화마그네슘, 제올라이트, 황산바륨 등을 들 수 있다. The flame retardant polypropylene resin composition having excellent weather resistance of the present invention includes a variety of conventional additives such as reinforcing materials, fillers, heat stabilizers, weather stabilizers, antistatic agents, lubricants, slip agents, pigments, dyes, and the like within the range of the characteristics of the present invention. Specific examples thereof include carbon fiber, calcium carbonate, clay, alumina, carbon black, magnesium hydroxide, zeolite, barium sulfate, and the like.
본 발명의 폴리프로필렌 수지 조성물을 제조하는 방법으로는 2축 압출기를 사용한 혼련이 바람직하며, 보편적으로 알려진 폴리프로필렌 수지 조성물을 제조하는 가공조건을 이용하고, 폴리프로필렌 융점 이상에서의 배합 또한 가능하다. As a method for producing the polypropylene resin composition of the present invention, kneading using a twin screw extruder is preferable, and mixing at a polypropylene melting point or more is also possible using processing conditions for producing a polypropylene resin composition which is commonly known.
본 발명은 하기 실시예 및 비교예에 의하여 보다 구체적으로 이해될 수 있으며, 하기의 실시예는 본 발명을 예시하기 위한 예에 지나지 않으며, 본 발명의 보호범위를 제한하고자 하는 것은 아니다.The present invention can be understood in more detail by the following examples and comparative examples, the following examples are only examples for illustrating the present invention, and are not intended to limit the protection scope of the present invention.
실시예 및 비교예Examples and Comparative Examples
표 1의 성분 및 배합 비율로, 폴리프로필렌 수지, 실리카 혹은 규회석, 난연제, 난연조제 및 UV안정제를 헨셀믹서로 드라이 블렌드한 후, JSW TEX44 알파(ALPHA) 2축 혼련압출기의 호퍼에 한번에 모두 투입하여 압출기 내부에서 함께 용융혼련하여 동 수지 조성물을 제조한 후, 삼성클뢰크너 FCM-110(형체력=110톤)으로 사출하여 ASTM규격에서 정하는 시편을 제작하고, 인장강도, 신율, 굴곡탄성율, 충격강도, 난연성 및 변색(외관)을 측정하였다. In the ingredients and blending ratios of Table 1, polypropylene resin, silica or wollastonite, flame retardant, flame retardant aid and UV stabilizer were dry blended with a Henschel mixer, and then all were added to the hopper of the JSW TEX44 Alpha (ALPHA) twin-screw kneading extruder at once. After melting and kneading together in the extruder to manufacture the resin composition, and then injected into Samsung Klucner FCM-110 (molding force = 110 tons) to produce a specimen specified in the ASTM standard, tensile strength, elongation, flexural modulus, impact strength, Flame retardancy and discoloration (appearance) were measured.
또한, 내광성 평가를 위하여 Weather-O-Meter에서 4000시간까지 어닐링하면서 인장강도, 아이조드 충격강도 및 변색 등 물성변화를 측정하였다. 그 결과를 표 1에 나타내었다. In addition, for evaluation of light resistance, annealing for up to 4000 hours at Weather-O-Meter was performed to measure changes in physical properties such as tensile strength, Izod impact strength and discoloration. The results are shown in Table 1.
각 시험물성별 시험조건은 다음과 같다. Test conditions for each test property are as follows.
1) 인장강도 및 신율 1) Tensile strength and elongation
ASTM D638의 방법으로 상온에서 측정하였다. It was measured at room temperature by the method of ASTM D638.
2) 굴곡탄성율 2) Flexural modulus
ASTM D790의 방법으로 상온에서 측정하였다. It was measured at room temperature by the method of ASTM D790.
3) 충격강도 3) impact strength
ASTM D256의 방법으로 상온에서 측정하였다. It was measured at room temperature by the method of ASTM D256.
4) 난연성 4) Flame retardant
UL94 수직 연소시험 방법으로 측정하였다. It was measured by the UL94 vertical combustion test method.
5) 변색도5) degree of discoloration
육안으로 변색을 관찰하였다. The discoloration was observed visually.
표 1의 실시예 1∼2와 비교예 1∼3에 사용된 각 성분에 대한 설명은 다음과 같다.The description of each component used in Examples 1-2 of Table 1 and Comparative Examples 1-3 is as follows.
1) 폴리프로필렌 : 고결정성 폴리프로필렌, 삼성토탈, 1) Polypropylene: Highly crystalline polypropylene, Samsung Total,
용융지수(MI):30g/10분 Melt Index (MI): 30g / 10min
2) 무기충전제 : 2) Inorganic fillers:
- 실리카 : 고순도 천연 결정성 실리카, KOSEM, 평균입경 4㎛ -Silica: High purity natural crystalline silica, KOSEM, average particle size 4㎛
- 규회석(Wollastonite) : NYCO Minerals, 평균입경 10㎛Wollastonite: NYCO Minerals, average particle diameter 10㎛
- 탈크(Talc, Magnesium silicate hydrate) : KOCH, 평균입경 10㎛, -Talc (Talc, Magnesium silicate hydrate): KOCH, average particle diameter 10㎛,
비중 2.9g/㎤ Specific gravity 2.9 g / cm 3
3) 난연제 : 3) Flame Retardant:
- 난연제-1 : 트리스(트리브로모펜틸)포스페이트, Deadsea Flame retardant-1: Tris (tribromopentyl) phosphate, Deadsea
- 난연제-2 : 데카브로모디페닐옥사이드, ALBERMALE -Flame retardant-2: decabromodiphenyl oxide, ALBERMALE
4) 난연조제 : 삼산화안티몬, Suzuhiro 4) Flame retardant aid: antimony trioxide, Suzuhiro
5) UV안정제 : UV제-1 : UV제-2 = 1:15) UV stabilizer: UV agent-1: UV agent-2 = 1: 1
- UV제-1 : 2-(2'-히드록시-3'-터셔리-부틸-5-메틸페닐)-5-클로로-벤조트리 UV agent-1: 2- (2'-hydroxy-3'-tertiary-butyl-5-methylphenyl) -5-chloro-benzotri
아졸, CIBA GEIGY Azole, CIBA GEIGY
- UV제-2 : 비스-(2,2,6,6-테트라메틸-4-피페리디닐)세바케이트UV agent-2: bis- (2,2,6,6-tetramethyl-4-piperidinyl) sebacate
상기 표 1의 결과에서 알 수 있듯이, 탈크를 적용한 비교예 1은 난연성 확보가 어려웠으며, 실리카 혹은 규회석에 내광성이 우수한 TPP 난연제를 적용한 실시예 1~2의 경우, DBDPO 난연제를 사용한 비교예 2~3에 비하여 W-O-M 장기 실험 후에도 변색 발생이 적었으며, 인장강도 및 아이조드 충격강도 등 물성이 유지되는 우수한 내후성을 나타내었다. As can be seen from the results of Table 1, Comparative Example 1 to which talc was applied was difficult to secure flame retardancy, and in Examples 1 to 2 where TPP flame retardants having excellent light resistance to silica or wollastonite were used, Comparative Examples 2 to 2 using DBDPO flame retardants. It showed less discoloration after WOM long-term test compared to 3, and showed excellent weather resistance that maintained physical properties such as tensile strength and Izod impact strength.
본 발명에 의하여 제조된 내후성이 우수한 난연성 폴리프로필렌 수지 조성물은 에어컨 실외기 하우징 및 옥외 스피커 하우징 등 옥외에서 사용됨에 따라 높은 내후성과 난연성을 요구하는 가전 및 산업용 부품류 소재로 사용하기에 적합하다.The flame-retardant polypropylene resin composition excellent in weatherability prepared according to the present invention is suitable for use in home appliances and industrial parts that require high weatherability and flame retardancy as it is used outdoors such as an air conditioner outdoor unit housing and an outdoor speaker housing.
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KR102154445B1 (en) * | 2019-11-06 | 2020-09-10 | 한화토탈 주식회사 | Flame-retardant Polypropylene Resin Composition with Excellent Resistance to Hot Wire Ignition |
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KR102154445B1 (en) * | 2019-11-06 | 2020-09-10 | 한화토탈 주식회사 | Flame-retardant Polypropylene Resin Composition with Excellent Resistance to Hot Wire Ignition |
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