KR20100027316A - Non-halogen flame-retardant polypropylene resin composition having high rigidity - Google Patents
Non-halogen flame-retardant polypropylene resin composition having high rigidity Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/49—Phosphorus-containing compounds
- C08K5/5399—Phosphorus bound to nitrogen
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/14—Glass
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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
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
Description
본 발명은 강성이 우수한 비할로겐계 난연 폴리프로필렌 수지 조성물에 관한 것으로서, 좀더 상세하게는 폴리프로필렌 수지에 유리섬유 등을 처방하여 내열성을 강화하고, 난연성과 내열안정성이 우수한 비할로겐 난연제를 통하여 난연성 확보한 강성이 우수한 비할로겐계 난연 폴리프로필렌 수지 조성물에 관한 것이다.The present invention relates to a non-halogen-based flame retardant polypropylene resin composition having excellent rigidity, and more specifically, to prescribe glass fiber or the like to polypropylene resin to enhance heat resistance, and to secure flame retardance through a non-halogen flame retardant having excellent flame resistance and heat stability. The present invention relates to a non-halogen flame-retardant polypropylene resin composition having excellent rigidity.
소형 내열가전 제품을 중심으로 내열성이 우수한 폴리프로필렌이 널리 사용되어 왔고, 특히 안정성 문제가 대두되면서 화재 위험성으로부터의 안전성 확보를 위하여 난연 폴리프로필렌이 광범위하게 사용되어 왔다.Polypropylene having excellent heat resistance has been widely used around small heat-resistant home appliances, and flame retardant polypropylene has been widely used to secure safety from fire hazards, especially as safety issues arise.
최근, 환경문제에 대한 관심이 고조되면서 기존의 할로겐계 난연제의 유해성 문제가 제기되면서 친환경적인 비할로겐계 난연소재로의 대체가 요구되어 왔다.Recently, as interest in environmental problems has increased, the problem of the existing halogen-based flame retardants has been raised, and replacement with environmentally friendly non-halogen-based flame retardant materials has been required.
반면에, 비할로겐계 난연제의 경우 기존의 할로겐계 난연제에 비하여 난연성이 열세이고 열안정성 등이 부족하여 용도확대의 걸림돌이 되어 왔다. On the other hand, non-halogen-based flame retardants have been inferior in flame retardancy and lack of thermal stability as compared to conventional halogen-based flame retardants, which has been an obstacle to expansion of use.
이와 관련하여 대한민국공개특허 2005-0110406호 및 2007-0063463호에서는 난연성 확보를 위하여 무기계 난연제인 수산화마그네슘을 적용하였으나, 수산화마그네슘의 경우 난연성이 부족함에 따라 동일한 난연 등급을 확보하기 위하여서는 기존의 할로겐계 난연제에 비하여 과량의 난연제가 첨가되어야 하므로 그에 따른 충격강도 등 물성 및 가공성의 저하를 피할 수 없는 한계가 있었다.In this regard, in Korean Patent Publication Nos. 2005-0110406 and 2007-0063463, magnesium hydroxide, an inorganic flame retardant, was applied to secure flame retardancy. However, magnesium hydroxide has a conventional halogen-based flame retardancy to secure the same flame retardant grade due to lack of flame retardancy. Compared with the flame retardant, an excessive amount of flame retardant has to be added, and thus, there is a limitation that the degradation of physical properties and processability such as impact strength is inevitable.
본 발명은 상기와 같은 종래기술들의 문제점을 해결하고자 하는 것으로, 비할로겐계 유기 난연제를 첨가함으로서 난연제의 함량을 감소시키고, 유리섬유(Glass Fiber) 등 필러(Filler)를 첨가하여 내열성과 강성을 향상시키고, 치수안정성을 확보한 난연성 폴리프로필렌 수지 조성물을 제공하는 것이다.The present invention is to solve the problems of the prior art as described above, by reducing the content of the flame retardant by adding a non-halogen-based organic flame retardant, improve the heat resistance and rigidity by adding a filler (glass fiber), etc. It is to provide a flame retardant polypropylene resin composition having a dimensional stability.
본 발명은 상기의 문제점을 해결하기 위한 것으로, 폴리프로필렌 수지 10.0 ~ 96.9중량%, 인계 난연제 1.0 ~ 40.0중량%, 난연조제 1.0 ~ 10.0중량%, 무기충전제 1.0 ~ 30.0중량%, 및 상용화제로서 변성 폴리프로필렌 0.1 ~ 10.0중량% 또는 유기실란 화합물 0.1 ~ 10.0중량%을 포함하는 것을 특징으로 하는 비할로겐계 난연 폴리프로필렌 수지 조성물을 제공한다.The present invention is to solve the above problems, polypropylene resin 10.0 to 96.9% by weight, phosphorus flame retardant 1.0 to 40.0% by weight, flame retardant aid 1.0 to 10.0% by weight, inorganic filler 1.0 to 30.0% by weight, and modified as a compatibilizer It provides a non-halogen flame-retardant polypropylene resin composition comprising 0.1 to 10.0% by weight of polypropylene or 0.1 to 10.0% by weight of the organosilane compound.
또한, 상기 인계 난연제는 암모늄 폴리포스페이트 또는 그 전처리 화합물인 것을 특징으로 한다.In addition, the phosphorus-based flame retardant is characterized in that the ammonium polyphosphate or a pretreatment compound thereof.
또한, 상기 난연조제는 트리스-투-하이드록시 에틸-이소시아눌레이트인 것을 특징으로 한다.In addition, the flame retardant aid is characterized in that tris-to-hydroxy ethyl-isocyanurate.
또한, 상기 무기충전제는 평균입경이 5 ~ 15㎛, 길이가 1 ~ 16mm 범위에서의 쵸핑된 스트랜드 형태의 유리섬유인 것을 특징으로 한다.In addition, the inorganic filler is characterized in that the glass fiber in the form of chopped strands in the range of the average particle diameter of 5 ~ 15㎛, length 1 ~ 16mm.
또한, 상기 폴리프로필렌 수지는 용융지수가 1 ~ 60g/10분인 결정성 프로필 렌 단독중합체 또는 에틸렌-프로필렌 공중합체인 것을 특징으로 한다.In addition, the polypropylene resin is characterized in that the crystalline propylene homopolymer or ethylene-propylene copolymer having a melt index of 1 ~ 60g / 10 minutes.
또한, 상기 변성 폴리프로필렌은 프로필렌 단독중합체, 에틸렌-프로필렌 공중합체 또는 프로필렌/알파-올레핀 비공역 디엔화합물 공중합체를 불포화 카르본산 또는 그 유도체에 의하여 변성한 것인 것을 특징으로 한다.In addition, the modified polypropylene is characterized in that the propylene homopolymer, ethylene-propylene copolymer or propylene / alpha-olefin nonconjugated diene compound copolymer modified by unsaturated carboxylic acid or derivatives thereof.
본 발명에 의하여 제조된 강성이 우수한 비할로겐계 난연 폴리프로필렌 수지 조성물은 난연성, 내열성 및 강성이 우수하고, 치수안정성을 확보한 폴리프로필렌 수지 조성물을 제공하여, 친환경 소재로 대체되는 드럼세탁기, 식기세척기 등 가전제품의 내장부품용 소재로 사용하기에 적합하다.Non-halogen flame-retardant polypropylene resin composition excellent in rigidity prepared by the present invention provides a polypropylene resin composition excellent in flame retardancy, heat resistance and rigidity, secured dimensional stability, drum washing machine, dishwasher replaced by environmentally friendly materials It is suitable for use as a material for interior parts of home appliances.
본 발명에 따른 강성이 우수한 비할로겐계 난연 폴리프로필렌 수지 조성물은 폴리프로필렌 수지 10.0 ~ 96.8중량%, 인계 난연제 1.0 ~ 40.0중량%, 난연조제 1.0 ~ 10.0중량%, 무기충전제 1.0 ~ 30.0중량%, 상용화제로서 변성 폴리프로필렌 0.1 ~ 10.0중량% 를 포함하는 것을 특징으로 한다.Non-halogen flame retardant polypropylene resin composition excellent in rigidity according to the present invention is polypropylene resin 10.0 ~ 96.8% by weight, phosphorus flame retardant 1.0 ~ 40.0% by weight, flame retardant aid 1.0 ~ 10.0% by weight, inorganic filler 1.0 ~ 30.0% by weight, commercialization It is characterized in that it comprises 0.1 to 10.0% by weight of modified polypropylene as a zero.
본 발명의 조성물에 포함되는 폴리프로필렌 수지는 용융지수(MI)가 1 ~ 60g/10분(ASTM D1238, 230℃)인 결정성 프로필렌 단독중합체 또는 에틸렌-프로필렌 공중합체가 바람직하다. 상기 용융지수가 1g/10분 미만인 경우에는 부품의 성형성이 양호하지 못하여 생산성이 저하되는 반면, 용융지수가 60g/10분을 초과할 경우 에는 충격강도가 급격히 저하된다. The polypropylene resin included in the composition of the present invention is preferably a crystalline propylene homopolymer or ethylene-propylene copolymer having a melt index (MI) of 1 to 60 g / 10 minutes (ASTM D1238, 230 ° C). When the melt index is less than 1g / 10 minutes, the moldability of the parts is not good, the productivity is lowered, whereas when the melt index exceeds 60g / 10 minutes, the impact strength is sharply lowered.
본 발명에서 사용되는 난연제는 폴리프로필렌 수지 조성물의 난연성 부여를 위해 비할로겐계 난연제가 사용되고, 구체적으로는 인계 난연제가 바람직하다. 인계 난연제로서는 암모늄 폴리포스페이트 또는 멜라민 등을 그 전처리 화합물로서 이용하여 표면처리한 암모늄 폴리포스페이트 제품 등을 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 a non-halogen flame retardant is used for imparting flame retardancy of the polypropylene resin composition, specifically, a phosphorus flame retardant is preferable. As the phosphorus flame retardant, it is preferable that ammonium polyphosphate or melamine or the like is used as the pretreatment compound. The use amount is preferably 1.0 to 40.0% by weight. If the content of the flame retardant is less than 1.0% by weight, the flame retardancy may not be sufficiently secured, and when the content of the flame retardant is more than 40.0% by weight, no further flame retardancy improvement effect may be expected, and the physical properties may be reduced and There is a risk of deterioration of workability.
본 발명에서 사용되는 난연조제로서는 트리스-투-하이드록시 에틸-이소시아눌레이트를 사용하며, 함량은 1.0 ~ 10.0중량%가 바람직하다. 난연조제의 함량이 1.0중량% 미만인 경우에는 인계 난연제와의 상승효과를 충분히 기대할 수 없으며, 10.0중량%를 초과하는 경우에는 더 이상의 난연성 향상 효과를 기대할 수 없다.As the flame retardant aid used in the present invention, tris-to-hydroxy ethyl-isocyanurate is used, and the content is preferably 1.0 to 10.0% by weight. If the content of the flame retardant aid is less than 1.0% by weight can not be expected a synergistic effect with the phosphorus-based flame retardant sufficiently, if more than 10.0% by weight can not be expected to further improve the flame retardancy.
본 발명의 조성물에 포함되는 무기충전제로서는 혼련성 작업을 고려하여 평균입경이 5 ~ 15㎛, 길이가 1 ~ 16mm 범위에서의 쵸핑된 스트랜드 형태(chopped strand)의 유리섬유를 사용하는 것이 바람직하지만 이에 한정되는 것은 아니다. 상기 유리섬유는 평균입경이 5㎛ 미만인 경우 혼합하는 동안에 대부분이 깨지게 되어 강성발현 효과가 미흡해지며, 15㎛를 초과할 경우에는 성형품의 변형이 악화되어 외관 상태가 불량해진다. 또한, 무기충전제의 함량은 1.0 ~ 30.0중량% 사용되는 것이 바람직한데, 무기충전제의 함량이 1.0중량% 미만인 경우에는 강성발현의 효과가 미흡하며, 30.0중량%를 초과할 경우에는 압출 작업성이 떨어지고, 또한 휨 현상이 유발되어 외관상태가 양호하지 못하다.As the inorganic filler included in the composition of the present invention, in consideration of the kneading operation, it is preferable to use chopped strand glass fibers having an average particle diameter of 5 to 15 µm and a length of 1 to 16 mm. It is not limited. When the glass fiber has an average particle diameter of less than 5 μm, most of the glass fibers are broken during mixing, so that the rigid expression effect is insufficient, and when the glass fiber exceeds 15 μm, the deformation of the molded article is deteriorated and the appearance is poor. In addition, the content of the inorganic filler is preferably used 1.0 to 30.0% by weight, when the content of the inorganic filler is less than 1.0% by weight the effect of rigid expression is insufficient, when the content exceeds 30.0% by weight extrusion workability is inferior In addition, the appearance of warp is poor due to warpage.
본 발명의 조성물에 포함되는 상용화제는 폴리프로필렌 및 무기충전제와의 혼련성 향상을 위해 사용되고, 구체적으로는 변성 폴리프로필렌 또는 유기실란 화합물이 바람직하다. The compatibilizer included in the composition of the present invention is used for improving kneading with polypropylene and an inorganic filler, and specifically, a modified polypropylene or an organosilane compound is preferable.
상기 변성 폴리프로필렌은 프로필렌 단독중합체, 에틸렌/프로필렌 공중합체 또는 프로필렌/알파-올레핀 비공역 디엔화합물 공중합체를 불포화 카르본산 또는 그 유도체에 의하여 변성한 것으로, 그 함량은 0.1 ~ 10.0중량%가 바람직하다. 변성 폴리프로필렌의 함량이 0.1중량% 미만인 경우에는 무기충전제와 폴리프로필렌 수지와의 계면 접착력을 충분히 유지할 수 없어 물성 향상효과가 없으며, 10.0중량%를 초과하는 경우에는 더 이상의 물성 향상효과가 없다. The modified polypropylene is obtained by modifying a propylene homopolymer, an ethylene / propylene copolymer or a propylene / alpha-olefin nonconjugated diene compound copolymer with an unsaturated carboxylic acid or a derivative thereof, and the content thereof is preferably 0.1 to 10.0% by weight. . When the content of the modified polypropylene is less than 0.1% by weight, the interfacial adhesion between the inorganic filler and the polypropylene resin may not be sufficiently maintained, and when the content of the modified polypropylene is greater than 10.0% by weight, there is no further improvement in physical properties.
본 발명의 폴리프로필렌 수지 조성물에는 상기의 구성성분 이외에도 보강재, 내열안정제, 내후안정제, 대전방지제, 활제, 슬립제, 산화방지제, 안료, 염료 등과 같은 통상의 각종 첨가제가 본 발명의 특징에 어긋나지 않는 범위 내에서 첨가될 수 있으며, 그 구체적인 예로는 탈크, 운모, 탄소섬유, 탄산칼슘, 황산칼슘, 클레이, 실리카, 알루미나, 카본블랙, 수산화마그네슘, 제올라이트, 황산바륨 등을 들 수 있다.In the polypropylene resin composition of the present invention, in addition to the above components, a range of conventional additives such as reinforcing materials, heat stabilizers, weather stabilizers, antistatic agents, lubricants, slip agents, antioxidants, pigments, dyes, and the like do not deviate from the characteristics of the present invention. Specific examples thereof include talc, mica, carbon fiber, calcium carbonate, calcium sulfate, clay, silica, alumina, carbon black, magnesium hydroxide, zeolite, barium sulfate, and the like.
본 발명에 따른 폴리프로필렌 수지 조성물을 제조하는 방법으로는 2축 압출 기를 사용하여 혼련하는 것이 바람직하며, 무기충전제로서 유리섬유를 사용하므로 보편적으로 잘 알려진 것과 같이 충분하게 유리섬유의 형상유지를 위하여 유리섬유를 압출기 도중에서 측면 투입하는 제조공정을 이용하고, 폴리프로필렌 융점 이상에서 배합과 제조하는 것이 바람직하다. As a method for producing the polypropylene resin composition according to the present invention, it is preferable to knead using a twin screw extruder, and because glass fiber is used as the inorganic filler, glass is sufficiently maintained for maintaining the shape of the glass fiber as is commonly known. It is preferable to mix | blend and manufacture a fiber more than polypropylene melting | fusing point using the manufacturing process which introduces a fiber side by side in the middle of an extruder.
본 발명은 하기의 실시예에 의하여 보다 구체적으로 이해될 수 있으며, 하기의 실시예는 본 발명을 예시하기 위한 예에 지나지 않으며, 본 발명의 보호 범위를 제한하고자 하는 것은 아니다. The present invention can be understood in more detail by the following examples, which are only examples for illustrating the present invention, and are not intended to limit the protection scope of the present invention.
실시예Example 1 및 1 and 비교예Comparative example 1~2 1 ~ 2
하기에 기재된 성분을 포함하는 실시예 1 및 비교예 1~2의 폴리프로필렌 수지 조성물을 합성하였다.The polypropylene resin composition of Example 1 and Comparative Examples 1-2 containing the component described below was synthesize | combined.
1) 폴리프로필렌: 고결정성 폴리프로필렌, 삼성토탈, 용융지수(MI): 10g/10분 1) Polypropylene: Highly crystalline polypropylene, Samsung Total, Melt index (MI): 10g / 10min
2) 브롬계 난연제 : 비스-펜타브로모페녹시-에탄, Albemarle, 브롬함량 82.3% 2) Bromine-based flame retardants: Bis-pentabromophenoxy-ethane, Albemarle, Bromine content 82.3%
3) 인계 난연제 : 암모늄 폴리포스페이트, Budenheim, P2O5 68%3) Phosphorus flame retardant: ammonium polyphosphate, Budenheim, P 2 O 5 68%
4) 난연조제 : 트리스-투-하이드록시 에틸-이소시아눌레이트, BASF, Mw : 261.24) Flame retardant aid: Tris-to-hydroxy ethyl-isocyanurate, BASF, Mw: 261.2
5) 무기충전제 : 유리섬유, NEG, 입경 9∼13㎛/길이 3.0∼4.5mm5) Inorganic filler: glass fiber, NEG, particle size 9 ~ 13㎛ / length 3.0 ~ 4.5mm
6) 변성폴리프로필렌 : 반응된 무수말레인산을 중량기준 0.2중량% 이상 포함하는 용융지수 100g/10분인 변성폴리프로필렌, 삼성토탈 6) Modified polypropylene: Modified polypropylene with 100g / 10min of melt melt index containing 0.2% by weight or more of reacted maleic anhydride by weight, Samsung Total
표 1과 같은 성분 및 배합 비율로, 폴리프로필렌, 난연제 및 난연조제, 변성 폴리프로필렌 및 안정제를 헨셀믹서로 드라이 블렌드한 후, JSW TEX44 알파(ALPHA) 2축 혼련압출기의 호퍼에 한번에 모두 투입시키고, 유리섬유는 압출기 도중 측면공급으로 투입하여 압출기 내부에서 함께 용융 혼련하여 동 수지 조성물을 제조한 후, 삼성클뢰크너 FCM-110(형체력=110톤)을 이용하여 사출성형방법으로 ASTM D790 규격에서 규정한 굴곡강도 측정용 시편과 ASTM D256 규격에서 규정한 Izod 충격강도 측정용 시편, UL94에서 규정한 난연 시편을 제작하였다.With the ingredients and blending ratios shown in Table 1, polypropylene, flame retardant and flame retardant aids, modified polypropylene and stabilizers 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, The glass fiber was fed into the side feed during the extruder, melt kneaded together in the extruder to produce the copper resin composition, and then injection molding using Samsung Klucner FCM-110 (molding force = 110 tons) was defined in ASTM D790 standard. Flexural strength test specimens, Izod impact strength measurement specimens specified in ASTM D256 standard, and flame retardant specimens specified in UL94 were fabricated.
UL94 에서 규정한 난연 시편을 이용하여 UL94 수직연소시험을 통하여 난연성 평가 결과, V-0등급의 난연성을 확보하였음을 확인할 수 있었다. As a result of flame retardancy evaluation through the UL94 vertical combustion test using the flame retardant specimen specified by UL94, it was confirmed that the flame retardancy of the V-0 grade was secured.
다음으로, ASTM D790 규격 기준에 의거하여 굴곡강도를 측정하였으며, ASTM D256 규격 기준에 의거하여 Izod 충격강도를 비교 측정한 결과, 기계적 물성 특히 강성이 매우 우수함을 확인할 수 있었다. 측정 결과를 하기 표 3에 나타내었다.Next, the flexural strength was measured based on ASTM D790 standard, and the Izod impact strength was measured based on the ASTM D256 standard. The measurement results are shown in Table 3 below.
비할로겐계 난연제를 적용하고 유리섬유를 첨가한 실시예-1에서 기존의 할로겐계 난연제를 적용하고 Talc를 첨가한 비교예-1과 같은 수준의 난연성을 확보 할 수 있었고, 비할로겐계 난연제를 적용하고 Talc를 첨가한 비교예-2 에 비하여, 굴곡탄성율과 Izod 충격강도 등 전반적으로 우수한 물성을 확보할 수 있었다.The non-halogen-based flame retardant was applied to the same halogen-based flame retardant as in Example-1 to which glass fiber was added and the halogen-based flame retardant to Comparative Example-1 to which Talc was added. In comparison with Comparative Example-2 containing Talc, excellent physical properties such as flexural modulus and Izod impact strength were obtained.
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