KR101716207B1 - Polyketone Nano-Composite - Google Patents
Polyketone Nano-Composite Download PDFInfo
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- KR101716207B1 KR101716207B1 KR1020100139297A KR20100139297A KR101716207B1 KR 101716207 B1 KR101716207 B1 KR 101716207B1 KR 1020100139297 A KR1020100139297 A KR 1020100139297A KR 20100139297 A KR20100139297 A KR 20100139297A KR 101716207 B1 KR101716207 B1 KR 101716207B1
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Abstract
본 발명은 폴리케톤 나노복합체에 관한 것으로서, 알킬디아민기를 말단에 함유한 유기화제로 표면 처리된 유기화된 몬모릴로나이트를 포함하는 폴리케톤 나노복합체에 관한 것이다. 본 발명은 유기화된 몬모릴로나이트, 커플링제 및 폴리케톤 수지를 용융 혼합하여 컴파운딩법으로 제조된 폴리케톤 나노복합체를 제공하고, 종래 폴리케톤 수지보다 신도 및 충격 강도가 개선된 폴리케톤 나노복합체를 제공한다.TECHNICAL FIELD The present invention relates to a polyketone nanocomposite, and more particularly, to a polyketone nanocomposite comprising an organized montmorillonite surface-treated with an organic agent containing an alkyldiamine group at the terminal. The present invention provides a polyketone nanocomposite produced by compounding by melt-kneading organic montmorillonite, a coupling agent and a polyketone resin, and provides a polyketone nanocomposite having improved elongation and impact strength compared with conventional polyketone resins .
Description
본 발명은 폴리케톤 나노복합체에 관한 것으로서, 상세하게는 알킬디아민기를 말단에 함유한 유기화제로 표면처리된 몬모릴로나이트, 커플링제 및 폴리케톤 수지를 컴파운딩법으로 혼합하여 제조된 폴리케톤 나노복합체에 관한 것이다.TECHNICAL FIELD The present invention relates to a polyketone nanocomposite, and more particularly, to a polyketone nanocomposite prepared by mixing montmorillonite, a coupling agent and a polyketone resin surface-treated with an organic agent having an alkyldiamine group at the terminal thereof by a compounding method will be.
점토 광물을 이용한 고분자 나노복합체 제조기술은, 몬모릴로나이트와 같은 실리케이트 층상 구조를 가진 점토 광물을 나노 스케일의 판상 기본 단위로 박리하여 고분자 수지에 분산시키는 기술로서, 폴리에틸렌이나 폴리프로필렌과 같은 무극성 범용 고분자의 낮은 기계적 물성을 엔지니어링 플라스틱 수준까지 개선시킬 수 있는 방법이다.The technology for producing polymer nanocomposites using clay minerals is a technique for separating clay minerals having a silicate layer structure such as montmorillonite as a nanoscale plate-like basic unit and dispersing them in a polymer resin. It is a way to improve the mechanical properties to engineering plastics level.
그러나, 상기와 같이 판상의 몬모릴로나이트를 고분자 수지에 박리·분산시키는 것은 매우 힘들기 때문에 이를 해결하기 위하여 저분자량의 유기화제를 점토 광물 사이에 삽입시켜 판상의 실리케이트 간의 간격을 넓힘으로써 고분자 수지의 침투를 용이하게 하는 방법을 이용하고 있다.However, as described above, it is very difficult to remove and disperse the plate-like montmorillonite in the polymer resin. Therefore, in order to solve this problem, a low molecular weight organic agent is inserted between the clay minerals to widen the interval between the plate- It is easy to use the method.
점토 광물을 나노 스케일의 판상 기본 단위로 박리하여 고분자 수지에 분산시키는 방법으로는 용액법, 중합법, 컴파운딩법이 있으며, 이들 중 중합법과 컴파운딩법은 각각 80년대와 90년대에 기초 연구가 진행되어 현재 미국, 일본을 비롯한 서구선진국에서는 상업화까지 이루어진 기술이다.The clay minerals are separated into nanoscale plate-like basic units and dispersed in the polymer resin. Solution, polymerization, and compounding methods are available. Polymerization and compounding methods of these clay minerals are basic researches in the 1980s and 1990s It has been developed and commercialized in developed countries such as the US and Japan.
특히, 컴파운딩법은 용융 상태의 고분자쇄를 점토 광물 실리케이트 층 사이에 삽입시킨 다음 이를 기계적으로 혼합시켜 점토 광물을 분산시키는 기술로서, 1993년 코넬대 연구팀이 폴리스티렌 용융체를 직접 삽입시켜 층간 나노복합체를 제조하였으며, 1997년 일본 토요타 연구소에서 컴파운딩법에 의해 박리형 폴리프로필렌 나노복합체 제조 기술을 발표함으로써 이에 대한 연구가 세계적으로 진행되고 있다.In particular, the compounding method is a technique for dispersing clay minerals by inserting polymer chains in a molten state between clay mineral silicate layers and mechanically mixing them. In 1993, the Cornell team inserted polystyrene melts directly to manufacture interlayer nanocomposites In 1997, Toyota Research Laboratories of Japan announced the manufacture of peelable polypropylene nanocomposite by compounding method.
토요타 연구진의 기술에 의하면, 고분자의 기계적, 열적 특성을 향상시키기 위하여 컴파운딩시 일반적으로 첨가되던 기존의 무기물 충진재들이 고분자 사슬 내에 1마이크로 이상의 입자 크기로 덩어리져 분산되어 있기 때문에, 첨가된 무기물충진재의 양에 비해 기계적, 열적 강도의 향상이 미약한 단점을 개선할 수 있었다.According to the technology of Toyota researchers, in order to improve the mechanical and thermal properties of polymers, conventional inorganic fillers generally added during compounding are dispersed in a particle size of 1 micrometer or more in the polymer chain, so that the added inorganic filler It is possible to improve the mechanical strength and the thermal strength in comparison with the amount.
최근 이러한 나노복합체를 제조하는 종래 기술을 살펴보면, 한국 공개특허 10-2010-0022723에 따르면 나일론 66에 유기화 처리된 나노 클레이 물질을 혼합하고 강한 전단력을 이용하여 나노 클레이층 사이에 고분자를 삽입시키는 컴파운딩 방법을 이용하여 기계적 물성을 향상시킬 수 있었다.According to Korean Unexamined Patent Application Publication No. 10-2010-0022723, a nano-clay material which has been subjected to an organizing treatment is mixed with nylon 66, and a compounding method for inserting a polymer between nanoclay layers using a strong shear force The mechanical properties could be improved.
상기의 여러 선행 방법들은 충격 강도가 떨어지는 단점이 있고, 글리콜에 침투시 물성이 현저히 저하되는 단점이 있다.The above prior art methods have disadvantages in that the impact strength is lowered, and the physical properties upon penetration into glycols are remarkably deteriorated.
본 발명은 알킬기의 양 말단에 반응성이 우수한 아민기를 함유한 유기화제로 표면처리된 유기화된 몬모릴로나이트를 사용하여 신도 및 충격 강도가 개선된 폴리케톤 나노복합체를 제공하는 것을 목적으로 한다.An object of the present invention is to provide a polyketone nanocomposite having improved elongation and impact strength by using organominated montmorillonite surface-treated with an organic group having amine groups having excellent reactivity at both terminals of an alkyl group.
상기한 과제를 해결하기 위하여, 본 발명의 적절한 실시 형태에 따르면, 전체 나노복합체 중량에 대하여 유기화된 몬모릴로나이트 2∼10 중량%, 커플링제 0.5 내지 5중량% 및 폴리케톤 수지 85~97.5중량%를 포함하는 것을 특징으로 하는 폴리케톤 나노복합체를 제공한다.According to a preferred embodiment of the present invention, there is provided a composition comprising 2-10% by weight of organomonated montmorillonite, 0.5-5% by weight of a coupling agent and 85-97.5% by weight of a polyketone resin, based on the total weight of the nanocomposite Wherein the polyketone nanocomposite is a polyketone nanocomposite.
본 발명의 다른 적절한 실시 형태에 따르면, 상기 나노복합체는 신도 7.0∼30.0%, 충격강도 7.0∼30.0 kg·cm/cm, 및 굴곡탄성률 15,000∼30,000 kg/㎠인 것을 특징으로 한다.According to another preferred embodiment of the present invention, the nanocomposite has an elongation of 7.0 to 30.0%, an impact strength of 7.0 to 30.0 kg · cm / cm, and a flexural modulus of 15,000 to 30,000 kg / cm 2.
본 발명의 또 다른 적절한 실시 형태에 따르면, 상기 유기화된 몬모릴로나이트는 하기 화학식 1로 표시되는 알킬디아민기를 말단에 함유한 유기화제로 표면처리된 것인 것을 특징으로 한다.According to another preferred embodiment of the present invention, the organominated montmorillonite is characterized by being surface-treated with an organizing agent containing an alkyl diamine group represented by the following formula (1) at the terminal thereof.
[화학식 1][Chemical Formula 1]
H2N(CH2)nNH2 H 2 N (CH 2 ) n NH 2
상기에서 n은 6 내지 20의 정수이다.In the above, n is an integer of 6 to 20.
본 발명의 또 다른 적절한 실시 형태에 따르면, 상기 커플링제는 무수말레인산(maleic anhydride)이 그라프트된 폴리올레핀계 커플링제인 것을 특징으로한다.According to another preferred embodiment of the present invention, the coupling agent is a polyolefin-based coupling agent grafted with maleic anhydride.
본 발명에서 제조된 폴리케톤 나노복합체는 유기화된 몬모릴로나이트 및 커플링제가 포함되어 있어서 신도 및 충격 강도가 개선된다. 본 발명의 나노복합체는 자동차 외장 부품 중 내충격성을 요구하는 자동차 휠커버 부품으로 바람직하게 사용할 수 있다.The polyketone nanocomposite prepared according to the present invention includes organic montmorillonite and a coupling agent to improve elongation and impact strength. The nanocomposite of the present invention can be suitably used as an automobile wheeler part requiring impact resistance among automobile exterior parts.
이하에서 발명을 더욱 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명에 따른 폴리케톤 나노복합체는 유기화제로 표면처리된 몬모릴로나이트 및 커플링제를 폴리케톤과 컴파운딩법을 통해 용융 혼합하여 제조된다.
The polyketone nanocomposite according to the present invention is prepared by melt-mixing montmorillonite surface-treated with an organic agent and a coupling agent with a polyketone compounding method.
본 발명의 폴리케톤 나노복합체를 제조하기 위하여, 먼저 알킬디아민기를 말단에 함유한 유기화제로 표면처리하여 유기화된 몬모릴로나이트를 제조해야 한다.In order to prepare the polyketone nanocomposite of the present invention, it is necessary to prepare organic montmorillonite by surface treatment with an organic agent containing an alkyl diamine group at the terminal.
상기에서 사용된 알킬디아민 타입의 유기화제는 다음 화학식 1로 나타낸바와 같이, 알킬기의 양 말단에 반응성이 우수한 아민기가 결합되어 있기 때문에, 본 발명에서 사용되는 커플링제 내의 무수말레인산기(maleic anhydride)와의 반응성이 우수하여 최종 제조된 나노복합체의 신도 및 충격 강도의 개선 효과가 뛰어나다. The alkyldiamine-type organic coupling agent used in the present invention has an amine group having excellent reactivity at both terminals of the alkyl group as shown in the following formula (1). Therefore, the coupling agent of the alkyldiamine type with the maleic anhydride in the coupling agent used in the present invention The nanocomposite having excellent reactivity is excellent in improving elongation and impact strength of the final nanocomposite.
[화학식 1][Chemical Formula 1]
(H2N(CH2)12NH2)(H 2 N (CH 2 ) 12 NH 2 )
상기에서, n은 6 내지 20의 정수이다.In the above, n is an integer of 6 to 20.
한편, 상기와 같은 유기화된 몬모릴로나이트는 전체 나노복합체 중량대비 2∼10 중량%를 혼합하는 것이 바람직하다. 유기화된 몬모릴로나이트의 함량이 2중량% 미만이면 나노 점토 광물의 분산이 너무 활발하여 굴곡탄성률이 저하되는 문제가 있고, 10 중량%를 초과하는 경우 나노복합체의 신도와 충격 강도가 떨어지는 문제점이 있기 때문이다.
The organic montmorillonite is preferably mixed with 2 to 10% by weight based on the total weight of the nanocomposite. If the amount of the organomonated montmorillonite is less than 2% by weight, dispersion of the nano-clay mineral becomes too active to lower the flexural modulus of the nano-clay mineral. When the amount of the montmorillonite is more than 10% by weight, the elongation and impact strength of the nanocomposite deteriorate .
본 발명에서 상기 커플링제는 베이스 고분자인 폴리케톤 수지와 무기충진재인 유기화된 몬모릴로나이트 간의 상용성을 증진시킬 목적으로 사용된다.In the present invention, the coupling agent is used for the purpose of improving the compatibility between the polyketone resin as the base polymer and the organic montmorillonite as the inorganic filler.
구체적으로는 수평균 분자량이 10,000 이하인 올레핀계 올리고머 수지에 유기화된 몬모릴로나이트의 표면과 베이스 고분자인 폴리케톤 수지를 화학적으로 결합시킬 수 있는 무수말레인산이 그라프트된 것을 사용하는 것이 바람직하다. 상기 올레핀계 올리고머 수지의 수평균 분자량이 10,000을 초과할 경우에는 베이스 고분자인 폴리케톤 수지와의 상용성이 떨어져 신도와 충격 강도가 낮아지는 문제가 있다.Specifically, it is preferable to use grafted maleic anhydride which can chemically bond the surface of the montmorillonite organicized with the olefinic oligomer resin having a number average molecular weight of 10,000 or less and the polyketone resin as the base polymer. When the number average molecular weight of the olefinic oligomer resin exceeds 10,000, compatibility with the polyketone resin as a base polymer is deteriorated and the elongation and impact strength are lowered.
본 발명에서 커플링제는 전체 나노복합체 중량대비 0.5∼5 중량% 사용하는 것이 바람직하다. 본 발명에서는 수평균 분자량이 5,700인 이스트만사의 에폴렌 C-18(Epolene C-18)을 사용하였다.In the present invention, the coupling agent is preferably used in an amount of 0.5 to 5 wt% based on the total weight of the nanocomposite. In the present invention, Eastman's Epolene C-18 (Epolene C-18) having a number average molecular weight of 5,700 was used.
상기 커플링제의 첨가량이 0.5중량% 미만인 경우 첨가량이 미비해 신도와 충격 강도의 개선효과가 미흡하며, 5 중량%를 초과하는 경우 굴곡탄성률이 낮아져 나노 복합체로서의 목적을 달성할 수 없는 문제점이 있다. 따라서 커플링제의 첨가량은 전체 나노복합체 100 중량%에 대하여 0.5∼5중량%인 것이 바람직하다.
If the addition amount of the coupling agent is less than 0.5 wt%, the effect of improving the elongation and impact strength is insufficient and the flexural modulus is lowered when the addition amount is more than 5 wt%, so that the object of the nanocomposite can not be achieved. Therefore, the amount of the coupling agent to be added is preferably 0.5 to 5% by weight based on 100% by weight of the entire nanocomposite.
본 발명의 나노복합체의 베이스 고분자인 폴리케톤 수지는 통상의 것을 사용할 수 있으며, 통상적으로 폴리케톤 수지는 220℃ 융점을 가진다. 본 발명에서 폴리케톤 수지는 전체 나노복합체 중량 대비 85~97.5중량%인 것이 바람직하다. The polyketone resin, which is the base polymer of the nanocomposite of the present invention, may be any conventional one, and the polyketone resin usually has a melting point of 220 캜. In the present invention, the polyketone resin is preferably 85 to 97.5% by weight based on the total weight of the nanocomposite.
한편, 본 발명의 목적을 손상하지 않는 범위 내에서 열안정제, 이형제, 내후제 또는 안료 등을 첨가할 수 있다. 이와 같이 얻어진 나노복합체는 신도와 충격강도 등의 기계적 물성이 우수해진다.
On the other hand, a heat stabilizer, a releasing agent, a lubricant, a pigment, or the like may be added within the range not impairing the object of the present invention. The nanocomposite thus obtained is excellent in mechanical properties such as elongation and impact strength.
본 발명의 폴리케톤 나노복합체의 제조 과정은 다음과 같다.The process for producing the polyketone nanocomposite of the present invention is as follows.
먼저 이축 압출기를 이용하여 폴리케톤 수지, 커플링제 및 유기화된 몬모릴로나이트를 투입하여 용융 혼련시켜 칩(CHIP) 형태로 제조한다. 제조된 칩을 건조시킨 다음, 스크류식 사출기를 이용하여 각각의 시편을 제작한다.
First, a polyketone resin, a coupling agent and an organic montmorillonite are put into a twin-screw extruder and melted and kneaded to form a chip (CHIP). After drying the manufactured chips, each specimen is prepared by using a screw extruder.
제작된 시편의 물성평가는 다음과 같은 방법으로 수행한다.The properties of the prepared specimens are evaluated in the following manner.
1) 신도 : ASTM D638에 준하여 1/8 인치의 덤벨형 시편을 제작한 후, 50mm/분의 속도에서 측정하였다.1) Shindo: A 1/8 inch dumbbell specimen was prepared according to ASTM D638 and then measured at a speed of 50 mm / min.
2) 충격 강도 : ASTM D256에 준하여 1/4 인치의 시편을 제작하여 상온에서 아이조드 노치(Izod Notched) 충격강도를 측정하였다.2) Impact strength: A 1/4 inch specimen was prepared in accordance with ASTM D256 and the Izod Notched impact strength was measured at room temperature.
3) 굴곡탄성률 : ASTM D790에 준하여 1/4 인치의 시편을 제작한 후, 5mm/분의 속도에서 측정하였다.
3) Flexural modulus: A 1/4 inch specimen was prepared in accordance with ASTM D790 and then measured at a speed of 5 mm / min.
이하, 본 발명을 실시예에 의하여 상세히 설명하지만, 본 발명이 실시예에 의해 한정되는 것은 아니다.
Hereinafter, the present invention will be described in detail by way of examples, but the present invention is not limited to the examples.
실시예 1 ~ 4Examples 1 to 4
폴리케톤 고분자 수지, 에폴렌 C-18 커플링제 및 도데실디아민(H2N(CH2)12NH2)으로 유기화된 몬모릴로나이트를 245℃로 가열된 이축 압출기 내에서 용융 혼련하여 칩(chip) 형태로 제조하였다. 폴리케톤, 커플링제 및 유기화된 몬모릴로나이트의 조성 및 함량은 다음 표 1과 같다. 또한 각 실시예에서 사용된 유기화제는 Nanom® 1.30P(Nanocor Inc. (USA) 제조)이다. 제조된 칩은 제습형 건조기를 사용하여 5시간 동안 건조시킨 다음, 가열된 스크류식 사출기를 이용하여 용융 혼련과 같은 온도(245℃)에서 시편을 제작하였다.Montmorillonite organicized with polyketone polymer resin, epolene C-18 coupling agent and dodecylamine (H 2 N (CH 2 ) 12 NH 2 ) was melted and kneaded in a twin-screw extruder heated to 245 ° C. to form a chip . The composition and content of the polyketone, the coupling agent and the organic montmorillonite are shown in Table 1 below. The organic agent used in each example is Nanom ® 1.30P (manufactured by Nanocor Inc. (USA)). The prepared chip was dried for 5 hours using a dehumidifying dryer, and then a specimen was prepared at a temperature (245 ° C) such as melt kneading using a heated screw extruder.
제작된 시편을 이용하여 상기와 같은 방법으로 신도, 충격 강도, 굴곡탄성률 등을 측정하였으며, 그 결과는 다음 표 1에 나타내었다.The elongation, impact strength and flexural modulus of the prepared specimens were measured in the same manner as described above. The results are shown in Table 1 below.
(중량%)Polyketone
(weight%)
(2,820g)94
(2,820 g)
(2,700g)90
(2,700 g)
(2,760g)92
(2,760 g)
(2,640g)88
(2,640 g)
(중량%)Eploene C-18
(weight%)
(60g)2
(60 g)
(60g)2
(60 g)
(120g)4
(120 g)
(120g)4
(120 g)
(중량%)Montmorillonite
(weight%)
(120g)4
(120 g)
(240g)8
(240 g)
(120g)4
(120 g)
(240g)8
(240 g)
(%)Shindo
(%)
(kg·f·㎝/㎝)Impact strength
(kg · f · cm / cm)
(kg·f/㎠)Flexural modulus
(kg · f / cm 2)
비교예 1 ∼ 4Comparative Examples 1 to 4
폴리케톤 고분자 수지 및 에폴렌 C-18 커플링제를 포함하는 나노복합체를 실시예 1과 동일한 방법으로 제조하였다. 나노복합체의 각 성분의 함량은 다음 표 2과 같으며, 물성 평가 결과를 표 2에 나타내었다.A nanocomposite comprising a polyketone polymer resin and an epolene C-18 coupling agent was prepared in the same manner as in Example 1. The content of each component of the nanocomposite is shown in Table 2, and the evaluation results of the physical properties are shown in Table 2.
(중량%)Polyketone
(weight%)
(2,940g)98
(2,940 g)
(2,880g)96
(2,880 g)
(2,820g)94
(2,820 g)
(2,700g)90
(2,700 g)
(중량%)Eploene C-18
(weight%)
(60g)2
(60 g)
(120g)4
(120 g)
(180g)6
(180 g)
(30g)10
(30 g)
(%)Shindo
(%)
(kg·f·㎝/㎝)Impact strength
(kg · f · cm / cm)
(kg·f/㎠)Flexural modulus
(kg · f / cm 2)
상기 표 1와 2에 나타낸 것처럼, 본 발명의 폴리케톤 나노복합체는 유기화된 몬모릴로나이트를 사용하지 않은 나노복합체와 비교하여 신도 및 충격 강도가 우수한 것을 확인할 수 있다.As shown in Tables 1 and 2, the polyketone nanocomposite of the present invention is superior in elongation and impact strength as compared with nanocomposite not using organic montmorillonite.
Claims (4)
상기 유기화된 몬모릴로나이트는 하기 화학식 1로 표시되는 알킬디아민기를 말단에 함유한 유기화제로 표면처리된 것이며,
상기 나노복합체는 신도 27∼28%, 충격강도 21∼30 kg·cm/cm, 및 굴곡탄성률 25,320∼27,150 kg/㎠인 것을 특징으로 하는 폴리케톤 나노복합체.
[화학식 1]
H2N(CH2)nNH2
(상기에서 n은 6 내지 20의 정수이다.)4 to 8% by weight of organic montmorillonite, 2 to 4% by weight of a coupling agent and 90 to 94% by weight of a polyketone resin, based on the total weight of the nanocomposite,
The organominated montmorillonite is surface-treated with an organizing agent containing an alkyl diamine group represented by the following formula (1)
Wherein the nanocomposite has an elongation of 27 to 28%, an impact strength of 21 to 30 kg / cm / cm, and a flexural modulus of 25,320 to 27,150 kg / cm < 2 >.
[Chemical Formula 1]
H 2 N (CH 2 ) n NH 2
(Wherein n is an integer of 6 to 20)
상기 커플링제는 무수말레인산(maleic anhydride)이 그라프트된 폴리올레핀계 커플링제인 것을 특징으로 하는 폴리케톤 나노복합체.The method according to claim 1,
Wherein the coupling agent is a polyolefin-based coupling agent in which maleic anhydride is grafted.
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