KR20120004834A - Blend composition comprising polyketone and nylon 6 and manufacturing method of composite using it - Google Patents
Blend composition comprising polyketone and nylon 6 and manufacturing method of composite using it Download PDFInfo
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- KR20120004834A KR20120004834A KR1020100065526A KR20100065526A KR20120004834A KR 20120004834 A KR20120004834 A KR 20120004834A KR 1020100065526 A KR1020100065526 A KR 1020100065526A KR 20100065526 A KR20100065526 A KR 20100065526A KR 20120004834 A KR20120004834 A KR 20120004834A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/005—Processes for mixing polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L73/00—Compositions of macromolecular compounds obtained by reactions forming a linkage containing oxygen or oxygen and carbon in the main chain, not provided for in groups C08L59/00 - C08L71/00; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
Abstract
Description
본 발명은 폴리케톤과 나일론 6가 혼합된 블렌드 조성물 및 이를 이용한 복합재의 제조방법에 관한 것으로서, 본 발명의 블렌드 조성물은 별도의 상용화제를 포함하지 아니하면서도 우수한 기계적 물성을 나타낼 수 있어, 자동차용 엔진, 샤시, 내외장 플라스틱 부품 등으로 유용하게 적용할 수 있다.
The present invention relates to a blend composition of polyketone and nylon 6 and a method for producing a composite using the blend composition. The blend composition of the present invention may exhibit excellent mechanical properties without including a separate compatibilizer, and thus, an engine for an automobile. It can be usefully applied to the chassis, interior and exterior plastic parts, etc.
나일론 6는 내열성 및 내유성이 우수한 엔지니어링 플라스틱으로서 자동차용 엔진/샤시/내외장 플라스틱 부품 등에 널리 사용되고 있다. 그러나 나일론 분자 사슬에 존재하는 아마이드기에 의해 수분 흡수가 이루어져 사용 중 물성 및 치수 변화가 야기되며, 특히 겨울철에는 제설제로 사용되는 염화칼슘의 침투가 용이하여 물성이 악화되는 단점이 있다. Nylon 6 is an engineering plastic with excellent heat resistance and oil resistance, and is widely used in automobile engines, chassis, interior plastic parts, and the like. However, the water absorption is caused by the amide group present in the nylon molecular chain, causing a change in physical properties and dimensions during use. In particular, in winter, calcium chloride, which is used as a snow removing agent, is easily penetrated, thereby deteriorating physical properties.
나일론 6의 흡수성을 개선하기 위해 흡수성이 보다 낮은 나일론 66, 나일론 612, 나일론 12 등을 블렌드하여 사용하는 경우가 있으나, 흡수성 개선이 미미하거나 소재 가격이 많이 상승되는 단점이 있다. 또한 나일론 6의 내염화칼슘성 개선을 위해 나일론 612나 폴리에틸렌, 폴리프로필렌 등의 폴리올레핀을 블렌딩하여 사용하는 경우가 있으나, 나일론 6/나일론 612의 경우에는 가격상승이 과다하며, 나일론 6/폴리올레핀 블렌드의 경우에는 상용성 부재로 상용화제를 과다하게 사용하여야 하며, 물성 산포가 커지는 단점이 있다. 또한 부품에 따라서는 나일론 6의 내충격성 개선을 위해 MA-g-EOR (Maleic Anhydride grafted Ethylene Octene Rubber) 등의 변성 고무를 사용하지만 역시 가격이 상승하고, 강성이 저하되는 단점이 있다.In order to improve the absorbency of nylon 6, nylon 66, nylon 612, nylon 12, etc., which have a lower absorbency, may be used in a blend, but there are disadvantages in that the absorbency improvement is insignificant or the material price is increased. In addition, in order to improve the calcium chloride resistance of nylon 6, polyolefin such as nylon 612, polyethylene, and polypropylene may be blended, but the price increase is excessive in the case of nylon 6 / nylon 612, and in the case of nylon 6 / polyolefin blend There must be an excessive use of a compatibilizer in the absence of a compatibility, there is a disadvantage that the spread of physical properties. In addition, some parts use modified rubber such as MA-g-EOR (Maleic Anhydride grafted Ethylene Octene Rubber) to improve the impact resistance of nylon 6, but also have a disadvantage in that price increases and rigidity decreases.
한편, 폴리케톤은 일산화탄소, 에틸렌, 프로필렌을 단량체로 중합된 삼중공중합체 (terpolymer) 로서 나일론 6에 비해 내흡수성 및 내열성이 우수하고 가격이 저렴한 것으로 알려져 있으나 강성이 낮고 비중이 높은 단점이 있다.
On the other hand, polyketone is a terpolymer polymerized with carbon monoxide, ethylene, and propylene as a monomer, and is known to have excellent absorption and heat resistance and low cost compared to nylon 6, but has a disadvantage of low rigidity and high specific gravity.
이에 본 발명자들은 상기와 같은 문제점을 해결하고자 노력한 결과, 나일론 6와 폴리케톤을 일정 비율로 혼합하면 내염성, 내흡수성, 내충격성, 내열성 등의 성능이 현저하게 개선되어 자동차용 엔진, 샤시, 내외장 플라스틱 부품 소재로 적합하게 적용될 수 있다는 것을 확인함으로써 본 발명을 완성하게 되었다.Accordingly, the present inventors have tried to solve the above problems, when the mixture of nylon 6 and polyketone in a certain ratio, the performance of flame resistance, water absorption, impact resistance, heat resistance, etc. is remarkably improved, so that the engine, chassis, interior and exterior for automobiles The present invention has been completed by confirming that it can be suitably applied to plastic component materials.
따라서, 본 발명은 나일론 6와 폴리케톤을 일정 비율로 용융 블렌딩하여 나일론 6의 물성을 크게 개선한 블렌드 조성물을 제공하는데 그 목적이 있다.
Accordingly, an object of the present invention is to provide a blend composition in which nylon 6 and polyketone are melt blended at a predetermined ratio, thereby greatly improving the physical properties of nylon 6.
본 발명은, 하기 화학식 1로 표시되는 폴리케톤과 나일론 6가 30 : 70 ~ 90 : 10 의 중량비로 혼합되어 이루어지는 폴리케톤/나일론 6 블렌드 조성물을 그 특징으로 한다. The present invention is characterized by a polyketone / nylon 6 blend composition in which a polyketone represented by the following formula (1) and nylon 6 are mixed in a weight ratio of 30:70 to 90:10.
상기 화학식 1에서, n : m = 4 : 96 ~ 12 : 88 이다.
In Chemical Formula 1, n: m = 4: 96∼12: 88.
또한 본 발명은, 하기 화학식 1로 표시되는 폴리케톤과 나일론 6를 30 : 70 ~ 90 : 10 의 중량비로 혼합하고 이를 압출하는 단계를 포함하는 폴리케톤/나일론 6 복합재의 제조방법을 또다른 특징으로 한다.In another aspect, the present invention, the polyketone represented by the general formula (1) and nylon 6 in a weight ratio of 30: 70 ~ 90: 10 and a method for producing a polyketone / nylon 6 composite comprising the step of extruding it as another feature do.
[화학식 1][Formula 1]
상기 화학식 1에서, n : m = 4 : 96 ~ 12 : 88 이다. In Chemical Formula 1, n: m = 4: 96∼12: 88.
본 발명의 폴리케톤/나일론 6 복합재는 내충격성, 내열성, 내염성, 내흡수성 등이 나일론 6에 비하여 개선되어 자동차용 엔진, 샤시, 외장 부품 등에 적용되는 경우 내구성이 향상되고 원가를 절감되는 효과를 기대할 수 있다.
Polyketone / nylon 6 composite material of the present invention is expected to improve the impact resistance, heat resistance, flame resistance, water absorption and the like compared to nylon 6 when applied to automotive engines, chassis, exterior parts, etc. durability and cost reduction effect Can be.
도 1은 폴리케톤의 카르보닐기와 나일론 6의 아마이드기 상호 간에 생성되는 수소결합을 도식화한 것이다.1 is a schematic diagram of hydrogen bonds formed between the carbonyl group of polyketone and the amide group of nylon 6.
이하에서는 본 발명을 더욱 자세하게 설명하겠다.Hereinafter, the present invention will be described in more detail.
본 발명에 따른 폴리케톤/나일론 6 블렌드 조성물은 폴리케톤과 나일론 6이 30 : 70 ~ 90 : 10 의 중량비로 혼합되어 이루어지는 것을 특징으로 하며, 바람직하게는 50 : 50 ~ 80 : 20 의 중량비로 혼합되는 것이 좋다. 상기 폴리케톤의 함량이 상기 비율을 초과하는 경우에는 블렌드 조성물의 비중이 크게 증가하고, 블렌드의 내충격성 향상 효과가 미미한 단점이 있으며, 나일론 6의 함량이 상기 비율을 초과하는 경우에는 블렌드의 내염성, 내열성 및 내흡수성 향상 효과가 미미한 문제가 있다. The polyketone / nylon 6 blend composition according to the present invention is characterized in that the polyketone and nylon 6 are mixed in a weight ratio of 30:70 to 90:10, preferably in a weight ratio of 50:50 to 80:20. It is good to be. If the content of the polyketone exceeds the ratio, the specific gravity of the blend composition is greatly increased, and the impact resistance improvement effect of the blend is insignificant.If the content of nylon 6 exceeds the ratio, the flame resistance of the blend, There is a problem in that the effect of improving heat resistance and water absorption is insignificant.
이는 폴리케톤의 카르보닐기와 나일론 6의 아마이드기 상호 간에 수소결합이 가능하여, 별도의 상용화제를 사용하지 않은 채 복합재로 제조하여 기계적 물성의 개선할 수 있게 된다(도 1). It is possible to hydrogen bond between the carbonyl group of polyketone and the amide group of nylon 6, it is possible to improve the mechanical properties by producing a composite without using a separate compatibilizer (Fig. 1).
본 발명에서 폴리케톤은 하기 화학식 1로 표시되는 화합물을 사용한다. Polyketone in the present invention uses a compound represented by the following formula (1).
[화학식 1][Formula 1]
상기 화학식 1에서, n : m = 4 : 96 ~ 12 : 88 범위에 있는 화합물을 사용하는데, n : m = 4 : 96 미만일 경우, 소재 비중이 높아지고 내충격성이 낮아지는 단점이 있으며, n : m = 12 : 88 초과시에는 강성이 낮아지는 단점이 있다.In the above formula 1, using a compound in the range of n: m = 4: 96 ~ 12: 88, when n: m = 4: less than 96, there is a disadvantage that the specific gravity is high and the impact resistance is lowered, n: m = 12: When more than 88 has the disadvantage that the stiffness is lowered.
상기 폴리케톤은 당업계에 널리 알려진 방법을 통하여 제조될 수 있으며, 그 일례로, 하기 반응식 1과 같은 방법으로도 제조될 수 있다. The polyketone may be prepared by a method well known in the art, for example, may be prepared by the same method as Scheme 1 below.
[반응식 1]Scheme 1
상기 폴리케톤 및 나일론 6의 유동지수 (Melt Index)는 D ASTM 1238 조건에 따라 측정 시 각각 5 ~ 70 g/10분 범위에 있는 것이 바람직하다. 상기 유동지수가 5 g/10분 미만이면 부품 성형성이 취약해 지며, 유동지수가 70 g/10분 을 초과하면 충격 강도 등의 물성이 저하된다. 폴리케톤과 나일론 6의 유동지수 차는 30 g/10분 이하인 것이 바람직하며, 유동지수의 차가 30 g/10분 을 초과할 경우에는 다이 스웰 (die swell) 발생으로 인하여 가공성이 취약해 진다.The melt index of the polyketone and nylon 6 is preferably in the range of 5 to 70 g / 10 minutes, respectively, as measured according to the conditions of D ASTM 1238. If the flow index is less than 5 g / 10 minutes, the moldability of the component becomes weak, and if the flow index exceeds 70 g / 10 minutes, physical properties such as impact strength are lowered. It is preferable that the flow index difference between polyketone and nylon 6 is 30 g / 10 minutes or less. If the difference in flow index exceeds 30 g / 10 minutes, die swell occurs and the workability becomes weak.
또한, 본 발명의 블렌드 조성물은 각종 첨가제 및 보강제, 예를 들면 장기 내열안정제, 내후안정제, 착색제, 대전방지제, 활제, 슬립제(SLIP제), 난연제, 강성보강제, 충격보강제 등을 본 발명의 목적에 어긋나지 않는 범위에서 포함하는 것도 가능하다.In addition, the blend composition of the present invention includes various additives and reinforcing agents, for example, long-term heat stabilizer, weather stabilizer, colorant, antistatic agent, lubricant, slip agent (SLIP agent), flame retardant, stiffener, impact modifier, etc. It is also possible to include in the range which does not deviate.
또한 본 발명은 상기 폴리케톤/나일론 6 블렌드 조성물을 압출하여 복합재를 제조하는 방법을 권리범위로 포함하며, 이때 통상의 이축 압출기를 사용하여 용융블렌딩하여 제조되는 것이 바람직하다. 또한 상기 압출은 220 ~ 260 ℃ 범위에서 이루지는 것이 바람직한데, 220℃ 미만일 경우에는 상기 블렌드 조성물이 용융되지 않아 가공이 어려워지며, 260 ℃ 를 초과하면 조성물이 열화되어 충격강도 등의 기계적 물성이 낮아지는 문제가 있다. In addition, the present invention includes a method for producing a composite by extruding the polyketone / nylon 6 blend composition in the scope, it is preferably prepared by melt blending using a conventional twin screw extruder. In addition, the extrusion is preferably made in the range of 220 ~ 260 ℃, if less than 220 ℃ the blend composition is not melted and difficult to process, if it exceeds 260 ℃ the composition is deteriorated to lower the mechanical properties such as impact strength There is a problem.
이하 본 발명을 실시예에 의거하여 더욱 상세히 설명하겠는바, 본 발명이 다음 실시예에 의해 한정되는 것은 아니다.
Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by the following Examples.
[실시예][Example]
실시예Example 1 : One : 폴리케톤Polyketone /나일론 6 복합재의 제조/ Nylon 6 Composites
분자량 32,000인 하기 화학식 1의 폴리케톤(n : m = 7 : 93)과 나일론 6 (KN177N, 코오롱사)을 중량비 70 : 30 으로 혼합하고 이를 240 ℃에서 용융 블렌딩하였다.Polyketone (n: m = 7: 93) and nylon 6 (KN177N, Kolon) having a molecular weight of 32,000 were mixed at a weight ratio of 70:30 and melt blended at 240 ° C.
[화학식 1][Formula 1]
상기 폴리케톤과 나일론 6는 D ASTM 1238 조건에 따른 유동지수가 각각 50, 35 g/10분으로 나타났다. The polyketone and nylon 6 showed a flow index of 50 and 35 g / 10 min, respectively, according to the conditions of D ASTM 1238.
상기 용융블렌딩된 조성물을 동방향 이축 압출기를 사용하여 펠렛화 한 후, 조성물 내 수분 흡수에 의한 물성 약화를 고려하여 제조된 펠렛을 100℃ 오븐에서 6시간 동안 건조시켰다. 이후 이를 다시 사출기(Engel사, 한국, 형체력 150 톤)를 사용하여 사출시 온도는 피딩 호퍼부에서 노즐 순으로 230/240/245/245℃로, 사출압력은 400 bar 로 조절하면서 사출함으로써 규격 시편을 제조하였다.
After the melt blended composition was pelletized using a coaxial twin screw extruder, the prepared pellet was dried in an oven at 100 ° C. for 6 hours in consideration of physical property deterioration due to water absorption in the composition. Then, using an injection machine (Engel, Korea, clamping force of 150 tons), the temperature during injection is 230/240/245/245 ℃ from the feeding hopper to the nozzle and the injection pressure is adjusted to 400 bar. Was prepared.
실시예 2 Example 2
상기 폴리케톤과 나일론 6의 중량비가 50 : 50 으로 혼합되는 것을 제외하고는 상기 실시예 1과 동일하게 복합재를 제조하였다.
A composite material was prepared in the same manner as in Example 1, except that the weight ratio of the polyketone and nylon 6 was mixed at 50:50.
비교예 1 Comparative Example 1
실시예 1에서 폴리케톤만을 사용하여 펠렛화하고, 사출하는 것을 제외하고 동일하게 진행하여 폴리케톤 소재를 제조하였다.
Except for pelletizing using only the polyketone in Example 1, and proceeding in the same manner to produce a polyketone material.
비교예 2 Comparative Example 2
실시예 1에서 나일론 6만을 사용하여 펠렛화하고, 사출하는 것을 제외하고 동일하게 진행하여 나일론 소재를 제조하였다. Except for pelletizing using only nylon 6 in Example 1, and proceeding in the same manner except the injection to prepare a nylon material.
물성측정시험Physical property test
상기 실시예 1 ~ 2 및 비교예 1 ~ 2 에서 제조한 복합재 및 소재의 기계적 물성을 측정하기 위하여, 각 측정법에서 제시하는 방법으로 물성을 측정하여 그 결과를 표1에 나타내었다. 여기서 인장물성 측정시편은 덤벨형 모양의 시편이며, 충격강도 시편은 시편에 노치(notch)가 형성된 시편의 모양을 사용한다.
In order to measure the mechanical properties of the composite materials and materials prepared in Examples 1 and 2 and Comparative Examples 1 and 2, the physical properties were measured by the methods presented in the respective measurement methods, and the results are shown in Table 1. The tensile property measurement specimen is a dumbbell-shaped specimen, and the impact strength specimen is a specimen having a notch formed in the specimen.
1) 굴곡탄성율 측정방법1) How to measure flexural modulus
ASTM D 790에 의거하여 측정용 시편(127 × 12.7 × 6.4 ㎜)을 만들어, 만능시험기(Instron 4467)를 사용(시험속도 : 10mm/분), 상온에서 굴곡탄성율을 측정하였다.
Test specimens (127 × 12.7 × 6.4 mm) were made in accordance with ASTM D 790, and the flexural modulus was measured at room temperature using a universal testing machine (Instron 4467) (test speed: 10 mm / min).
2) 내열성 측정방법2) Heat resistance measuring method
ASTM D 648에 의거하여 측정용 시편을 만들어 열변형 측정기(YASUDA, No.148-HD-PC)를 사용(하중 : 0.45 Mpa)하여 상온에서 내열성을 측정하였다.
Test specimens were prepared according to ASTM D 648, and heat resistance was measured at room temperature using a heat deflection measuring instrument (YASUDA, No.148-HD-PC) (load: 0.45 Mpa).
3) 흡수율 측정방법3) Absorption rate measurement method
25℃, 50%RH 조건의 챔버에 시편을 3주간 방치한 후, 질량의 변화(%)를 측정하였다.
After leaving the specimen for 3 weeks in a chamber at 25 ° C. and 50% RH, the change in mass (%) was measured.
4) 충격강도 측정방법4) How to measure impact strength
ASTM D 256에 의거하여 노치(notch)가 형성된 측정용 시편(63.5 × 12.7 × 6.4 ㎜)을 만들어 아이조드 충격기(YASUDA, No.258-PC-L)를 사용, 상온에서 충격강도값을 측정하였다.
According to ASTM D 256, notched (notch) measuring specimens (63.5 × 12.7 × 6.4 mm) were made, and the impact strength value was measured at room temperature using an Izod impact machine (YASUDA, No. 258-PC-L).
5) 내염성 측정방법 5) Flame resistance measuring method
25중량% 염화칼슘 수용액에 ASTM D 368 type 1에 의거한 인장시편을 500 시간동안 침지시킨 후, 침지 전후의 인장강도 유지율을 측정하였으며, 인장강도는 만능시험기(Instron 4467)를 사용(시험속도 : 50 mm/분)하여 측정하였다.
After dipping the tensile test piece according to ASTM D 368 type 1 in 25 wt% aqueous calcium chloride solution for 500 hours, the tensile strength retention was measured before and after immersion, and the tensile strength was measured using a universal testing machine (Instron 4467). mm / min).
6) 비중 측정방법6) Specific gravity measurement method
ASTM D 792에 의거하여 시편의 비중을 측정하였다.
Specific gravity of the specimen was measured according to ASTM D 792.
[MPa]Flexural modulus
[MPa]
[℃]Heat resistance (HDT)
[° C]
[%]Absorption rate
[%]
(23℃)
[J/m]Izod impact strength
(23 ℃)
[J / m]
(인장강도유지율)
[%]Calcium Chloride Resistance
Tensile Strength Retention Rate
[%]
상기 표 1에서 보는 바와 같이 본원발명의 복합재는 종래 사용되는 나일론 6 소재에 비하여 굴곡탄성율, 내흡수성, 내열성, 내충격성, 내염성 등이 크게 향상된 것을 확인할 수 있었다. As shown in Table 1, the composite of the present invention was confirmed that the flexural modulus, water absorption, heat resistance, impact resistance, flame resistance and the like significantly improved compared to the conventional nylon 6 material.
따라서 본원발명의 복합재는 종래 자동차용 엔진, 샤시, 외장 플라스틱 부품 소재로 사용되는 나일론 6를 대체할 수 있을 것으로 기대된다.
Therefore, the composite material of the present invention is expected to be able to replace the nylon 6 used as a conventional automotive engine, chassis, exterior plastic parts material.
Claims (6)
[화학식 1]
상기 화학식 1에서, n : m = 4 : 96 ~ 12 : 88 이다.
A polyketone / nylon 6 blend composition, characterized in that the polyketone represented by the formula (1) and nylon 6 are mixed in a weight ratio of 30:70 to 90:10.
[Formula 1]
In Chemical Formula 1, n: m = 4: 96∼12: 88.
The polyketone / nylon 6 blend composition of claim 1, wherein the polyketone and nylon 6 are mixed in a weight ratio of 50:50 to 80:20.
The polyketone / nylon 6 blend composition according to claim 1, wherein the polyketone and nylon 6 have a flow index according to the conditions of D ASTM 1238, respectively, in the range of 5 to 70 g / 10 minutes.
4. The polyketone / nylon 6 blend composition according to claim 3, wherein the difference between the polyketone and the flow index of nylon 6 is 30 g / 10 minutes or less.
[화학식 1]
상기 화학식 1에서, n : m = 4 : 96 ~ 12 : 88 이다.
Method for producing a polyketone / nylon 6 composite material comprising the step of mixing the polyketone represented by the formula (1) and nylon 6 in a weight ratio of 30: 70 ~ 90: 10, and extruding.
[Formula 1]
In Chemical Formula 1, n: m = 4: 96∼12: 88.
The method of claim 5, wherein the extrusion is carried out at a temperature of 220 ~ 260 ℃.
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