KR101364811B1 - Cutting method of carbon nanotubes - Google Patents
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- KR101364811B1 KR101364811B1 KR1020120098565A KR20120098565A KR101364811B1 KR 101364811 B1 KR101364811 B1 KR 101364811B1 KR 1020120098565 A KR1020120098565 A KR 1020120098565A KR 20120098565 A KR20120098565 A KR 20120098565A KR 101364811 B1 KR101364811 B1 KR 101364811B1
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- C01B32/00—Carbon; Compounds thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
Description
본 발명은 진동의 완충이나 전달 방지를 위하여 사용하는 고무 제품인 방진용 고무의 기계적 특성을 향상시킬 수 있을 뿐만 아니라 화학적, 열적, 전기적 특성을 향상시킬 수 있도록 한 탄소나노튜브의 절단방법에 관한 것이다.The present invention relates to a method for cutting carbon nanotubes that can improve the mechanical, thermal, and electrical properties as well as the mechanical properties of the anti-vibration rubber, which is a rubber product used for the buffering or transmission of vibration.
일반적으로, 방진용 고무는 진동의 완충이나 전달 방지를 위하여 사용하는 고무 제품으로 여러 산업분야에서 광범위하게 사용이 되고 있고 특히 자동차의 엔진을 지지하기 위한 마운트가 방진용 고무로 제조가 된다.
상기 방진용 고무는 인장강도나 내구성 등을 향상시키는 강화제로 카본블랙이나 실리콘 (silane compound)을 이용하여 합성하고 있다.
이와 관련하여, 한국공개특허공보 제2010-0071699호에 공개된 종래 고에너지로 기능화된 탄소나노튜브를 함유한 타이어 트레드고무 조성물은 타이어 트레드 원료고무에 보강제로 고에너지로 기능화된 탄소나노튜브와 카본블랙을 함께 첨가하고, 탄소나노튜브의 분산성 향상을 위해 실랑 커플링제를 포함하여 기존의 트레드 고무조성물보다 내마모성 및 발열성이 향상된 타이어 트레드 고무조성물을 기재하고 있다.In general, anti-vibration rubber is a rubber product used to prevent vibration or transmission of vibrations, and is widely used in various industrial fields. In particular, a mount for supporting an engine of an automobile is made of anti-vibration rubber.
The anti-vibration rubber is synthesized using carbon black or silicon (silane compound) as a reinforcing agent to improve tensile strength and durability.
In this regard, tire tread rubber compositions containing carbon nanotubes functionalized with conventional high energy published in Korean Patent Publication No. 2010-0071699 are carbon nanotubes and carbon functionalized with high energy as a reinforcing agent to tire tread raw rubber. It is described a tire tread rubber composition that is added to the black together, including a silane coupling agent to improve the dispersibility of the carbon nanotubes, wear resistance and heat generation improved than the conventional tread rubber composition.
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여기서, 카본블랙과 기본적인 구조에서 동소체인 탄소나노튜브의 강도는 카본블랙과 비교가 되지 않을 뿐만 아니라 무게가 가볍고 동일한 무게일 때 강철이 지니는 인장강도의 100배에 달하는 것으로 알려져 있고, 고탄성, 고전도성 등 매우 우수한 물성을 지니고 있다.Here, the strength of allocarbon carbon nanotubes in carbon black and basic structure is not only compared with carbon black, but also known to reach 100 times the tensile strength of steel at light weight and the same weight. It has very good physical properties.
상기한 탄소나노튜브(Carbon Nano Tube: CNT)는 하나의 탄소 원자에 이웃하는 세 개의 탄소 원자가 결합되어 있으며, 이러한 탄소 원자간의 결합에 의해서 육각 환형이 이루어지고, 이들이 벌집형태로 반복된 평면이 말려 원통형 튜브를 이룬 물질로서, 다양한 분야에서 탄소나노튜브를 사용하여 제품의 특성을 향상시키기 위해 노력하고 있다.The carbon nanotube (CNT) has three carbon atoms adjacent to one carbon atom bonded thereto, and hexagonal rings are formed by the bonds between the carbon atoms. As a material consisting of a cylindrical tube, carbon nanotubes are used in various fields to improve product characteristics.
그러나, 상기한 바와 같이 탄소나노튜브는 기계적, 열적, 전기적, 화학적 특성이 매우 우수한 물질이지만 머리카락처럼 엉켜있는 형태를 띄고 있기 때문에, 이를 원료고무에 혼합하여 제조하게 되면 한쪽으로 뭉치게 되고 이로 인해 방진용 고무의 기계적 특성(특히 인장강도)을 저하시키게 되는 문제점이 있다.However, as described above, carbon nanotubes are very excellent in mechanical, thermal, electrical, and chemical properties, but because they are tangled like hairs, when they are manufactured by mixing them with raw rubber, they are bound to one side. There is a problem of lowering the mechanical properties (particularly tensile strength) of the rubber.
본 발명의 목적은 상기한 문제점을 해결하기 위한 것으로서, 탄소나노튜브를 원료고무에 혼합하여 제조할 때 잘게 절단하여 혼합하도록 함으로써, 탄소나노튜브가 원료고무와 혼합될 때 균일하게 분산되도록 하여 방진용 고무의 기계적, 열적, 전기적, 화학적 특성 특히, 인장강도를 향상시킬 수 있도록 한 탄소나노튜브의 절단방법을 제공함에 있다.An object of the present invention is to solve the above problems, by mixing the carbon nanotubes in the raw material rubber to be finely cut and mixed, so that the carbon nanotubes are uniformly dispersed when mixed with the raw material rubber for dust The present invention provides a method for cutting carbon nanotubes to improve mechanical, thermal, electrical and chemical properties of rubber, in particular tensile strength.
상기한 목적을 실현하기 위하여 본 발명은 탄소나노튜브를 절단하는 방법으로 탄소나노튜브(MWCNT) 0.5g에 질산 150㎖를 혼합하여 리플럭스(reflux 역류) 하면서 혼합물을 만드는 단계와, 상기한 혼합물을 PTFE멤브레인을 이용하여 필터링을 하는 단계와, 상기한 필터링 단계중 묽은 수산화나트륨(NaOH) 용액과 증류수를 섞으면서 혼합물을 중화시키며 pH7로 맞추는 단계와, 상기한 필터링된 혼합물을 80℃에서 1시간 정도 건조시키는 단계로 구성함을 특징으로 한다.In order to achieve the above object, the present invention comprises the steps of making a mixture while refluxing by mixing 150 ml of nitric acid to 0.5 g of carbon nanotubes (MWCNT) in a method of cutting carbon nanotubes; Filtering by using PTFE membrane, neutralizing the mixture by mixing dilute water with dilute water solution of sodium hydroxide (NaOH) in the filtering step, and adjusting the filtered mixture at 80 ° C. for about 1 hour. Characterized in that it comprises a step of drying.
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이상과 같이 본 발명은 방진용 고무를 제조할 때 카본 블랙과 함께 탄소나노튜브를 균일하게 혼합함으로써, 방진용 고무의 기계적 특성인 인장강도를 대폭 향상시킬 수 있는 잇점이 있는 것이다.As described above, the present invention has the advantage of greatly improving the tensile strength, which is a mechanical property of the rubber for dustproofing, by uniformly mixing carbon nanotubes with carbon black when manufacturing the rubber for dustproofing.
도 1은 본 발명에 따른 탄소나노튜브가 함유된 방진용 고무조성물을 제조하는 단계를 설명하는 순서도,
도 2는 탄소나노튜브를 절단하는 방법을 도시한 순서도.1 is a flow chart illustrating the steps of preparing a dustproof rubber composition containing carbon nanotubes according to the present invention;
2 is a flowchart illustrating a method of cutting carbon nanotubes.
도 1은 본 발명에 따른 탄소나노튜브가 함유된 방진용 고무조성물의 제조 방법을 도시한 순서도이고, 도 2는 본 발명에서 탄소나노튜브를 절단하기 위하여 산처리를 하는 순서를 도시한 순서도이다.1 is a flowchart illustrating a method of manufacturing a dustproof rubber composition containing carbon nanotubes according to the present invention, and FIG. 2 is a flowchart illustrating an acid treatment to cut carbon nanotubes in the present invention.
본 발명에 따른 방진용 고무조성물은 하기한 실시예에 기재된 바와 같은 조성비율을 갖게 되는 바, 원료고무 100에 대한 Phr(parts per hundred resin) 비율로 기재되어 있다.The anti-dust rubber composition according to the present invention has a composition ratio as described in the following examples, and is described in terms of parts per hundred resin (Phr) relative to the raw material rubber 100.
(실시예)(Example)
상기한 원료고무(SIR10)와 카본블랙, 산화아연(ZnO), 스테아릭산(Stearic acid)은 통상의 방진용 고무조성물을 제조할 때 많이 사용하는 원료들이고, 카본 블랙 N774 (SRF) (입자 크기 : 60~100㎚)은 방진용 고무의 우수한 동특성을 위해 첨가하는 것이다.The above raw material rubber (SIR10), carbon black, zinc oxide (ZnO), stearic acid (Stearic acid) are the raw materials used in the production of rubber composition for dustproof dust, carbon black N774 (SRF) (particle size: 60-100 nm) is added for excellent dynamic characteristics of the rubber for dustproof.
또한, 카본블랙 N990 (MT) (입자 크기 : 200~500㎚)은 충진제로서의 역할을 수행 하는 것이며, 노화방지제로서는 (RD)가 사용되고, 고무 표면의 크랙(CRACK)을 보호하기 위해 왁스(Sunprax-682s)가 사용되며, 내산화제로서는 (Kumanox-13)이 사용되고, 백카본은 (Z 155) 그리고 고무 촉진제는 (TBBS)이며, 유기가황제는 (TBTD-190)이 사용되고 있다.In addition, carbon black N990 (MT) (particle size: 200-500 nm) serves as a filler, (RD) is used as an anti-aging agent, and wax (Sunprax-) to protect the cracks on the rubber surface. 682s) is used, (Kumanox-13) is used as an oxidation resistant agent, (Z 155) is a back carbon, (TBBS) is a rubber accelerator, and (TBTD-190) is used for an organic vulcanizing agent.
상기한 내산화제는 내산화성, 내굴곡성, 내오존균열, 동파방지에 탁월한 효과가 있고 분해성이 좋아 가공성이 양호하다.The oxidizing agent is excellent in oxidation resistance, flex resistance, ozone crack, freeze prevention and good degradability and good workability.
여기에서 방진용 고무의 우수한 동특성을 위해 사용되는 카본 블랙 N774 (SRF)의 입자크기는 평균 약60㎚의 입자크기를 사용하고, 충진제로 사용되는 카본블랙 N990 (MT)의 입자크기는 평균 약250㎚의 입자크기를 사용하는 것이 바람직하다.The particle size of carbon black N774 (SRF) used here for the excellent dynamic properties of the rubber for dustproof is used, the average particle size of about 60nm, the average particle size of carbon black N990 (MT) used as a filler is about 250 Preference is given to using particle sizes of nm.
특히, 상기한 탄소나노튜브로는 멀티월탄소나노튜브(MWCNT)가 사용되고 있는 바, 상기한 탄소나노튜브는 긴 머리카락 형태를 띄지만 본원에서는 이를 산처리하여 짧게 절단한 것을 사용하는 것으로서 방진용 고무조성물의 혼합 시 균일하게 분산되도록 한다.In particular, the carbon nanotubes are multi-walled carbon nanotubes (MWCNT) is used, the carbon nanotubes have a long hair form, but in the present application is used to cut short by acid treatment of the rubber for dustproof Ensure uniform dispersion upon mixing of the composition.
상기한 바와 같은 방진용 고무조성물을 제조하기 위해서는 통상적인 방진용 고무조성물 제조방법을 따르고 있는 바, 이는 도 1에 도시된 바와 같이 원료고무, 약품, 카본블랙 및 탄소나노튜브를 혼합한 후 일정 시간동안 교반하여 CMB(Carbon Master Batch)를 제조하게 된다.In order to manufacture the anti-vibration rubber composition as described above, the conventional anti-vibration rubber composition manufacturing method is followed, which is a predetermined time after mixing the raw material rubber, chemicals, carbon black and carbon nanotubes as shown in FIG. While stirring to prepare a carbon master batch (CMB).
특히, 니더(kneader)와 같은 설비에서 교반을 하면 더 우수한 결과물을 얻을 수 있다.In particular, agitation in equipment such as kneader can provide better results.
한편, 상기 탄소나노튜브는 30-125㎚의 길이로 절단되어 혼합하는 것이 바람직하다.On the other hand, the carbon nanotubes are preferably cut to a length of 30-125nm and mixed.
여기서, CMB는 원료고무와 충진제인 카본블랙, 탄소나노튜브, 연화제 등의 배합약품을 넣고 촉진제는 넣지 않은 상태에서 믹싱한 것을 나타낸다.Here, CMB refers to a mixture of a raw material rubber and a compounding agent such as carbon black, carbon nanotube, and softener, which are fillers, and mixed without the accelerator.
CMB를 제조한 후에는 냉각 건조 공정을 거친 후 일정 시간동안의 숙성과정을 거쳐서 다시 2차 CMB를 제조하게 된다.After the CMB is manufactured, the second CMB is manufactured again through a aging process for a predetermined time after undergoing a cooling drying process.
상기한 2차 CMB에 고무촉진제와 가류제를 투입하여 원하는 물성을 갖는 방진용 고무조성물인 FMB(Final Master Batch)를 만들게 되는 바, 상기한 바와 같이 제조된 방진용 고무조성물은 탄소나노튜브가 균일하게 혼합되어 있기 때문에, 기계적인 성능 특히 인장강도가 매우 향상된다.The rubber accelerator and the vulcanizing agent are added to the secondary CMB to make a FMB (Final Master Batch), which is a dustproof rubber composition having desired properties. The dustproof rubber composition prepared as described above has uniform carbon nanotubes. Mechanically, in particular, tensile strength is greatly improved.
즉, 탄소나노튜브 자체의 강도가 매우 우수하기 때문에 이를 잘게 절단하여 방진용 고무조성물에 혼합하게 되면 방진용 고무조성물의 인장강도가 대폭 향상될 수 있는 것이다.That is, since the strength of the carbon nanotube itself is very excellent, when the finely cut and mixed in the anti-vibration rubber composition, the tensile strength of the anti-vibration rubber composition can be significantly improved.
여기서, FMB(Final Master Batch)는 CMB에 황과 같은 가류제 및 촉진제 등의 각종 배합약품 등을 투입하여 믹싱한 상태를 나타내는 것으로 고무로서의 공정을 완료하여 바로 가공이 가능한 고무를 나타낸다.Here, FMB (Final Master Batch) refers to a state in which a variety of compounding agents such as vulcanizing agents such as sulfur and accelerators are added to CMB and mixed, and refers to rubber that can be processed immediately after completing the process as rubber.
도 2는 상기한 탄소나노튜브를 잘게 절단하는 산처리 공정을 도시한 것으로서, 먼저 탄소나노튜브(MWCNT) 분말 0.5g과 질산(HNo3)150㎖의 용액을 약 160℃에서 리플럭스(reflux 역류) 하면서 18시간동안 혼합하여 혼합물을 만들게 된다.FIG. 2 illustrates an acid treatment process of finely cutting the carbon nanotubes. First, a solution of 0.5 g of carbon nanotube (MWCNT) powder and 150 ml of nitric acid (HNo 3 ) is refluxed at about 160 ° C. (reflux backflow). The mixture is made for 18 hours.
이 상태에서 PTFE(Poly tetrafluoroethylene)멤브레인을 이용하여 필터링을 하게 되는 바, 이때 상기한 혼합물은 산성을 띄게 되기 때문에 이를 중화시키기 위해 필터링 과정에 묽은 수산화나트륨(NaOH) 용액과 증류수를 섞으면서 필터링을 하고, 혼합물을 pH7로 맞추게 된다.In this state, filtering is performed using PTFE (Poly tetrafluoroethylene) membrane. In this case, the above mixture is acidic, and the mixture is filtered by diluting with dilute water and dilute water solution in order to neutralize it. The mixture is brought to pH 7.
상기한 바와 같이 필터링된 혼합물은 80℃에서 1시간 정도 건조시키게 되는 바, 상기한 바와 같이 처리된 탄소나노튜브에는 카르복실기가 형성된다.As described above, the filtered mixture is dried at 80 ° C. for about 1 hour, and thus, a carboxyl group is formed on the carbon nanotubes treated as described above.
즉, 상기한 탄소나노튜브는 강산성인 질산에 의해 잘게 절단되게 되는 바, 이를 필터링하고 중화시키며 건조시켜서 본 발명의 방진용 고무조성물에 혼합 사용하게 되는 것이다.That is, the carbon nanotubes are finely cut by nitric acid, which is strongly acidic, and then mixed with the dustproof rubber composition of the present invention by filtering, neutralizing and drying them.
특히, 본원에서 사용되는 2종류의 카본블랙 입자크기를 보면, 카본 블랙 N774 (SRF)의 입자크기는 약60㎚이고, 카본블랙 N990 (MT)의 입자크기는 약250㎚로 상이하기 때문에 2종류의 카본블랙(SRF, MT)이 혼합되면 필연적으로 입자간의 공극이 발생되는 바, 이를 메우기 위한 최적의 크기는 30-125㎚가 된다.In particular, when looking at the two types of carbon black particles used herein, the particle size of carbon black N774 (SRF) is about 60 nm, and the particle size of carbon black N990 (MT) is about 250 nm. When carbon black (SRF, MT) is mixed, inevitably voids are generated between the particles, and the optimum size for filling them is 30-125 nm.
따라서, 상기한 절단된 탄소나노튜브의 입자크기를 30-125㎚로 절단 형성하게 되면, 입자간의 공극을 메울 수 있게 됨으로써 기계적 특성을 보다 향상시킬 수 있게 된다.Therefore, when the particle size of the cut carbon nanotubes is cut to 30-125 nm, the gaps between the particles can be filled to improve mechanical properties.
Claims (5)
상기한 혼합물을 PTFE멤브레인을 이용하여 필터링을 하는 단계와,
상기한 필터링 단계중 묽은 수산화나트륨(NaOH) 용액과 증류수를 섞으면서 혼합물을 중화시키며 pH7로 맞추는 단계와,
상기한 필터링된 혼합물을 80℃에서 1시간 정도 건조시키는 단계로 구성함을 특징으로 하는 탄소나노튜브의 절단 방법.Mixing 150 ml of nitric acid (HNo 3 ) with 0.5 g of carbon nanotubes (MWCNT) to form a mixture while refluxing (reflux backflow);
Filtering the mixture using a PTFE membrane;
Neutralizing the mixture while mixing the diluted sodium hydroxide (NaOH) solution and distilled water and adjusting the pH to 7;
Method for cutting carbon nanotubes, characterized in that for drying the filtered mixture for 1 hour at 80 ℃.
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