KR101330364B1 - The method for synthesis of carbon nanotube pellet for polymer composites - Google Patents
The method for synthesis of carbon nanotube pellet for polymer composites Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 57
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 57
- 239000008188 pellet Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229920000642 polymer Polymers 0.000 title abstract description 5
- 239000002131 composite material Substances 0.000 title abstract description 4
- 230000015572 biosynthetic process Effects 0.000 title description 5
- 238000003786 synthesis reaction Methods 0.000 title description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000008187 granular material Substances 0.000 claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000975 co-precipitation Methods 0.000 claims description 2
- 238000009841 combustion method Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- 150000001298 alcohols Chemical class 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- DALDUXIBIKGWTK-UHFFFAOYSA-N benzene;toluene Chemical compound C1=CC=CC=C1.CC1=CC=CC=C1 DALDUXIBIKGWTK-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005453 pelletization Methods 0.000 abstract description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910021392 nanocarbon Inorganic materials 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000012018 catalyst precursor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
-
- B01J35/51—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
본 발명은 고분자 복합체 제조를 위한 탄소나노튜브 펠렛 합성방법에 관한 것으로, 더욱 상세하게는 탄소나노튜브를 합성하기 위한 촉매 분말을 펠렛화 또는 알갱이 형상화 한 후, 이를 이용하여 탄소나노튜브를 합성하여, 펠렛 형태의 탄소나노튜브를 제조하는 방법에 관한 것이다. 이를 위하여 본 발명은 탄소나노튜브를 합성하기 위한 분말 형태로 형성된 촉매 분말을 용액과 혼합하여 반죽을 만드는 단계, 상기에 만들어진 촉매/용액 반죽을 펠렛타이져 또는 압출기를 이용하여 펠렛형태 또는 알갱이 형태로 제조 후 건조하여는 단계, 건조된 촉매 펠렛 또는 알갱이를 반응기에 넣고 합성하여 펠렛형태 또는 알갱이 상의 탄소나노튜브를 얻는 단계로 이루어진 것에 특징이 있다.The present invention relates to a method for synthesizing carbon nanotube pellets for preparing a polymer composite, and more particularly, after pelletizing or pelletizing catalyst powder for synthesizing carbon nanotubes, synthesizing carbon nanotubes using the same, The present invention relates to a method for producing carbon nanotubes in pellet form. To this end, the present invention is to prepare a dough by mixing the catalyst powder formed in powder form for synthesizing carbon nanotubes with a solution, the catalyst / solution dough prepared in the pellet form or pellet form using a pelletizer or an extruder After manufacturing, the drying step is characterized in that the dried catalyst pellets or granules are put in a reactor and synthesized to obtain carbon nanotubes in pellet form or granules.
Description
본 발명은 고분자 복합체에 사용되는 탄소나노튜브 펠렛 또는 알갱이 형태의 탄소나노튜브 집합체를 만드는 방법에 관한 것으로, 더욱 상세하게는 탄소나노튜브 합성용 촉매를 펠렛 형태 또는 알갱이 형태로 제작하고, 이를 반응기를 통하여 탄소나노튜브를 합성을 통하여, 탄소나노튜브 분말이 아닌 펠렛 및 알갱이 형태로 탄소나노튜브 집합체를 제조하여, 고분자 복합체에 쉽게 혼합할 수 있는 펠렛 또는 알갱이 형태의 탄소나노튜브 집합체의 합성 방법에 관한 것이다.The present invention relates to a method for producing carbon nanotube pellets or granules of carbon nanotube aggregates used in a polymer composite, and more particularly, to prepare a catalyst for synthesizing carbon nanotubes in pellet form or granule form. Through the synthesis of carbon nanotubes through the production of carbon nanotube aggregates in the form of pellets and granules, not carbon nanotube powder, and a method for the synthesis of carbon nanotube aggregates in pellet or granule form that can be easily mixed into a polymer composite will be.
일반적으로 탄소나노튜브는 기존의 소재들과 비교하여보면 매우 우수한 전기적, 기계적, 화학적 특성을 가지고 있어, 전자, 전기제품, 고기능 복합체 등에 많은 연구가 이루어져 일부는 상용화되어지고 있다. 그러나 많은 연구와 개발이 실행되고 있으나 낮은 밀도 및 수십 마이크로의 분말 형태로 인한 처리과정에서의 흩날림으로 인한 인체에 대한 유해성 및 전기 제품의 오작동을 발생할 수 있으며, 또한 혼합하고자 하는 펠렛 및 분말 형태의 고분자와의 큰 겉보기 밀도 차이로 인한 분산의 어려움이 있는 실정이다. 특히 공정상 탄소나노튜브의 흩날리는 것을 방지하기 위해 수처리, 계면활성제처리로 보완하고 있으나, 처리과정에서 발생하는 탄소나노튜브 용액의 필터링 건조 등의 추가적인 비용이 발생하는 뿐만 아니라,원래의 합성된 탄소나노튜브에 비해 3차원 고밀도화에 의한 재분산성이 현격하게 떨어지고 있는 실정이다. 예컨데, 한국등록특허 10-1084977인 ‘나노카본액 조성물, 나노카본 수지 조성물, 나노카본 고형체, 나노카본 수지체 및 이들의 제조방법’에서는 탄소나노튜브를 액상에 분산, 건조 후, 수지 및 금속을 넣어 펠렛을 제조하는 방법이 기재되어 있으며, 한국공개특허 제10-2006-0006002호에는 계면활성제와 수성라텍스(수용성전구체)를 처리하여 분산을 하는 방법등이 기재되어 있다. 그러나 이러한 방법들은 탄소나노튜브를 분산, 또는 처리하기 위해 사용되는 용액이 탄소나노튜브 대비 10배에서 100배의 용액을 사용함에 따라, 탄소나노튜브의 필터 및 건조 등의 추가적인 비용이 발생함과 더불어, 사용된 용액을 후처리해야하는 등의 단점이 있다. In general, carbon nanotubes have very excellent electrical, mechanical, and chemical properties compared to conventional materials, and many studies have been made on electronics, electrical appliances, and high-performance complexes, and some of them are commercially available. However, many researches and developments have been carried out, but it may cause harm to the human body and malfunction of electrical products due to scattering during processing due to low density and dozens of microscopic powder forms, and also polymers in pellet and powder form to be mixed. There is a difficulty in dispersion due to the large apparent density difference with. In particular, in order to prevent the dispersion of carbon nanotubes in the process, it is supplemented with water treatment and surfactant treatment, but additional costs such as filtering and drying of carbon nanotube solutions generated during the treatment process are incurred. Compared to the nanotubes, the redispersibility due to the three-dimensional densification is significantly reduced. For example, in the 'nanocarbon liquid composition, nanocarbon resin composition, nanocarbon solid, nanocarbon resin, and preparation method thereof' of Korean Patent Registration No. 10-1084977, after dispersing and drying the carbon nanotube in a liquid phase, the resin and metal The method of preparing pellets is described, and Korean Laid-Open Patent Publication No. 10-2006-0006002 describes a method of dispersing by treating a surfactant and an aqueous latex (aqueous precursor). However, these methods have additional costs such as filter and drying of carbon nanotubes as the solution used to disperse or treat carbon nanotubes uses 10 to 100 times the solution of carbon nanotubes. , Disadvantages such as the need to post-treat the solution used.
본 발명은 상기한 문제점을 해결하기 위해 안출된 것으로 보관 및 취급이 용이하고, 제조가 간단한 펠렛 및 알갱이 형태의 탄소나노튜브 집합체의 제조 방법을 제공하는 데 있다.The present invention has been made to solve the above problems and to provide a method for producing a carbon nanotube aggregate in the form of pellets and granules is easy to store and handle, and easy to manufacture.
본 발명은 탄소나노튜브를 합성하기 위해 제조된 분말의 촉매를 펠렛 형태 또는 기존의 분말 촉매보다 큰 형태의 알갱이 상으로 제조하여, 탄소나노튜브 반응용 합성장치를 통하여, 원래의 알갱이 형태의 촉매 크기보다 커지거나 동등하며, 형태는 펠렛 또는 알갱이 형태의 탄소나노튜브 제조 방법을 제공한다. The present invention is to prepare a catalyst of the powder prepared for synthesizing carbon nanotubes in pellet form or granules of a larger form than the conventional powder catalyst, through the carbon nanotube reaction synthesis apparatus, the size of the original granule catalyst It is larger or equivalent, and provides a method for producing carbon nanotubes in pellet or granule form.
본 발명은 탄소나노튜브를 합성하기 위한 촉매를 펠렛 또는 알갱이로 제조 후, 탄소나노튜브를 제조함에 따라 합성된 탄소나노튜브의 형태가 펠렛 또는 알갱이 형태를 유지하면서 원래보다 큰 형태가 됨에 따라, 저밀도의 분말형태의 탄소나노튜브에 비해 흩날림이 적어, 취급하기가 쉽다. According to the present invention, after preparing a catalyst for synthesizing carbon nanotubes into pellets or granules, as the carbon nanotubes are manufactured in the form of carbon nanotubes, the density of the carbon nanotubes becomes larger than the original while maintaining the pellets or granules. It has less scattering than powdered carbon nanotubes, and is easy to handle.
도 1은 일반적인 방법에 의한 탄소나노튜브를 제조하는 순서를 나타낸 공정도 및 본 발명에 사용되는 탄소나노튜브 제조를 나타낸 공정도.
도 2는 실시예 1 및 2에 의해 합성된 촉매 및 탄소나노튜브 분말 사진.
도 3은 본 발명에 의한 실시예 3 및 4에 의해 합성된 촉매 및 탄소나노튜브 집합체 사진 1 is a process chart showing the procedure for producing carbon nanotubes by a general method and a process chart showing the carbon nanotubes used in the present invention.
Figure 2 is a catalyst and carbon nanotube powder pictures synthesized by Examples 1 and 2.
Figure 3 is a catalyst and carbon nanotube aggregate photos synthesized by Examples 3 and 4 according to the present invention
본 발명을 첨부된 도면을 참조하여 상세히 설명하면 다음과 같다.The present invention will now be described in detail with reference to the accompanying drawings.
도 1(a)는 일반적으로 담지체를 사용하여 탄소나노튜브를 합성할 경우에 사용되는 분말 형태의 촉매를 제조하는 공정을 나타낸 것으로, 촉매 전구체 및 담지체를 용액내에서 혼합 후, pH 등의 조절을 통한 담지체에 촉매가 달라붙게 하고, 이를 필터링 및 건조를 통한 용액 제거 후, 분쇄하여 탄소나노튜브를 합성한다. 촉매의 담지법은 여기에서 나와있는 담지법(Precipitation)외에도 공침법 및 연소법 등의 다양한 방법으로 탄소나노튜브용 촉매를 합성할 수 있다. 도1(b)는 펠렛형 및 흩날림이 적은 알갱이 상의 탄소나노튜브를 합성하기 위한 공정을 나타낸 것으로, 도1(a)에 의해 제조된 탄소나노튜브용 촉매를 용액과 혼합한 후, 필터링을 통한 압출이 가능한 상태로 만들기 위하여 용액을 일부 제거한 다음(용액의 양에 따라 필터를 통한 점도조절이 필요치 않을 수 있다) 압출기에 넣고, 펠럿형태 및 작은 알갱이 형태로 제작한다. 촉매 제조방법에 따라서는 1(a)에서 필터링 후 바로 펠렛화할 수 있다. 이 후, 건조를 한 다음 탄소나노튜브 반응기를 이용하여 탄소나노튜브를 합성하게 되면, 탄소나노튜브의 수율에 따라 얽힘 및 펠렛 형태 또는 수 mm 및 수 cm 크기의 탄소나노튜브 집합체를 얻게 된다. Figure 1 (a) generally shows a process for producing a catalyst in powder form used when synthesizing carbon nanotubes using a carrier, after mixing the catalyst precursor and the carrier in a solution, such as pH The catalyst adheres to the support through control, and after removal of the solution through filtering and drying, it is pulverized to synthesize carbon nanotubes. The catalyst supporting method can synthesize a catalyst for carbon nanotubes by various methods such as a coprecipitation method and a combustion method in addition to the support method described herein. Figure 1 (b) shows a process for synthesizing pellet-shaped and less scattered carbon nanotubes, the catalyst for carbon nanotubes prepared by Figure 1 (a) after mixing with the solution, through filtering Part of the solution is removed to make it extrudable (it may not be necessary to adjust the viscosity through the filter, depending on the amount of solution) and then placed in the extruder to form pellets and pellets. Depending on the catalyst preparation method, pelletization may be performed immediately after filtering in 1 (a). Thereafter, when the carbon nanotubes are synthesized using the carbon nanotube reactor after drying, the carbon nanotube aggregates are entangled and pellet-shaped or several mm and several cm in size according to the yield of the carbon nanotubes.
도 2는 실시예 1 및 실시예 2에 의해 합성한 탄소나노튜브 분말을 나타내고 있다. 분말 형태의 촉매를 사용하였고, 담지된 촉매량에 따라 실시예 1에서는 수율이 200%며, 실시예 2에서는 수율이 1000%이나, 수율과 상관없이 두가지 모두 분말형태의 탄소나노튜브로 합성되어져 있음을 알 수 있다. FIG. 2 shows carbon nanotube powders synthesized in Examples 1 and 2. FIG. The catalyst in powder form was used, and the yield was 200% in Example 1 and 1000% in Example 2, depending on the amount of catalyst supported. However, both were synthesized as carbon nanotubes in powder form regardless of the yield. Able to know.
도 3은 실시예 3 및 실시예 4에 의해 제조한 펠렛형태의 촉매를 가지고 합성한 탄소나노튜브 집합체 형태를 보이고 있다. 5mm 정도의 펠렛형태의 촉매를 사용한 경우, 수율이 200%인 탄소나노튜브 집합체는 원래의 촉매 펠렛의 크기와 유사한데 반해, 수율이 1000%인 경우는 탄소나노튜브 집합체가 커져, 지름이 10mm 정도 됨을 알 수 있다. 합성 도중 촉매 펠렛이 일부 분쇄됨에 따라 일부의 탄소나노튜브 집합체도 분말형태가 아닌 작은 형태의 탄소나노튜브 집합체로 형성되었다. Figure 3 shows the carbon nanotube aggregate form synthesized with the catalyst of the pellet form prepared in Examples 3 and 4. In the case of using a pellet catalyst of about 5 mm, the carbon nanotube aggregate having a yield of 200% is similar to the size of the original catalyst pellet, whereas the carbon nanotube aggregate is large when the yield is 1000% and the diameter is about 10 mm. It can be seen that. As the catalyst pellets were partially crushed during the synthesis, some of the carbon nanotube aggregates were also formed as small carbon nanotube aggregates rather than powders.
도 1(a)의 방법을 이용하여 촉매인 몰리브데늄 및 철을 담지체 마그네시아(MgO)의 중량 대비 각각 0.1 및 0.01이 되도록 제조한 분말 약 250g을 가정용 믹서로 분쇄한 후, 900도에서 메탄 분위기에서 회전식 열화학기상증착 장치를 이용하여 연속적으로 탄소나노튜브를 합성하였다. 합성된 탄소나노튜브 수율은 약 200% 정도였다. Using the method of FIG. 1 (a), about 250 g of a powder prepared such that molybdenum and iron as catalysts are 0.1 and 0.01, respectively, based on the weight of the carrier magnesia (MgO), is crushed with a domestic mixer, and then methane is used at 900 ° C. Carbon nanotubes were continuously synthesized using a rotary thermochemical vapor deposition apparatus in an atmosphere. The synthesized carbon nanotube yield was about 200%.
도 1(a)의 방법을 이용하여 촉매인 몰리브데늄 및 철을 담지체 마그네시아(MgO)의 중량 대비 각각 0.2 및 0.01이 되도록 제조한 분말 약 250g을 가정용 믹서로 분쇄한 후, 900도에서 메탄 분위기에서 회전식 열화학기상증착 장치를 이용하여 연속적으로 탄소나노튜브를 합성하였다. 합성된 탄소나노튜브 수율은 약 1000% 정도였다.Using the method of FIG. 1 (a), about 250 g of a powder prepared so that the catalysts of molybdenum and iron are 0.2 and 0.01 with respect to the weight of the carrier magnesia (MgO), respectively, was pulverized with a domestic mixer, and then methane at 900 degrees. Carbon nanotubes were continuously synthesized using a rotary thermochemical vapor deposition apparatus in an atmosphere. The synthesized carbon nanotube yield was about 1000%.
실시예 1에서와 같은 방법으로 제조한 촉매 분말250g에 에탄올용액 500g을 첨가하여 고점도의 반죽을 제조하였고, 이 반죽을 노즐의 직경이 4mm인 압출기를 통하여 펠렛 형태로 제조하였다. 약 100도에서 4시간 건조 후, 제조된 펠렛을 900도에서 메탄 분위기에서 회전식 열화학기상증착 장치를 이용하여 연속적으로 탄소나노튜브를 합성하였다. 250 g of catalyst powder prepared in the same manner as in Example 1 was added to 500 g of ethanol solution to prepare a high viscosity dough, and the dough was prepared in pellet form through an extruder having a diameter of 4 mm. After 4 hours of drying at about 100 degrees, the prepared pellets were continuously synthesized using a rotary thermochemical vapor deposition apparatus in a methane atmosphere at 900 degrees.
실시예 2에서와 같은 방법으로 제조한 촉매 분말250g에 에탄올용액 500g을 첨가하여 고점도의 반죽을 제조하였고, 이 반죽을 노즐의 직경이 4mm인 압출기를 통하여 펠렛 형태로 제조하였다. 약 100도에서 4시간 건조 후, 제조된 펠렛을 900도에서 메탄 분위기에서 회전식 열화학기상증착 장치를 이용하여 연속적으로 탄소나노튜브를 합성하였다.
250 g of catalyst powder prepared in the same manner as in Example 2 was added to 500 g of ethanol solution to prepare a high viscosity dough, and the dough was prepared in pellet form through an extruder having a diameter of 4 mm. After 4 hours of drying at about 100 degrees, the prepared pellets were continuously synthesized using a rotary thermochemical vapor deposition apparatus in a methane atmosphere at 900 degrees.
Claims (2)
Mixing the catalyst powder formed in powder form for synthesizing carbon nanotubes with a solution to make a dough, and preparing the catalyst / solution dough prepared in the form of pellets or granules using a pelletizer or an extruder and drying them , Putting the dried pellets or pellets of the catalyst in the reactor and synthesized to obtain a carbon nanotube aggregate of pellets or granules.
In the claim 1, the solution refers to a solution such as an aqueous solution, alcohols such as methanol and ethanol, an organic solution such as benzene toluene, and the like, and the catalyst powder refers to a supporting method, a coprecipitation method, It refers to a catalyst powder produced by a method such as the combustion method, from which a method for obtaining a carbon nanotube aggregate in the form of pellets or granules.
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