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WO2018160042A1 - Catalyseur pour la production en masse de nanotubes de carbone à multiples parois - Google Patents

Catalyseur pour la production en masse de nanotubes de carbone à multiples parois Download PDF

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Publication number
WO2018160042A1
WO2018160042A1 PCT/KR2018/002549 KR2018002549W WO2018160042A1 WO 2018160042 A1 WO2018160042 A1 WO 2018160042A1 KR 2018002549 W KR2018002549 W KR 2018002549W WO 2018160042 A1 WO2018160042 A1 WO 2018160042A1
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WIPO (PCT)
Prior art keywords
catalyst
carbon nanotubes
walled carbon
bundle
apparent density
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2018/002549
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English (en)
Korean (ko)
Inventor
류상효
성현경
정충헌
김동환
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kumho Petrochemical Co Ltd
Original Assignee
Korea Kumho Petrochemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from KR1020180024482A external-priority patent/KR102085940B1/ko
Application filed by Korea Kumho Petrochemical Co Ltd filed Critical Korea Kumho Petrochemical Co Ltd
Priority to CN202310083990.9A priority Critical patent/CN115888729A/zh
Priority to JP2019548044A priority patent/JP6890187B2/ja
Priority to US16/490,765 priority patent/US11524277B2/en
Priority to CN201880025867.9A priority patent/CN110545914A/zh
Publication of WO2018160042A1 publication Critical patent/WO2018160042A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
    • 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
    • C01B32/162—Preparation characterised by catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2235/00—Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
    • B01J2235/30—Scanning electron microscopy; Transmission electron microscopy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties

Definitions

  • the present invention relates to a catalyst for mass production of multi-walled carbon nanotubes.
  • Carbon nanotube is a hexagonal honeycomb tubular structure in which one carbon atom is bonded to three other carbon atoms, and its electrical, thermal, and mechanical properties are superior to other materials to be applied to various industrial fields. have.
  • Such carbon nanotubes are generally arc-discharge, pyrolysis, laser vaporization, chemical vapor deposition, plasma chemical vapor deposition, and thermochemistry. It is prepared by various methods such as thermal chemical vapor deposition, chemical vapor condensation, and the like.
  • the production method of the catalyst is spray drying (spray dry) is made at a low temperature of 200 ⁇ 350 °C, in order to form a hole in the catalyst, it is essential to use a water-soluble polymer as a pore-forming agent, making the catalyst in a form suitable for synthesis
  • spray drying spray dry
  • a water-soluble polymer as a pore-forming agent
  • the present invention is to solve the above problems of the prior art, an object of the present invention is to provide a catalyst suitable for the production process of multi-walled carbon nanotubes using a fluidized bed reactor.
  • One aspect of the present invention includes a metal component according to the following formula,
  • It provides a catalyst for producing multi-walled carbon nanotubes having a hollow structure of 0.5 ⁇ 10 ⁇ m thickness.
  • Ma is at least two metals selected from Fe, Ni, Co, Mn, Cr, Mo, V, W, Sn and Cu
  • Mb is at least one metal selected from Mg, Al, Si and Zr
  • the apparent density of the catalyst may be 0.05 ⁇ 0.70 g / mL.
  • the thickness may be 1 ⁇ 8 ⁇ m.
  • the hollow ratio of the hollow structure may be more than 50% by volume.
  • Another aspect of the present invention provides a carbon nanotube assembly including a bundle of carbon nanotubes consisting of a plurality of multi-walled carbon nanotubes grown on the catalyst for preparing the multi-walled carbon nanotubes.
  • the average bundle diameter of the bundle-type carbon nanotubes may be 0.5 ⁇ 20 ⁇ m
  • the average bundle length (bundle length) may be 10 ⁇ 200 ⁇ m.
  • the Raman spectral intensity ratio (I G / I D ) of the multi-walled carbon nanotubes may be 0.7 ⁇ 1.5.
  • the average diameter of the multi-walled carbon nanotubes may be 5 ⁇ 50nm.
  • the apparent density of the multi-walled carbon nanotubes may be 0.01 ⁇ 0.07g / mL.
  • a catalyst having a hollow structure that is, a spherical or partially broken spherical sphere having a hollow structure, that is, a core-shell structure by spray pyrolysis of an aqueous catalyst solution in which all metal catalyst components are dissolved without using a separate carrier is used. It can be produced, by controlling the thickness of the shell, the hollow ratio, and the density of the catalyst constituting the hollow structure to a certain range to optimize the composition and structure of the catalyst in a fluidized bed reactor can produce a large amount of multi-walled carbon nanotubes.
  • FIG. 1 is an SEM image of a catalyst for preparing multi-walled carbon nanotubes according to an embodiment of the present invention.
  • FIG. 2 is an SEM image of a catalyst for preparing multi-walled carbon nanotubes according to a comparative example of the present invention.
  • One aspect of the present invention includes a metal component according to the following formula,
  • It provides a catalyst for producing multi-walled carbon nanotubes having a hollow structure of 0.5 ⁇ 10 ⁇ m thickness.
  • Ma is at least two metals selected from Fe, Ni, Co, Mn, Cr, Mo, V, W, Sn and Cu
  • Mb is at least one metal selected from Mg, Al, Si and Zr
  • the catalyst may be used in a gas phase synthesis method for synthesizing carbon nanotubes, wherein Ma is at least two metals selected from Fe, Ni, Co, Mn, Cr, Mo, V, W, Sn and Cu, and Mb is Since it is at least one metal selected from Mg, Al, Si and Zr, it may contain at least three or more metals, preferably three to five metal components.
  • the Ma is a catalyst component and an active component in the catalyst, and compared to the case of using a single metal component as the catalyst component and the active component, impurities in the carbon nanotube synthesis process by using a mixture of two or more metal components Purity can be improved by suppressing production.
  • catalyst component refers to a substance that substantially lowers the chemical reaction energy of the substance, i.e., the main catalyst
  • active component refers to a substance that aids in the action of the catalyst component, i.e., a promoter. it means.
  • the catalyst component and the active component have a uniform distribution within a certain range, the synthesis yield of carbon nanotubes may be improved.
  • the mole fractions x and y of Ma and Mb may satisfy a relationship of 2.0 ⁇ x ⁇ 7.5 and 2.5 ⁇ y ⁇ 8.0, respectively.
  • x is less than 2.0, the activity of the catalyst and the synthesis yield of carbon nanotubes may be lowered.
  • the x is greater than 7.5, the content of Mb, which is a support component, is relatively low, resulting in a decrease in the durability of the catalyst. There is a problem that is difficult to apply to the continuous fluidized bed chemical vapor deposition method for.
  • the catalyst may have a hollow structure having a thickness of 0.5 to 10 ⁇ m, preferably 1 to 8 ⁇ m, and the hollow ratio may be 50% by volume or more.
  • the apparent density of the catalyst may be 0.05 ⁇ 0.70 g / mL.
  • the term “hollow structure” refers to a three-dimensional structure with an empty interior, for example, a spherical or polyhedral structure with an empty interior, wherein the hollow structure is a closed structure in which the entire hollow is closed. ), Some of the hollows may be interpreted to include an open structure, or a combination thereof.
  • the catalyst since the catalyst has a hollow structure, the apparent density is lower than that of the conventional catalyst, so that the catalyst can be applied to a continuous fluidized bed chemical vapor deposition method, and carbon nanotubes can be grown outward from the outer surface of the hollow structure. In addition, it can also grow inward from the inner surface of the hollow structure can significantly improve the carbon nanotube synthesis yield.
  • Another aspect of the invention (a) dissolving the metal precursor in a solvent to prepare a precursor solution; And (b) forming a catalyst by spraying the precursor solution into the reactor while pyrolysis to form a catalyst.
  • Ma is at least two metals selected from Fe, Ni, Co, Mn, Cr, Mo, V, W, Sn and Cu
  • Mb is at least one metal selected from Mg, Al, Si and Zr
  • the metal precursor may be one selected from the group consisting of nitrates, sulfates, alkoxides, chlorides, acetates, carbonates, and mixtures of two or more thereof, but is not limited thereto.
  • the solvent may be a polar solvent, and water, methanol, ethanol, propanol, isopropanol, butanol, or a mixed solvent of two or more thereof may be used as the polar solvent, preferably, water, more Preferably, deionized water can be used.
  • the use of deionized water as a solvent can minimize impurities in the precursor solution, thereby improving the purity of the final catalyst prepared. Improving the purity of the catalyst may mean improved purity of the carbon nanotubes as a result.
  • the precursor solution may be pyrolyzed while spraying into the reactor to form a catalyst.
  • Step (b) may include: (i) spraying a precursor solution into the reactor by supplying air of 2 to 5 atmospheres as a carrier gas and introducing external air; And (ii) pyrolyzing the sprayed precursor solution at 600 to 1,200 ° C. to form a catalyst.
  • the precursor solution may be sprayed into the reactor and converted into finer droplets in order to control the particle size, apparent density, and the like of the catalyst.
  • the pressure can be adjusted in the range of 2 to 5 atm. If the spraying pressure is less than 2 atm, the particle size, apparent density, etc. of the catalyst may not be controlled within a predetermined range, thereby lowering the purity of the carbon nanotubes synthesized therethrough. On the other hand, when the spray pressure is more than 5 atm, the particle size of the droplets is excessively small, so that the catalysts obtained may aggregate with each other.
  • the droplet size can be more precisely controlled, and thus the particle size, apparent density, etc. of the catalyst can be precisely controlled.
  • droplets may be formed by spraying a gas simultaneously with spraying the precursor solution, or spray droplets may be formed by spraying a gas after spraying the precursor solution.
  • the method of preparing the catalyst further includes spraying the gas into the reactor before the step (ii). It may include.
  • gas air, nitrogen, argon or a mixed gas of two or more thereof may be used, and preferably air may be used.
  • electrostatic attraction may be added to the gas spray to improve the efficiency of the droplet formation.
  • the pressure of the spraying gas can be adjusted within the range of 2 to 5 atmospheres, and the effect of the case out of the above range is described above. It's like that.
  • the catalyst may be finally prepared by heating the droplets to evaporate the solvent and decomposing the precursor.
  • the temperature of the reactor may be 600 ⁇ 1,200 °C, preferably, 700 ⁇ 900 °C.
  • the temperature of the reactor is less than 600 °C, the dry state of the catalyst is poor and requires an additional process is disadvantageous in terms of economics, through which the purity or physical properties of the carbon nanotubes manufactured may be reduced.
  • the temperature of the reactor is more than 1,200 °C excessive cost to build equipment or equipment not only causes economic losses, but also the performance of the catalyst may be degraded due to the formation of solid solution or modification of the crystal structure.
  • Another aspect of the present invention provides a carbon nanotube assembly including a bundle of carbon nanotubes consisting of a plurality of multi-walled carbon nanotubes grown on the catalyst for preparing the multi-walled carbon nanotubes.
  • the bundle type carbon nanotubes may basically exist in a form in which a plurality of carbon nanotubes, preferably, a plurality of multi-walled carbon nanotubes are aggregated with each other.
  • Each carbon nanotube and the aggregate thereof may be straight, curved, or a mixture thereof.
  • An average bundle diameter of the bundled carbon nanotubes may be 0.5 to 20 ⁇ m, and an average bundle length may be 10 to 200 ⁇ m.
  • the Raman spectral intensity ratio (I G / I D ) of the multi-walled carbon nanotubes may be 0.7 to 1.5, the average diameter may be 5 to 50nm, the apparent density may be 0.01 ⁇ 0.07g / mL. .
  • the catalyst of Comparative Example 5 is the same in composition and composition as the catalyst of Example 5, but the catalyst is prepared by spray drying, and Example 5 is different from the method of preparing the catalyst. Specifically, in the case of Comparative Example 5 compared to the spray pyrolysis method of Example 5 to prepare a catalyst powder by spraying the precursor solution in the reactor at a temperature of 200 °C relatively low, 700 °C, 1 hour in an air atmosphere heat treatment furnace The solid catalyst powder of the solid shape was prepared by heat treatment for a while.
  • the catalysts of Comparative Examples 6 and 7 were prepared by the co-precipitation method and the combustion method, respectively, and they each had a plate shape as shown in FIG.
  • the catalyst of Comparative Example 8 is a catalyst prepared using alumina (Al 2 O 3 ) powder which is not dissolved in water as a precursor of Al in the catalyst component.
  • 1 and 2 are SEM images of a catalyst for preparing multi-walled carbon nanotubes according to Examples and Comparative Examples, respectively.
  • all the catalyst powder of Example 1 has a spherical or partially broken sphere of a core-shell structure, in particular, in the case of a partially broken sphere, at least 50% of the surface of the hollow structure It can be seen that the shell is made of a flake formed of a metal component in the region.
  • Carbon nanotubes were synthesized using catalyst powders according to Examples and Comparative Examples. Specifically, each catalyst powder was introduced into a fluidized bed chemical vapor deposition reactor having a diameter of 350 mm, and maintained at 700-800 ° C. in a nitrogen atmosphere. Thereafter, a mixture of nitrogen and ethylene was supplied at a rate of 150 L per minute for 40 minutes to synthesize carbon nanotubes grown on the respective catalyst powders.
  • the apparent density of the catalyst powder was obtained by measuring the weight by filling the catalyst powder in the mass cylinder, and dividing the measured weight by the volume of the mass cylinder.
  • the apparent density of the carbon nanotubes was measured in the same manner.
  • the synthesis yield of carbon nanotubes was calculated according to the formula "weight of synthesized carbon nanotubes (g)] / [weight of injected catalyst powder (g)] * 100". The measurement results are shown in Table 2 below.
  • the catalysts of Comparative Examples 4, 5, 6, and 8 are difficult to float in the fluidized bed chemical vapor deposition method of synthesizing carbon nanotubes while floating the catalyst powder with the reaction gas with an apparent density of 0.70 g / mL or more. there is a problem.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

Un mode de réalisation de la présente invention concerne un catalyseur pour la fabrication de nanotubes de carbone à multiples parois, le catalyseur comprenant des constituants métalliques selon l'équation Ma:Mb = x:y et ayant une structure creuse ayant une épaisseur de 0,5 à 10 µm. Dans l'équation ci-dessus, Ma représente au moins deux métaux choisis parmi Fe, Ni, Co, Mn, Cr, Mo, V, W, Sn et Cu; Mb représente au moins un métal choisi parmi Mg, Al, Si et Zr; x et y représentent chacun la proportion molaire de Ma et Mb; et x + y = 10, 2,0 ≤ x ≤ 7,5 et 2,5 ≤ y ≤ 8,0.
PCT/KR2018/002549 2017-03-03 2018-03-02 Catalyseur pour la production en masse de nanotubes de carbone à multiples parois Ceased WO2018160042A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN202310083990.9A CN115888729A (zh) 2017-03-03 2018-03-02 用于大量生产多壁碳纳米管的催化剂
JP2019548044A JP6890187B2 (ja) 2017-03-03 2018-03-02 多重壁カーボンナノチューブの大量生産のための触媒
US16/490,765 US11524277B2 (en) 2017-03-03 2018-03-02 Catalyst for mass production of multi-wall carbon nanotubes
CN201880025867.9A CN110545914A (zh) 2017-03-03 2018-03-02 用于大量生产多壁碳纳米管的催化剂

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR20170027853 2017-03-03
KR10-2017-0027853 2017-03-03
KR10-2018-0024482 2018-02-28
KR1020180024482A KR102085940B1 (ko) 2017-03-03 2018-02-28 다중벽 탄소나노튜브의 대량 생산을 위한 촉매

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4470667A4 (fr) * 2022-10-28 2025-07-23 Lg Chemical Ltd Catalyseur pour la production de nanotubes de carbone et procédé de production de ce catalyseur

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101007183B1 (ko) * 2008-10-23 2011-01-12 제일모직주식회사 탄소나노튜브 합성용 담지촉매, 그 제조방법 및 이를 이용한 탄소나노튜브
KR101241034B1 (ko) * 2010-08-10 2013-03-11 금호석유화학 주식회사 분무 열분해 방법을 이용한 고수율 탄소나노튜브 합성용 촉매조성물의 제조 방법
KR20130094364A (ko) * 2012-02-13 2013-08-26 금호석유화학 주식회사 초저밀도 특성을 지닌 번들 구조의 고전도성 탄소나노튜브 및 이의 제조방법
KR101303061B1 (ko) * 2012-09-25 2013-09-03 금호석유화학 주식회사 다중벽 탄소나노튜브 제조용 촉매조성물
KR101508101B1 (ko) * 2013-09-30 2015-04-07 주식회사 엘지화학 높은 비표면적을 갖는 탄소나노튜브 및 그 제조 방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101007183B1 (ko) * 2008-10-23 2011-01-12 제일모직주식회사 탄소나노튜브 합성용 담지촉매, 그 제조방법 및 이를 이용한 탄소나노튜브
KR101241034B1 (ko) * 2010-08-10 2013-03-11 금호석유화학 주식회사 분무 열분해 방법을 이용한 고수율 탄소나노튜브 합성용 촉매조성물의 제조 방법
KR20130094364A (ko) * 2012-02-13 2013-08-26 금호석유화학 주식회사 초저밀도 특성을 지닌 번들 구조의 고전도성 탄소나노튜브 및 이의 제조방법
KR101303061B1 (ko) * 2012-09-25 2013-09-03 금호석유화학 주식회사 다중벽 탄소나노튜브 제조용 촉매조성물
KR101508101B1 (ko) * 2013-09-30 2015-04-07 주식회사 엘지화학 높은 비표면적을 갖는 탄소나노튜브 및 그 제조 방법

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4470667A4 (fr) * 2022-10-28 2025-07-23 Lg Chemical Ltd Catalyseur pour la production de nanotubes de carbone et procédé de production de ce catalyseur

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