WO2015105302A1 - Catalyseur pour la synthèse de nanotubes de carbone à parois multiples, procédé de production dudit catalyseur, et nanotubes de carbone à parois multiples synthétisés par ledit catalyseur - Google Patents

Catalyseur pour la synthèse de nanotubes de carbone à parois multiples, procédé de production dudit catalyseur, et nanotubes de carbone à parois multiples synthétisés par ledit catalyseur Download PDF

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Publication number
WO2015105302A1
WO2015105302A1 PCT/KR2015/000053 KR2015000053W WO2015105302A1 WO 2015105302 A1 WO2015105302 A1 WO 2015105302A1 KR 2015000053 W KR2015000053 W KR 2015000053W WO 2015105302 A1 WO2015105302 A1 WO 2015105302A1
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Prior art keywords
catalyst
carbon nanotubes
carbon nanotube
walled carbon
walled
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PCT/KR2015/000053
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English (en)
Korean (ko)
Inventor
강득주
김주희
김주식
Original Assignee
주식회사 제이오
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Priority claimed from KR1020140174427A external-priority patent/KR101756453B1/ko
Application filed by 주식회사 제이오 filed Critical 주식회사 제이오
Priority to JP2016543626A priority Critical patent/JP7179441B2/ja
Priority to US15/110,737 priority patent/US9975774B2/en
Priority to CN201580003474.4A priority patent/CN105873679B/zh
Publication of WO2015105302A1 publication Critical patent/WO2015105302A1/fr

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    • B01J35/617—
    • 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
    • B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8898—Manganese, technetium or rhenium containing also molybdenum
    • B01J35/30—
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/06—Multi-walled nanotubes

Definitions

  • the present invention relates to a catalyst for synthesizing multi-walled carbon nanotubes. More specifically, the multi-walled carbon nanotubes can easily disperse the synthesized multi-walled carbon nanotubes and can significantly improve conductivity.
  • a catalyst for synthesis, a method for producing the catalyst, and a multi-walled carbon nanotube synthesized with the catalyst are examples of the multi-walled carbon nanotubes.
  • Carbon nanotubes are carbon allotropees that form a cylindrical tube structure by combining carbons in hexagons, and are called nanotubes because they have a small shape of ribs of several nm in diameter. These carbon nanotubes are hollow because they are light and are attracting attention as new materials due to their tensile strength up to 100 times or more and up to 90 ° without damage to steel of the same thickness. In addition, it has high thermal conductivity and electrical conductivity, and exhibits the characteristics of the conductor and the semiconductor depending on the angle at which the carbon layer is wound.
  • the carbon nano-leave may be classified into a single walled carbon nanotube (SWNT) and a multi-walled carbon nanotube (MWNT) according to the number of walls.
  • SWNT single walled carbon nanotube
  • MWNT multi-walled carbon nanotube
  • carbon nanotubes are electro-discharge, laser deposition, plasma
  • the present invention has been made to solve the problems of the prior art as described above, and a catalyst having a large specific surface area having a value of 30 or more divided by the volume of carbon nanotubes grown per catalyst lg by the volume of lg is prepared. , Using this to manufacture high quality multi-walled carbon nanotubes having a large specific surface area (preferably 3-10 ran in diameter and 3-10 in number of walls). And to provide a technology to enable mass production of low cost multi-walled carbon nanotubes greatly improved dispersibility.
  • the problem to be solved by the present application is not limited to the above-mentioned problem, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.
  • One aspect of the present application provides a multi-walled carbon nanotube having a volume of 30 or more divided by the volume of the catalyst lg divided by the volume of the multi-walled carbon nanotubes grown per catalyst lg represented by the following formula (1): V t / c- (W t x yt ) / (W c XY c ) (1)
  • W t is the weight of carbon nanotubes that can be listed as a unit catalyst (lg),
  • W c is lg as the unit catalyst weight, p t is the hanging density of carbon nanotubes, and p c is the hanging density of catalyst).
  • Another aspect of the present application provides a multi-walled carbon nano-leuver, characterized in that the surface area is 400 ⁇ 1000 m7g.
  • the surface area of the multi-walled carbon nanotubes is, for example,
  • niVg 400-1,000 preferably 500 1,000 niVg, more preferably 600 ⁇ 1,000 or m7g.
  • Another aspect of the present disclosure provides a composite containing multi-walled carbon nanoleubes.
  • the composite may include more than 0.5% by weight of the multi-walled carbon nanotubes, thereby having a conductivity, the matrix of the composite may be a polymer, a ceramic, a metal or a combination thereof.
  • an energy storage device including multi-walled carbon nanotubes.
  • Another aspect of the present application is composed of Fe, Co, Ca, Ni and Mo.
  • a plate-shaped catalyst for growing carbon nanotubes having a volume of carbon nanotubes divided by the volume of catalyst l g of 30 or more:
  • Wt is the weight of carbon nanotubes that can be grown as a unit catalyst (lg)
  • W c is lg as the weight of the unit catalyst
  • p t is the hanging density of carbon nanotubes
  • p e is the apparent density of the catalyst.
  • Another aspect of the present application provides a plate-shaped catalyst for growing carbon nanotubes having a specific surface area of 120 inVg or more.
  • Another aspect of the present application provides a carbon nanotube comprising a plate-shaped catalyst. In the case of the plate-shaped catalyst, the surface area is larger than that of the spherical or acicular catalyst,
  • Each surface of the plate-shaped catalyst of the present application is flat or has a curvature
  • the plate-shaped catalyst produced by the catalyst production method according to the present invention has a very low density. That is, since the surface area is very wide compared to the weight, synthesizing carbon nanotubes using such a catalyst, the dispersion energy is low, and the degree of damage in the dispersion process is very low to maintain high conductivity.
  • the multi-walled carbon nano-leave synthesized using the catalyst according to the production method of the present invention has a diameter comparable to that of a single-walled carbon nanotube (SWNT), and the number of walls is very homogeneous with 3 to 10. ', The specific surface area is large, indicating very high conductivity.
  • the carbon nanotubes grown by using the catalyst of the present invention have a purity of 98% or more, and thus, multi-walled carbon nanotubes can be synthesized by using the same amount of catalyst.
  • FIG. 1 is a scanning electron microscope (SEM) image of a catalyst prepared according to Example 1 of the present application.
  • Figure 2 of the multi-walled carbon nanotubes prepared according to Example 1 of the present application are a scanning electron microscope (SEM) image of a catalyst prepared according to Example 1 of the present application.
  • Figure 3 is a multi-walled carbon nanotubes prepared according to Example 2 of the present application.
  • FIG. 4 is a graph showing surface resistance according to the content of multi-walled carbon nanotubes (MWNT). 5 is a schematic view showing a method of preparing a catalyst for multiwall carbon nanotube synthesis.
  • a multi-wall having a value of 30 or more divided by the volume of the catalyst-g divided by the volume of the multi-walled carbon nanotubes grown per gram of the catalyst represented by the following formula (1)
  • V t / c (W t XY t ) / (W c xy c ) (1)
  • W t is the weight of carbon nanotubes that can be grown as a unit catalyst (lg)
  • W c is lg as the weight of the unit catalyst
  • p t is the hanging density of the carbon nanotubes
  • Pc is the hanging density of the catalyst
  • This surface area is a large surface area that has not been observed in multi-walled carbon nanotubes other than single-walled carbon nanotubes (SWNT).
  • This surface area is multi-walled by carbon nanotubes grown using the catalyst of the present invention. This is because the number is small and the diameter of the carbon nanotubes is small.
  • the multi-walled carbon nanotubes have a diameter of 3 to 10 nm, and the number of walls is 3 to 10, but is not limited thereto.
  • the diameter of the multi-walled nano-leeve is 3 to 10 ran, preferably 3 to 6 ran, more preferably 3-5 ran, and the number of walls of the multi-walled carbon nanotubes is 3-10, preferably 3-6, more preferably 3-5.
  • the multi-walled carbon nanotubes are characterized by having a purity of 98% or more, but is not limited thereto.
  • Another aspect of the present application provides a composite comprising multi-walled carbon nanotubes.
  • the composite may include more than 0.5% by weight of the multi-walled carbon nanotubes, thereby having a conductive all, the matrix of the composite may be a polymer, ceramic, metal, or these mixtures.
  • the plymer may be a thermoplastic polymer or a thermosetting polymer, but is not limited thereto.
  • Thermoplastic resins are plastic or deformable polymeric materials that can be dissolved in liquid and re-dissolved after curing.
  • the thermoplastic resin may be an acrylic resin, vinyl chloride resin, vinyl acetate resin, vinylacetyl resin,
  • Methyl methacryl resin, styrene resin, polypropylene resin, polyethylene resin, or polyamide resin (nylon) may be used, but is not limited thereto.
  • Thermosetting resins are polymeric materials that cure into a more powerful form upon application of energy, and once cured, cannot be heated or molded again.
  • the thermosetting resin may be a phenol resin, urea resin, melamine resin, unsaturated polyester resin, epoxy resin, polyurethane resin, polyamide resin, alkyd resin, or silicone resin, but is not limited thereto. It is not.
  • the electrical conductivity of the carbon nanotube conductive composite in general, for a multi-walled carbon nanotubes is an electrical permeation (percolation) occurs in the amount of about 1-2 wt. 0/0.
  • the multi-walled carbon nanotubes according to the present invention exhibit conductivity even at very low concentrations of 5 wt%.
  • the conductive composite using the same may be used in, for example, a bulk composite, a thin film composite, an energy field, and an electric and electronic field, and specifically, an electronic device antistatic and electrostatic dispersion plastic, an electromagnetic shielding, and a heat dissipation plastic, Conductive transparent electrodes used in OLEDs and solar cells, lithium ion battery additives, and carbon nanotube composites for concrete reinforcement and heat dissipation, but are not limited thereto.
  • Yet another aspect of the present disclosure provides an energy storage device including multi-walled carbon nanotubes. Carbon material including multi-walled carbon nanotubes is a very important material that determines the performance of the energy storage device, the energy storage device using the same, for example
  • Another aspect of the present application comprises at least one component selected from the group consisting of Fe, Co, Ca, Ni and Mo (preferably at least two components), and one component selected from the group consisting of Mn, Al, Mg and Si It includes the above (preferably two or more components), has a composition ratio represented by the following formula (1), the apparent density is 0.05 ⁇ 0.07g / m £, multi-walled carbon nanotubes grown per lg catalyst represented by the following formula 2 Provided is a plate-shaped catalyst for growing carbon nanotubes having a volume of 30 divided by the volume of catalyst lg:
  • a, b, c, d, e, w, x, z represents the mole fraction of each element, 0 ⁇ a ⁇ 10, 0 ⁇ b ⁇ 10, 0 ⁇ c ⁇ 10, 0 ⁇ d ⁇ 10, 0 ⁇ e ⁇ 10, 0 ⁇ w ⁇ 30, 0 ⁇ x ⁇ 30, 0 ⁇ y ⁇ 30, 0 ⁇ z ⁇ 30,
  • V t / c (W t XY t ) / (W c x Yc ) (2)
  • W t is the weight of carbon nanotubes that can be grown as a unit catalyst (lg)
  • W c is lg as the weight of the unit catalyst
  • p t is the apparent density of carbon nanotubes, and is the catalyst density of the catalyst).
  • the catalyst for example, iron ( ⁇ ) chloride tetrahydrate [Iron (II) chloride tetrahydrate], a substance containing iron (Fe) component [iron (II) sulfate heptahydrate [ Iron (II) sulfate heptahydrate], Iron (III) chloride anhydrous, Iron (III) nitrate nonahydrate [Iron (III) nitrate cobalt (II) acetate as a material comprising nonahydrate], ammonium iron (III) sulfate dodecahydrate, and cobalt (Co)
  • Calcium chloride anhydrous, Calcium nitrate tetrahydrate, Calcium sulfate dihydrate,
  • Ni nickel (II) chloride hexahydrate, nickel (II) nitrate hexahydrate, nickel (II) sulfate hexahydrate [Nickel (II) chloride hexahydrate] Nickel (II) sulfate hexahydrate], ammonium molybdate tetrahydrate, manganese (Mn), manganese (II) acetate tetrahydrate, manganese (II) chloride Tetrahydrate [Manganese (II) chloride
  • Manganese (II) nitrate hexahydrate Manganese (II) sulfate monohydrate, a material containing aluminum (Al), aluminum chloride nucleohydrate ( Aluminum chloride hexahydrate, Aluminum hydroxide, Aluminum
  • Another aspect of the present application provides a plate-shaped catalyst for growing carbon nanotubes having a specific surface area of 120 inVg or more.
  • the volume of multi-walled carbon nanotubes grown per catalyst lg divided by the volume of catalyst lg is 30 or more to increase the active reaction area by using a plate-shaped catalyst for growing carbon nanotubes.
  • Carbon nanotubes can be mass produced. Carbon nanotubes synthesized using the catalyst having a large specific surface area have low dispersion energy and high conductivity.
  • Another aspect of the present application provides a carbon nanotube comprising a plate-shaped catalyst. In the case of the plate-shaped catalyst, the surface area is larger than that of the spherical or acicular catalyst,
  • the range of high temperature for droplet spraying the mixture is, for example, 400 ⁇ 900 ° C., preferably 400-700 ° C., more preferably 400-500 ° C.
  • the present invention will be described in more detail with reference to Examples, but the present application is not limited thereto.
  • Example 1 The sum of the moles of Al and Mg in 100 of water is 16, and M6 (N0 3 ) 2 .63 ⁇ 40 and While adding and stirring A1C1 3 '6H 2 O, Fe (N0 3 ) 2 ' 9H 2 0 and Co (N0 3 ) 2 '6H 2 0 were added and stirred so that the sum of the moles of Fe and Co became 5. Thereafter, the mixture was calcined while spraying droplets in the range of 400-900 ° C. to obtain a catalyst.
  • Example 2 The same production method as in Example 1 was used, and the metal catalyst was prepared by changing the sum of the moles of AIII and Mg to 20.
  • Carbon nanotubes were prepared.
  • Preparation Example 2 Through a vapor deposition method using a catalyst obtained in Example 2 to raise the temperature of a reaction vessel under a carbon source gas and an inert gas to 400-1200 ° C.
  • Carbon nanotubes were prepared.
  • a batch type reactor As the reactors used to prepare the carbon nanotubes in Preparation Examples 1 and 2, a batch type reactor, a fluidized bed reactor, a rotary kiln reactor, etc. may be used.
  • a loop type fluidized bed reactor may be used, but is not limited thereto.
  • particulate plate catalysts with a maximized specific surface area were prepared.
  • 1 is a scanning electron microscope (SEM) image of a catalyst prepared according to Example 1.
  • FIG. The BET (Brunauer Emmett Teller) specific surface area measurement was 142 mVg, and the apparent density of the catalyst was applied according to Korean Industrial Standard (KS M ISO 1306). That is, in order to measure the walking density, the diameter is 100 ⁇ 10 ⁇ , there is no headlight on the straight wall of constant height, and it is not more than 50 mm higher than the edge of a cylindrical container with a capacity of 1,000 cm 3 when fully filled.
  • KS M ISO 1306 Korean Industrial Standard
  • the catalyst was placed in the center of the vessel, with excess catalyst used to make the cone higher than the edge of the vessel.
  • a straight line or spatula was horizontally contacted with the edge of the container at right angles, and then wiped once to select the surface and weighed with the catalyst.
  • the weight of the catalyst was determined by subtracting the cylinder weight to the nearest g number.
  • the coarse densities of the catalysts prepared in Example 1 and Example 2 measured as described above were 0.05 g / ⁇ and 0.02 g / m, respectively.
  • the multi-walled carbon nanotubes of Preparation Example 1 and Preparation Example 2 were prepared using the catalysts prepared in Examples 1 and 2, wherein the catalysts were synthesized per lg.
  • the amount of carbon nanotubes was 90g and 80g, respectively.
  • 2 g is dried over a little more than one hour of carbon nanotubes at 125 ° C and drying
  • the carbon nanotubes were placed in a weighed crucible and weighed up to 0.1 mg, which were placed in an electric furnace at 800 ⁇ 25 ° C until heated, and the lid was heated. After transferring to a desiccator and weighing with a real thread, the weight was measured to 0.1 mg, the crucible and the lid were washed, dried in a dryer at 125 ° C., and weighed again to 0.1 mg.
  • the BET specific surface areas of the multi-walled carbon nanotubes synthesized in Preparation Example 1 and Preparation Example 2 were 600 m7g, respectively, and the weight ratios (V t / C ) were 450 and 160, respectively.
  • the weight ratio (W) of the carbon nanotubes grown using the unit catalyst (lg) is 450, and the multi-walled carbon nanotubes grown to the volume of the unit catalyst lg. That's 450 times the volume of the tube. That is, since the volume of the unit catalyst lg is 20, it means that the volume of the multi-walled carbon nanotubes grown using the plate catalyst is 9,000 ⁇ (9 Liter).
  • FIGS. 2 and 3 show scanning electron microscope (SEM) and transmission electron microscope (TEM) images of carbon nanotubes prepared according to Preparation Example 1 and Preparation Example 2, respectively. Of 500 urn, 50 um, 1 ⁇ m, and 20 ran . The scale bar can be used to check the measured carbon nanotubes.
  • Figure 4 is a graph showing the surface resistance of the composite according to the content of the multi-walled carbon nanotubes (MWNT) grown using the catalyst of the present application, was measured to confirm the conductivity.
  • Nylon 66 / MWNT composite was prepared by varying the content of carbon nanotubes. As shown in FIG. 4, the composite starts to exhibit conductivity from the content of the multi-walled carbon nanotubes (MWNT) of 0.5 wt%, and as the content of the multi-walled carbon nanotubes increases, the conductivity of the composite rapidly increases. (A rapid decrease in surface resistance occurs as the content of multiwalled carbon nanotubes increases).
  • MWNT multi-walled carbon nanotubes
  • FIG. 5 A schematic diagram of a method for preparing a catalyst for multi-walled carbon nanotube synthesis is shown in FIG. 5.
  • the catalyst (plate-shaped catalyst) prepared by the catalyst production method according to the present invention has a very low density.
  • the surface area is very large compared to the weight, so that the production of multi-walled carbon nanotubes can be increased, and the multi-walled carbon nanotubes synthesized by using such catalysts have low dispersion energy during dispersion and damage in length during dispersion. It is very low enough to maintain high conductivity.
  • high-purity multi-walled carbon nanotubes synthesized using the catalyst prepared by the production method of the present invention have a diameter comparable to that of single-walled carbon nanotubes (SWNT), and the number of walls is very homogeneous, with 3-10.
  • SWNT single-walled carbon nanotubes

Abstract

La présente invention se rapporte à un catalyseur pour la synthèse de nanotubes de carbone à parois multiples et, plus particulièrement, un catalyseur pour la synthèse de nanotubes de carbone à parois multiples permettant de disperser facilement les nanotubes de carbone à parois multiples synthétisés et d'améliorer significativement la conductivité, à un procédé de production dudit catalyseur, et à des nanotubes de carbone à parois multiples synthétisés par ledit catalyseur.
PCT/KR2015/000053 2014-01-09 2015-01-05 Catalyseur pour la synthèse de nanotubes de carbone à parois multiples, procédé de production dudit catalyseur, et nanotubes de carbone à parois multiples synthétisés par ledit catalyseur WO2015105302A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2016543626A JP7179441B2 (ja) 2014-01-09 2015-01-05 多層カーボンナノチューブの合成のための触媒、及びその触媒で合成された多層カーボンナノチューブ
US15/110,737 US9975774B2 (en) 2014-01-09 2015-01-05 Catalyst for synthesizing multi-wall carbon nanotubes, method for producing catalyst, and multi-wall carbon nanotubes synthesized by catalyst
CN201580003474.4A CN105873679B (zh) 2014-01-09 2015-01-05 用于合成多壁碳纳米管的催化剂、其催化剂的制备方法及由其催化剂合成的多壁碳纳米管

Applications Claiming Priority (4)

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KR20140002743 2014-01-09
KR10-2014-0002743 2014-01-09
KR10-2014-0174427 2014-12-05
KR1020140174427A KR101756453B1 (ko) 2014-01-09 2014-12-05 다중벽 탄소나노튜브 합성을 위한 촉매, 그 촉매의 제조 방법 및 그 촉매로 합성된 다중벽 탄소나노튜브

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US11171322B2 (en) 2015-12-10 2021-11-09 Lg Chem, Ltd. Positive electrode having improved pore structure in positive electrode active material layer
CN114100614A (zh) * 2021-12-06 2022-03-01 桂林电子科技大学 一种中空碳材料负载Co-Cu-B纳米粒子的复合材料及其制备方法和应用

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11171322B2 (en) 2015-12-10 2021-11-09 Lg Chem, Ltd. Positive electrode having improved pore structure in positive electrode active material layer
CN114100614A (zh) * 2021-12-06 2022-03-01 桂林电子科技大学 一种中空碳材料负载Co-Cu-B纳米粒子的复合材料及其制备方法和应用

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