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CN-116764639-B - Catalyst and preparation method thereof, array type carbon nano tube and preparation method thereof

CN116764639BCN 116764639 BCN116764639 BCN 116764639BCN-116764639-B

Abstract

The application relates to the field of carbon nanotube catalyst materials, and particularly discloses a catalyst and a preparation method thereof, an array type carbon nanotube and a preparation method thereof. A catalyst is formed as platelet-shaped nanocrystals comprising at least one metal ion having microwave activity. The preparation method of the catalyst comprises the steps of S1, microwave auxiliary reaction, S2, standing and ageing, S3, and calcining treatment. The array type carbon nanotube is prepared by catalysis of a catalyst, and comprises a plurality of unit carbon nanotube bundles, wherein the unit carbon nanotube bundles comprise a plurality of carbon nanotubes which are intertwined and have a tube length of more than 1 mu m, and the tube diameter of the unit carbon nanotube bundles is 0.2-2 mu m. The carbon nano tube prepared by the catalyst has consistent length-diameter ratio, good orientation and higher purity, thereby being beneficial to exerting the excellent performance.

Inventors

  • LI ZHIWEN
  • NING GUOQING
  • ZHAO JIE
  • ZHANG MEIJIE
  • ZHENG TAO

Assignees

  • 江苏天奈科技股份有限公司

Dates

Publication Date
20260508
Application Date
20220309

Claims (2)

  1. 1. The preparation method of the array type carbon nano tube is characterized by comprising the following preparation steps: placing a catalyst in a reactor, heating to 700-750 ℃ under a protective gas by a program, stopping introducing the protective gas, introducing carbon source gas instead, and carrying out catalytic reaction for 20-50 min at 700-750 ℃ to obtain the array carbon nanotube; The preparation method of the catalyst comprises the following preparation steps: S1, carrying out microwave-assisted reaction, namely placing a metal ion salt solution with microwave activity into a microwave reaction device, heating by microwaves, adding an alkaline salt solution, and carrying out heat preservation and stirring reaction; s2, standing and aging, namely continuing microwave reaction after stopping stirring, filtering and collecting a filter cake after standing and aging, washing and drying, and collecting a reactant; s3, calcining, namely taking reactants, calcining, standing, cooling, grinding and sieving to obtain the catalyst for the array type carbon nano tube; wherein the catalyst is a flaky nano-grain and comprises n microwave active metal ions, and the type n of the microwave active metal ions is more than or equal to 4; the metal ions with microwave activity comprise a plurality of Fe ions, co ions, ni ions, zn ions, mg ions, al ions, mo ions and La ions; The metal ion salt with microwave activity described in the step S1 comprises metal ion salt capable of generating layered double hydroxide; The step S1 of microwave heating comprises the steps of adjusting the microwave power to 500-4000W, controlling the microwave heating reaction temperature to 50-100 ℃ and the microwave reaction time to 0.5-6 h; The alkaline salt solution comprises one or two of sodium carbonate solution, sodium bicarbonate solution, ammonium carbonate solution, ammonium bicarbonate solution or urea solution; The standing and ageing temperature is 50-100 ℃ and the standing and ageing time is 1-12 h; the array type carbon nano tube is provided with a plurality of unit carbon nano tube bundles; The unit carbon nanotube bundles comprise a plurality of carbon nanotubes which are intertwined and have a tube length of more than 1 mu m; The tube diameter of the unit carbon nanotube bundle is 0.2-2 mu m, and the powder resistivity is less than 30mΩ & cm.
  2. 2. The method for preparing array-type carbon nanotubes according to claim 1, wherein the specific surface area of the array-type carbon nanotubes is more than 400m2/g.

Description

Catalyst and preparation method thereof, array type carbon nano tube and preparation method thereof Technical Field The application relates to the field of carbon nanotube catalyst materials, in particular to a catalyst and a preparation method thereof, an array type carbon nanotube and a preparation method thereof. Background As a novel nanomaterial, carbon nanotubes have attracted much attention due to their unique nanostructure and excellent physicochemical properties. Carbon nanotubes have shown special properties in many fields, such as mechanics, electricity, thermal and optics, and thus have created potential new applications in many fields. Generally, carbon nanotubes can be classified into array-type carbon nanotubes and agglomerated carbon nanotubes according to their microscopic aggregation state. Because the carbon nanotubes grown on the unordered and piled catalyst show a certain aggregation structure, the carbon nanotubes are seriously wound and are in unordered arrangement, so that the subsequent dispersing and other processing processes become difficult. Therefore, under certain conditions, the carbon nano tubes can be obviously oriented, and parallel arrangement is realized, namely the carbon nano tube array is formed. Compared with the agglomerated carbon nanotubes, the array carbon nanotubes have consistent length-diameter ratio, good orientation and higher purity, thereby being beneficial to exerting the excellent performance. The related Chinese patent publication No. CN112871181A discloses a carbon nanotube catalyst, a preparation method thereof and a preparation method of carbon nanotubes, which can improve the yield of the carbon nanotubes and reduce the production cost of the carbon nanotubes. The preparation method of the carbon nanotube catalyst comprises the steps of mixing an active component solution, an inactive component solution and a carbon carrier to obtain a precursor solution, removing a solvent contained in the precursor solution to obtain a precursor, roasting the precursor under the anaerobic condition to obtain the carbon nanotube catalyst, and preparing the carbon nanotubes by using the catalyst. However, the carbon nanotubes prepared by the catalyst of the patent have uneven structure, the array type carbon nanotubes cannot be effectively prepared, and the process for preparing the nano catalyst by the traditional preparation method has the defects of slower reaction speed, longer aging time, larger particle size of the produced crystals and the like, which is not beneficial to the growth of the high-quality and high-yield carbon nanotubes. Disclosure of Invention In order to solve the problems that the existing array type carbon nanotube catalyst is poor in production efficiency and the quality of the catalytically produced carbon nanotube material is defective, the application provides a catalyst and a preparation method thereof, and an array type carbon nanotube and a preparation method thereof. In a first aspect, the present application provides a catalyst, which adopts the following technical scheme: A catalyst is a flaky nano-grain and comprises n microwave active metal ions, wherein the type n of the microwave active metal ions is more than or equal to 1. By adopting the technical scheme, the structure of the catalyst material is optimized, and the catalyst is prepared into nano grains in a sheet shape. The catalyst can obviously influence the structural characteristics of the carbon nano tube in the actual growth and preparation process, so that the optimized flaky nano crystal grain has higher activity, and is more suitable for mass production of array carbon nano tubes with more excellent multiplying power and conductivity. According to the technical scheme, the metal ions with microwave activity are selected to prepare the flaky nano-crystalline grains, so that the catalyst generates a thermal effect by exciting dipole steering polarization and interface polarization of polar microscopic particles in the actual production process, and the prepared catalyst material has a good flaky shape. Preferably, the metal ions with microwave activity comprise one or more of Fe ions, co ions, ni ions, zn ions, mg ions, al ions, mo ions and La ions. By adopting the technical scheme, the catalyst material prepared from the metal ions with microwave activity can continuously vibrate and move under the auxiliary condition of microwave heating, so that the number of crystal lattices with defects is reduced, the structure of the prepared catalyst material is more regular, and the structure of the prepared catalyst is further optimized. In a second aspect, the present application provides a method for preparing a catalyst, comprising the steps of: S1, carrying out microwave-assisted reaction, namely placing a metal ion salt solution with microwave activity into a microwave reaction device, heating by microwaves, adding an alkaline salt solution, and carrying out heat preser