Continuous Multi-Wall Carbon Nanotube Synthesis via Fluidized-Bed Reactor

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Solution Overview

Problem

Existing methods for preparing multi-walled carbon nanotubes using fixed-bed chemical vapor deposition reactors are not suitable for mass production due to low productivity and non-uniformity, and catalysts prepared by spray drying at low temperatures have high apparent density, making them unsuitable for fluidized-bed reactors.

Innovation Solution

A continuous process involving the preparation of a catalyst powder by dissolving metal precursors in a solvent, subjecting the solution to thermal decomposition while spraying into a reactor, and introducing the catalyst powder into a fluidized-bed reactor heated to 600° C. to 900° C., with specific metal compositions and hollow structures optimized for high conversion rates.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If catalysts are prepared by spray drying at low temperature (200-350°C), then the catalyst formation process is simple, but the apparent density becomes high and uniformity is poor

Engineering Contradiction:
Improvecatalyst preparation simplicityVSAvoidcatalyst uniformity
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent changes the temperature parameter from low temperature (200-350°C) to high temperature (700-900°C) spray pyrolysis, which fundamentally alters the catalyst formation process. This temperature change enables the formation of hollow spherical structures with controlled wall thickness and uniform composition, resolving the uniformity problem while maintaining ease of manufacture through a single-step process

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs composite catalyst materials with specific metal compositions (Fe-Co-Mo-V-W system) that form hollow spherical structures through spray pyrolysis. The composite nature of the catalyst, with multiple metal components working synergistically, achieves both high uniformity and appropriate apparent density (0.3-0.8 g/cm³), overcoming the limitations of simple spray-dried catalysts

Inventive Principle:
Principle #40Composite materials

2Ease of operation

If fixed-bed chemical vapor deposition reactor is used, then the process is simple to operate, but productivity is low and uniformity is poor

Engineering Contradiction:
Improvereactor operation simplicityVSAvoidcarbon nanotube production rate
Core Design Contradiction:
Ease of operationVSProductivity

Solution Approach 1:

The patent replaces the mechanical fixed-bed reactor system with a fluidized-bed reactor system. This substitution enables continuous fluidization of catalyst particles, allowing for continuous carbon nanotube synthesis at high productivity rates while maintaining operational simplicity through automated feed control and temperature management

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent implements a continuous process where catalyst particles are continuously fed into the fluidized-bed reactor, and carbon nanotubes are continuously synthesized and collected. This continuous operation eliminates the batch processing limitations of fixed-bed reactors, achieving high productivity and uniform product quality through sustained reaction conditions

Inventive Principle:
Principle #20Continuity of useful action

3Ease of manufacture

If spray drying is used for catalyst preparation, then the process is simple, but the catalyst requires additional firing process and has high apparent density

Engineering Contradiction:
Improvecatalyst preparation simplicityVSAvoidprocess steps
Core Design Contradiction:
Ease of manufactureVSDevice complexity

Solution Approach 1:

The patent changes the temperature parameter from low temperature (200-350°C) to high temperature (700-900°C) spray pyrolysis, which fundamentally alters the catalyst formation process. This temperature change enables the formation of hollow spherical structures with controlled wall thickness and uniform composition, resolving the uniformity problem while maintaining ease of manufacture through a single-step process

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent extracts and eliminates the separate firing process step by incorporating sintering into the spray pyrolysis process itself. The high-temperature spray pyrolysis (700-900°C) directly forms the hollow spherical catalyst structures with appropriate density and porosity, removing the need for subsequent firing treatment and simplifying the overall process

Inventive Principle:
Principle #2Taking out (Extraction)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method achieves a conversion rate of 80% or more, enabling the mass production of multi-walled carbon nanotubes with high economic efficiency and improved uniformity, suitable for fluidized-bed reactors.

Implementation Method 1

forming a catalyst powder by subjecting the precursor solution to thermal decomposition while spraying the same into a reactor

Methodology Applied
Scientific EffectThermal decomposition: Pyrolysis

Implementation Method 2

introducing the same into a fluidized-bed reactor heated to a temperature of 600° C. to 900° C.

Methodology Applied
Scientific EffectThermal heating: Heating

Implementation Method 3

synthesizing multi-walled carbon nanotubes from the catalyst powder by introducing the same into a fluidized-bed reactor

Methodology Applied
Scientific EffectChemical vapor deposition: Chemical Vapour Deposition

Data Source

PatentUS11117803B2Method for manufacturing multi-wall carbon nanotubes using continuous type process
Publication Date: 2021.09.14 KOREA KUMHO PETROCHEMICAL CO LTD
  • US11117803B2 patent drawing
  • US11117803B2 patent drawing

AI summary

A method for manufacturing multi-wall carbon nanotubes, includes the steps of: (a) dissolving a metal precursor in a solvent to prepare a precursor solution; (b) perform thermal decomposition while spraying the precursor solution into a reactor, thereby forming a catalyst powder; and (c) introducing the catalyst powder into a fluidized-bed reactor heated to 600-900° C. and spraying a carbon-based gas and a carrier gas to synthesize multi-wall carbon nanotubes from the catalyst powder, wherein steps (a) to (c) are performed in a continuous type and wherein the catalyst powder contains metal components according to equation 1 below. <Equation 1> Ma:Mb=x:y, wherein Ma represents at least two metals selected from Fe, Ni, Co, Mn, Cr, Mo, V, W, Sn, and Cu; Mb represents at least one metal selected from Mg, Al, Si, and Zr; x and y each represent the molar ratio of Ma and Mb; and x+y=10, 2.0≤x≤7.5, and 2.5≤y≤8.0.