Cobalt Catalyst Precursor Calcination via Periodic Heating Rates

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Solution Overview

Problem

The preparation of cobalt-containing Fischer-Tropsch synthesis catalysts often results in varying activity levels due to inconsistencies in the calcination process, particularly with regards to cobalt particle size and dispersion, which affects the catalyst's efficiency in hydrocarbon synthesis.

Innovation Solution

A process involving a combination of high and low heating rate periods during calcination, with specific temperature ranges and gas flow rates, is employed to produce a cobalt-containing hydrocarbon synthesis catalyst precursor, aiming to achieve small cobalt crystallites and enhanced catalyst activity. This process includes calcining a loaded catalyst support with a cobalt compound using high heating rates followed by low heating rates, and using inert or oxygen-containing gases to decompose the cobalt compound into cobalt oxide, thereby optimizing catalyst performance.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If a conventional calcination process is used with constant heating rate, then the process is simple to operate, but the cobalt particle size and dispersion are inconsistent leading to varying catalyst activity

Engineering Contradiction:
Improvecobalt particle size and dispersion consistencyVSAvoidcalcination process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The calcination process employs periodic variation of heating rates, alternating between high heating rate periods (at least 10°C/minute) and low heating rate periods (less than 10°C/minute). This periodic action creates controlled thermal cycles that promote uniform cobalt compound decomposition and prevent localized overheating, resulting in consistent small cobalt crystallite sizes and homogeneous dispersion throughout the catalyst support.

Inventive Principle:
Principle #19Periodic action

Solution Approach 2:

The invention changes the heating rate parameter dynamically during calcination, switching between high and low rates at different stages. This parameter variation allows optimization of different decomposition phases: high rates for rapid temperature achievement and low rates for controlled decomposition, thereby achieving precise control over cobalt particle formation and improving manufacturing precision without excessive process complexity.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If high heating rate is used throughout calcination, then the process time is reduced, but cobalt compound decomposition becomes uneven affecting catalyst activity

Engineering Contradiction:
Improvecalcination process speedVSAvoidcobalt compound decomposition uniformity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The calcination process employs periodic variation of heating rates, alternating between high heating rate periods (at least 10°C/minute) and low heating rate periods (less than 10°C/minute). This periodic action creates controlled thermal cycles that promote uniform cobalt compound decomposition and prevent localized overheating, resulting in consistent small cobalt crystallite sizes and homogeneous dispersion throughout the catalyst support.

Inventive Principle:
Principle #19Periodic action

Solution Approach 2:

The process applies preliminary low heating rate periods before the main high heating rate periods, allowing gradual preparation of the cobalt compound for decomposition. This preliminary action prevents sudden violent decomposition that would cause uneven particle distribution, while still maintaining overall process efficiency through subsequent high-rate heating phases.

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If low heating rate is used throughout calcination, then cobalt compound decomposition is uniform, but the process time increases reducing productivity

Engineering Contradiction:
Improvecobalt compound decomposition uniformityVSAvoidcalcination process speed
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The calcination process employs periodic variation of heating rates, alternating between high heating rate periods (at least 10°C/minute) and low heating rate periods (less than 10°C/minute). This periodic action creates controlled thermal cycles that promote uniform cobalt compound decomposition and prevent localized overheating, resulting in consistent small cobalt crystallite sizes and homogeneous dispersion throughout the catalyst support.

Inventive Principle:
Principle #19Periodic action

Solution Approach 2:

The process applies low heating rates only partially during specific critical decomposition phases, rather than throughout the entire calcination. This partial application of low heating rate ensures uniform decomposition where needed, while high heating rates are used in other phases to maintain overall productivity, achieving a balance between precision and speed.

Inventive Principle:
Principle #16Partial or excessive action

4Reliability

If high gas flow velocity is used during calcination, then oxygen supply for decomposition is sufficient, but heat loss increases reducing heating efficiency

Engineering Contradiction:
Improveoxygen supply adequacyVSAvoidheating efficiency
Core Design Contradiction:
ReliabilityVSUse of energy by moving object

Solution Approach 1:

The gas flow velocity is varied periodically, matching the heating rate profile. During high heating rate periods, gas flow is optimized to balance oxygen supply with heat retention. During low heating rate periods, higher gas flow ensures adequate oxygen for decomposition. This periodic coordination of gas flow with heating cycles maintains both reliability of decomposition and acceptable heating efficiency.

Inventive Principle:
Principle #19Periodic action

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

The described process effectively produces catalysts with smaller cobalt crystallites and improved activity, reducing particle break-up and maintaining catalyst precursor integrity, leading to enhanced hydrocarbon synthesis efficiency.

Implementation Method 1

calcining a loaded catalyst support comprising a catalyst support supporting a cobalt compound to decompose the cobalt compound and/ or to cause the cobalt compound to react with oxygen, the calcination thereby converting the cobalt compound into a cobalt oxide

Methodology Applied
Scientific EffectDecomposition: Decomposition (biological)

Implementation Method 2

cause the cobalt compound to react with oxygen, the calcination thereby converting the cobalt compound into a cobalt oxide

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 3

heating the loaded catalyst support over a heating temperature range of 90°C to 220°C using one or more high heating rate periods

Methodology Applied
Scientific EffectHeating: Heating

Data Source

PatentEP2704827B1A process for preparing a cobalt-containing hydrocarbon synthesis catalyst precursor
Publication Date: 2021.02.17 SASOL TECHNOLOGY (PTY) LTD

AI summary

A process for preparing a cobalt-containing hydrocarbon synthesis catalyst precursor includes calcining a loaded catalyst support comprising a catalyst support supporting a cobalt compound. The calcination includes heating the loaded catalyst support over a heating temperature range of 90°C to 220°C using (i) one or more high heating rate periods during the heating over the heating temperature range wherein heating of the loaded catalyst support takes place at a heating rate of at least 10°C/minute, and wherein a gas velocity of at least 5m3 n/kg cobalt compound/hour is effected over the loaded catalyst support, and (ii) one or more low heating rate periods during the heating over the heating temperature range wherein heating of the loaded catalyst support takes place at a heating rate of less than 6°C/minute. The cobalt compound is thereby calcined, with a cobalt-containing hydrocarbon synthesis catalyst precursor being produced.