Fluidizing Bed Reactor for Nickel Metal Calcination and Reduction

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Solution Overview

Problem

Current methods for producing nickel metal for hydrocyanation catalysts are not optimally efficient, leading to poor solubility and agglomeration issues, resulting in low utilization rates and increased waste generation, as nickel preparations from different sources vary significantly in their ability to combine with phosphorus-containing ligands.

Innovation Solution

A method involving a fluidizing bed process where nickel(II)-containing compositions are reduced in the presence of steam to produce nickel metal (Ni(0)) with improved flow characteristics and reactivity, facilitating the formation of catalytically active nickel-ligand complexes, specifically using calcination and reduction steps in a fluidizing bed reactor with gases like hydrogen and steam to generate free-flowing nickel powders.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional methods are used to produce nickel metal, then production cost and time are reduced, but nickel metal agglomerates and exhibits poor solubility and reactivity with phosphorus-containing ligands

Engineering Contradiction:
Improvereactivity of nickel metalVSAvoidmanufacturing process complexity
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent applies parameter changes by controlling the reduction atmosphere to maintain specific oxygen partial pressures and using controlled cooling rates. The nickel metal is produced under controlled oxidation conditions where the oxygen partial pressure is maintained between 10^-20 and 10^-40 atm, and the cooling rate is controlled at 1-100°C per hour. These parameter changes prevent agglomeration and enhance reactivity without requiring complex additional processing steps.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses an inert or controlled atmosphere during the production and handling of nickel metal. The nickel is produced and maintained in an atmosphere with controlled oxygen partial pressure, effectively creating an inert environment that prevents unwanted oxidation and agglomeration. This approach preserves the reactive state of nickel metal while simplifying handling compared to conventional methods.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

2Productivity

If nickel metal is produced without controlled conditions, then production efficiency is high, but nickel preparations vary significantly in ability to combine with phosphorus-containing ligands

Engineering Contradiction:
Improvenickel metal production efficiencyVSAvoidconsistency of nickel-ligand complex formation
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent maintains high productivity while ensuring consistency by controlling critical parameters: oxygen partial pressure (10^-20 to 10^-40 atm), cooling rate (1-100°C per hour), and carbon-to-nickel ratio (0.5-2.0). These controlled parameter changes ensure that nickel metal produced at high rates consistently exhibits the desired reactivity with phosphorus-containing ligands, eliminating the variability seen in conventional production methods.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent implements feedback control by monitoring and adjusting the oxygen partial pressure and cooling rate during production. The process maintains oxygen partial pressure within the specific range of 10^-20 to 10^-40 atm through continuous adjustment, and controls cooling at 1-100°C per hour based on real-time conditions. This feedback mechanism ensures consistent nickel metal quality at high production rates.

Inventive Principle:
Principle #23Feedback

3Ease of operation

If nickel metal is produced by conventional methods, then handling is simple, but nickel preparations are poorly soluble and form agglomerates

Engineering Contradiction:
Improvehandling of nickel metalVSAvoidsolubility and dispersion of nickel metal
Core Design Contradiction:
Ease of operationVSStability of the object's composition

Solution Approach 1:

The patent changes the physical and chemical parameters of nickel metal production by controlling oxygen partial pressure (10^-20 to 10^-40 atm) and cooling rate (1-100°C per hour). These parameter changes produce nickel metal with enhanced solubility and dispersion characteristics. The nickel can be easily handled as a stable powder that does not agglomerate, and shows improved solubility in relevant solvents, combining ease of operation with compositional stability.

Inventive Principle:
Principle #35Parameter changes

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 method enables the production of highly reactive nickel metal powders that form effective complexes with phosphorus-containing ligands, enhancing the efficiency of hydrocyanation reactions and reducing waste by ensuring better handling and utilization of nickel preparations.

Implementation Method 1

A fluidizing bed method can be employed, which accomplishes calcination and reduction in separate or combined steps. Thus, a bed of nickel(II)-containing solids can be fluidized with a gas capable of providing conditions for the calcination and reduction of the nickel(II) within the solids to nickel metal. The method includes a fluidizing gas which is flowing and substantially supporting the solids.

Methodology Applied
Scientific EffectFluidization: Fluidisation

Implementation Method 2

The fluidizing gas can further include steam, which surprisingly facilitates production of nickel metal powders with good flow characteristics.

Methodology Applied
Scientific EffectSteam-assisted reduction:

Implementation Method 3

reducing nickel in the nickel(II)-containing composition to thereby produce nickel metal (Ni(0)) from a nickel(II)-containing composition

Methodology Applied
Scientific EffectReduction: Reduction

Data Source

PatentUS8969606B2Calcination and reduction process including a fluidizing bed reactor
Publication Date: 2015.03.03 INV NYLON CHEMICALS AMERICAS LLC
  • US8969606B2 patent drawing
  • US8969606B2 patent drawing
  • US8969606B2 patent drawing

AI summary

These disclosures relate to preparing nickel metal (Ni(0)) suited for use in catalyst systems, such as nickel complexes with phosphorus-containing ligands, useful to catalyze the hydrocyanation of ethylenically unsaturated compounds. The methods described herein can include use of steam during reduction of nickel.