Integrated Reactor Clarifier for Precipitation Control

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Solution Overview

Problem

Existing methods for producing solid compounds by precipitation from solutions face challenges in independently adjusting process parameters, such as concentration of starting materials and salt concentration, which limits the flexibility and maximum achievable solids concentration, and makes it difficult to achieve specific particle size distributions and physical properties required for applications like battery precursors.

Innovation Solution

The use of an Integrated Reactor Clarifier System (IRKS) with a stirred reactor and an inclined clarifier allows for independent adjustment of process parameters, including solids concentration and salt concentration, enabling controlled particle size distribution and significantly increasing the maximum achievable solids concentration, thereby enhancing process flexibility and product properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If conventional precipitation methods are used, then solid compounds can be produced, but the process parameters (concentration of starting materials, salt concentration, solids concentration) cannot be adjusted independently, limiting flexibility and maximum achievable solids concentration

Engineering Contradiction:
Improveprocess parameter adjustment flexibilityVSAvoidsystem complexity
Core Design Contradiction:
Adaptability or versatilityVSDevice complexity

Solution Approach 1:

The system is divided into two functionally independent parts: a stirred reactor for precipitation and an integrated clarifier for separation. This segmentation allows independent control of process parameters in each unit - the reactor can operate with optimized precipitation conditions while the clarifier handles separation, enabling independent adjustment of starting material concentration, salt concentration, and solids concentration that was not possible in conventional single-vessel systems.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The clarifier is integrated directly into the reactor system, combining precipitation and separation functions in a unified apparatus. The clarifier receives the slurry directly from the reactor and enables continuous removal of supernatant, allowing the reactor to maintain high solids concentration while independently controlling salt concentration in the mother liquor, thus achieving parameter independence without requiring completely separate systems.

Inventive Principle:
Principle #5Merging (Combining)

2Productivity

If high solids concentration is achieved, then productivity increases, but the salt concentration in mother liquor also increases, limiting further solids concentration due to solubility constraints

Engineering Contradiction:
Improvespace-time yieldVSAvoidsalt concentration in mother liquor
Core Design Contradiction:
ProductivityVSQuantity of substance

Solution Approach 1:

The clarifier performs preliminary separation of the supernatant (mother liquor) from the precipitated solid phase before the slurry leaves the reactor. By continuously removing the supernatant containing dissolved salts through the integrated clarifier, the system prevents salt accumulation that would otherwise limit solids concentration, enabling continuous operation at high solids concentration and maximizing space-time yield.

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If process parameters are optimized for primary particle properties, then primary crystallite quality improves, but secondary particle properties (agglomerate characteristics) cannot be simultaneously optimized

Engineering Contradiction:
Improveprimary crystallite propertiesVSAvoidsecondary particle property control
Core Design Contradiction:
Manufacturing precisionVSAdaptability or versatility

Solution Approach 1:

The integrated clarifier acts as an intermediary between the precipitation reactor and the final product. It provides a controlled environment where secondary agglomeration can be managed separately from primary crystallization. The clarifier's controlled settling conditions allow optimization of secondary particle properties (agglomerate size, density) independently of primary crystallite properties, enabling simultaneous control of both levels of particle structure through separate parameter adjustment.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 approach allows for the production of tailor-made products with defined physical properties, particularly in battery precursors, by decoupling process parameters and increasing the space-time yield, enabling the production of high-quality materials with improved particle size distribution and density.

Implementation Method 1

the separation of the product suspension and the mother liquor is carried out by means of an integrated clarifier

Methodology Applied
Scientific EffectSedimentation: Sedimentation

Implementation Method 2

Device and method for the production of compounds by precipitating solids from solutions

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Data Source

PatentEP2007493B1Device and method for the production of compounds by precipitation
Publication Date: 2016.06.29 H C STARCK GMBH
  • EP2007493B1 patent drawingFigure 1~5
  • EP2007493B1 patent drawingFigure 6~7
  • EP2007493B1 patent drawingFigure 8

AI summary

The invention relates to a device and a method for the production of compounds by precipitation of solids from solutions, the physical and chemical properties of the solid particles formed on precipitation being flexible and can be independently fixable. Custom products can thus be produced with very high space-time yields and a particulate nickel/cobalt mixed hydroxide of formula NixCo1-x(OH)2, with a BET surface area of 20 m2/g and a tap density of greater than 2.4 g/cm3.