Continuous One-Pot Synthesis of Metal Salts

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Solution Overview

Problem

Traditional batch processes for synthesizing metal salts and metal complexes face challenges in managing phase transitions and particle size distribution, leading to heterogeneous products and operational inefficiencies, such as the formation of friable granules and broad particle size distributions, which complicate handling and homogeneity in the feeding industry.

Innovation Solution

A continuous one-pot synthesis process using a tubular reactor with a cylindrical stator and coaxial rotor, where reagents are fed and processed at high tangential speeds, forming a thin layer for enhanced heat exchange and mixing, allowing for efficient synthesis and drying of metal salts or metal complexes with controlled particle size and reduced energy consumption.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional batch processes are used for synthesizing metal salts, then the synthesis can be completed, but the reaction mixture undergoes problematic phase transitions from fluid to solid, forming friable granules with broad particle size distribution

Engineering Contradiction:
Improveparticle size distributionVSAvoidhandling of friable granules
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The patent employs a continuous flow reactor system where the salification reaction, drying, and granulation occur in a single continuous process without batch interruptions. This continuous operation maintains uniform reaction conditions and prevents the formation of friable granules by continuously moving the reaction mixture through controlled phases, thereby achieving narrow particle size distribution and eliminating handling problems associated with friable materials.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent utilizes controlled changes in temperature, residence time, and flow rate parameters within the continuous reactor to manage the phase transition of the reaction mixture. By precisely controlling these parameters, the process transforms the reaction mixture from fluid to granular form in a controlled manner, producing uniform particles with consistent size distribution and eliminating the broad distribution and friability issues of batch processes.

Inventive Principle:
Principle #35Parameter changes

2Strength

If batch processes are used, then synthesis can be performed, but extremely rugged reactors with oversized mixing forces are required to break up hardening mass

Engineering Contradiction:
Improvemixing forceVSAvoidreactor structure
Core Design Contradiction:
StrengthVSDevice complexity

Solution Approach 1:

The continuous flow reactor eliminates the need for rugged batch reactors by maintaining continuous motion of the reaction mixture through the system. The continuous flow design with controlled residence time prevents hardening mass formation, thereby eliminating the need for oversized mixing forces and rugged reactor structures, while achieving uniform product quality.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent replaces the mechanical mixing system of batch reactors with a continuous flow system where hydrodynamic conditions and controlled residence time achieve the desired mixing and reaction outcomes. This substitution eliminates the need for complex mechanical mixing equipment and rugged reactor structures while maintaining effective mass transfer and reaction homogeneity.

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

3Quantity of substance

If batch drying is used to achieve low humidity, then product humidity can be reduced to 1-2%, but the process generates broad particle size distribution including fine particulate matter below 40 micrometers

Engineering Contradiction:
ImprovehumidityVSAvoidparticle size distribution
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The patent combines the drying and granulation operations into a single integrated continuous process step. By merging these operations, the process achieves low humidity (1-2%) while simultaneously forming uniform granules with narrow size distribution, preventing the formation of fine particulate matter below 40 micrometers that would otherwise be generated by separate batch drying operations.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The continuous flow system maintains constant drying conditions and residence time, preventing the formation of fine particles during the drying process. The continuous movement of material through the dryer ensures uniform moisture removal and simultaneous granulation, achieving low humidity without generating the broad particle size distribution and fine particulate matter associated with batch drying.

Inventive Principle:
Principle #20Continuity of useful action

4Productivity

If traditional batch systems are used, then synthesis can be performed, but energy consumption is high and equipment requirements are excessive

Engineering Contradiction:
Improvesynthesis efficiencyVSAvoidenergy consumption
Core Design Contradiction:
ProductivityVSUse of energy by moving object

Solution Approach 1:

The continuous flow reactor maintains continuous operation without batch interruptions, eliminating the energy-intensive heating and cooling cycles required in batch processes. The continuous flow system with controlled residence time achieves complete reaction and drying in a single pass, significantly reducing energy consumption while maintaining high synthesis efficiency and productivity.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent extracts the drying function from a separate batch operation and integrates it into the continuous flow reaction system. This integration eliminates redundant energy consumption associated with separate batch drying operations, achieving both synthesis and drying in a single continuous process with reduced overall energy requirements and simplified equipment needs.

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

The process achieves a more uniform particle size distribution, increased yield, reduced energy usage, and improved handling characteristics, overcoming the limitations of traditional batch systems by enabling efficient synthesis and drying with minimal equipment and energy requirements.

Implementation Method 1

at least one rotor coaxial to the stator provided with centrifugation and stirring means, setting a tangential speed of rotation of the rotor to 10-50 m/s

Methodology Applied
Scientific EffectCentrifugal force: Centrifugal Force

Implementation Method 2

at least a first thermal jacket extended over at least 30% of the stator surface; setting said first thermal jacket to a temperature of 80-400° C.

Methodology Applied
Scientific EffectHeat transfer: Heat Exchanger

Data Source

PatentUS10604479B2Continuous process for the one-pot synthesis of metal salts and metal complexes
Publication Date: 2020.03.31 NOVUS INTERNATIONAL INC
  • US10604479B2 patent drawing
  • US10604479B2 patent drawing
  • US10604479B2 patent drawing

AI summary

A continuous process is described for the one-pot synthesis of compounds, such as metal salts and metal complexes, as well as optionally for the protection of the compounds thus obtained by coating and/or impregnation with suitable compounds.