Homogeneous Metal Complex Solutions via In Situ Reaction
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Solution Overview
Problem
The existing processes for preparing 3,7-diazabicyclo[3.3.1]nonane iron or manganese complex solutions in aprotic organic solvents, such as propylene glycol, are inefficient due to the need for multiple solvents, isolation, and drying steps, making them uneconomical for industrial-scale production.
Innovation Solution
A process for preparing homogeneous solutions of metal complexes in situ in diols or polyols, like propylene glycol, by reacting ligands with metal salts in a heterogeneous reaction, eliminating the need for isolation and drying, and allowing the formation of complexes with a dihydroxyketal carbonyl group under acidic conditions.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If the complex is isolated and dried then the product can be obtained in crystalline form, but the process requires long reaction times and multiple solvents
Solution Approach 1:
The patent merges the complex formation reaction with the solution preparation step by performing the reaction directly in propylene glycol. This eliminates the need for separate isolation and drying steps, as the complex forms directly in the final solvent medium, reducing total process time while maintaining product quality
Solution Approach 2:
The patent extracts the isolation and drying steps from the traditional multi-step process. By choosing propylene glycol as the reaction solvent from the beginning, the method removes the intermediate isolation step entirely, as the complex remains soluble in the final product solvent
2Ease of manufacture
If different solvents are used for ligand and metal salt dissolution then complex formation can be carried out, but multiple solvents require workup procedures
Solution Approach 1:
Propylene glycol serves multiple functions simultaneously: it acts as the solvent for dissolving the ligand, the solvent for dissolving the metal salt, and the final product solvent. This multi-functionality eliminates the need for solvent exchange or workup procedures, simplifying the manufacturing process
Solution Approach 2:
The patent changes the solvent parameter from traditional aprotic organic solvents to propylene glycol, which has different solubility characteristics. This parameter change allows both the ligand and metal salt to be dissolved in the same solvent, eliminating the need for separate dissolution steps and subsequent workup
3Stability of the object's composition
If the complex is dissolved in propylene glycol after isolation then the solution can be prepared, but the solubility is poor requiring long reaction times
Solution Approach 1:
The patent performs preliminary action by conducting the complex formation reaction directly in propylene glycol before any isolation step. The complex forms in situ in the final solvent, ensuring maximum solubility from the beginning and eliminating subsequent dissolution steps, thereby maximizing productivity
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 enables the direct formation of stable, homogeneous solutions of iron and manganese complexes in propylene glycol, reducing production costs and time, and maintaining the dihydroxyketal form of the carbonyl group, which is environmentally friendly and suitable for industrial-scale use.
Implementation Method 1
by complexing a ligand compound in situ with a metal salt
Implementation Method 2
it could not be clear to the person skilled in the art that under the selected conditions a complex of the formula (2) can be formed in which the carbonyl group is present as a dihydroxyketal (hydrate), since work is carried out in the presence of a solvent which also enters into ketalization reactions under acidic reaction conditions can
Data Source
AI summary
The invention relates to a method for producing homogeneous solutions of metal complexes of general formula (2): [MaLxXn]Ym , where M is a metal from the group comprising Mn(II), Mn(III), Mn(IV), Fe(II), Fe(III) or Fe(IV), X is a coordinated compound selected from mono- bi- or tri-charged anions or neutral molecules which are able to coordinate with a metal mono- bi- or tri-dentate, Y is a non-coordinated counter-ion which ensures charge equalization of the complex, L is a ligand of general formula (1) or the protonized or de-protonized form thereof, and a, x, n, m, R, R1, R2, R3 and z are as specified in claim 1, in diols or polyols, the monoethers or mixtures of said substances. Said method is characterized in that a ligand of the formula (1) is reacted with an iron or manganese salt in a heterogeneous reaction in the diol or polyol, the monoethers or mixtures of these substances.