Cyclic Compound Purification by Precipitation and Warm Solvent Washing
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Solution Overview
Problem
Existing methods for producing high-purity cyclic compounds with furan units, such as furan-2,5-dicarboxylic acid, require lengthy reaction times and complex purification steps, leading to low yields and high costs due to the need for silica adsorption, column chromatography, and distillation, which are not suitable for industrial-scale production.
Innovation Solution
A method involving selective precipitation and solvent washing of cyclic compounds at temperatures above the precipitation point, allowing for high-yield purification of cyclic compounds to 99% purity without additional purification steps, utilizing a reactor, precipitator, and washing solvent to separate and purify cyclic compounds efficiently.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional purification methods (silica adsorption, column chromatography, distillation) are used to obtain high-purity cyclic compounds, then purity reaches 99% or more, but production time increases to up to 9 hours and overall yield drops below 60%
Solution Approach 1:
The patent changes the temperature parameter of the washing solvent to above the precipitation temperature, which fundamentally alters the purification mechanism. This parameter change allows impurities to remain dissolved while the cyclic compound precipitates, achieving high purity without time-consuming conventional purification steps and maintaining high overall yield
Solution Approach 2:
The patent extracts impurities from the cyclic compound by washing the precipitated solid with a warm solvent. The impurities are selectively dissolved and removed in the washing solvent, leaving the purified cyclic compound as a solid residue, thereby achieving high purity through a simple extraction process rather than complex purification sequences
2Quantity of substance
If ring-closing reaction is performed to produce cyclic compounds from linear monomers, then cyclic compounds are obtained, but purity is limited to less than 95% due to thermodynamic equilibrium between linear and cyclic compounds
Solution Approach 1:
The patent utilizes phase transition by cooling the reaction mixture to precipitate the cyclic compound as a solid, separating it from the liquid phase containing linear compounds and impurities. This phase separation overcomes the thermodynamic equilibrium limitation by physically removing the cyclic compound from the equilibrium system
Solution Approach 2:
The patent extracts the cyclic compound from the reaction mixture by precipitation and subsequent washing. The cyclic compound is separated from linear compounds and impurities through selective precipitation, and further purified by washing with warm solvent that dissolves impurities but not the cyclic compound
3Duration of action of moving object
If distillation-assisted cyclodepolymerization is used to produce cyclic compounds, then reaction time is reduced and volatile side products are removed, but purity remains below 95% and high dilution of cyclic compounds occurs
Solution Approach 1:
The patent uses phase transition by cooling the reaction mixture to precipitate the cyclic compound as a solid, separating it from the liquid phase. This simple crystallization step achieves high purity without requiring lengthy conventional purification procedures, maintaining both short reaction time and high purity
Solution Approach 2:
The patent extracts impurities from the cyclic compound through washing with warm solvent. This simple extraction step removes remaining impurities after precipitation, achieving 99% or higher purity without the need for complex purification sequences that would extend reaction time
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 achieves high-purity cyclic compounds suitable for ring-opening polymerization, reducing production time and costs by eliminating the need for complex purification processes, thereby enhancing the efficiency and economic viability of biobased aromatic polyester production.
Implementation Method 1
the crude composition is cooled to a precipitation temperature being below the solubility temperature of at least one of the at least one cyclic compound contained in the crude composition for precipitating at least a portion thereof
Implementation Method 2
solubility temperature of at least one of the at least one cyclic compound
Implementation Method 3
washing the solid cyclic compound fraction obtained in step iii) with a washing solvent having a temperature of above the precipitation temperature used in step ii)
Data Source
AI summary
A method for preparing a purified cyclic compound composition includes providing in a reactor a reaction mixture containing a cyclizable linear compound and reacting the cyclizable linear compound to obtain a crude composition containing at least one cyclic compound, feeding a portion of the crude composition obtained to a precipitator, the crude composition cooled to a precipitation temperature below the solubility temperature of the cyclic compound contained for precipitating a portion thereof to obtain precipitated solid cyclic compound and unprecipitated liquid, separating a portion of the precipitated solid cyclic compound to obtain a solid cyclic compound fraction and unprecipitated liquid fraction, and washing the solid cyclic compound fraction obtained with a washing solvent having a temperature of above the precipitation temperature to obtain a washing solvent fraction and as purified cyclic compound composition a washed solid cyclic compound fraction.