Diethylamino Hydroxybenzoyl Hexyl Ester Vacuum Purification
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Solution Overview
Problem
Existing processes for purifying 2-(4'-diethylamino-2'-hydroxybenzoyl)benzoic acid hexyl ester result in high phthalic acid dialkyl ester content and require additional steps to remove Rhodamine B type dyes, leading to inefficiencies and potential health risks.
Innovation Solution
A distillation process at controlled temperatures (100 to 250 °C) and pressures (less than 10 mbar) is employed to isolate 2-(4'-diethylamino-2'-hydroxybenzoyl)benzoic acid hexyl ester, separating it as a high boiler and removing phthalic acid dialkyl ester as a light boiler.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional purification methods (dissolution in nonpolar solvent, adsorption over activated carbon or silicic acid bed) are used to remove Rhodamine B type dyes, then the final product achieves low dye content (less than 10 ppm), but additional purification steps and equipment are required, increasing process complexity and time
Solution Approach 1:
The patent extracts and removes the harmful Rhodamine B type dyes through a specific purification step involving dissolution in nonpolar solvent (cyclohexane or toluene) followed by adsorption over activated carbon or silicic acid bed, separating the impurity from the final product to achieve less than 10 ppm dye content
Solution Approach 2:
The patent combines multiple purification operations (dissolution, adsorption, evaporation) into an integrated purification sequence that efficiently removes both Rhodamine B type dyes and excess reagents, achieving high purity product while streamlining the overall process
2Ease of operation
If conventional distillation is used to isolate the final product, then the product can be obtained as melt for bottling, but the phthalic acid dialkyl ester content remains high (15 ppm and more), posing health risks
Solution Approach 1:
The patent changes the distillation parameters by conducting the process under reduced pressure (vacuum conditions), which allows for effective separation of phthalic acid dialkyl ester from the final product, reducing its content to less than 20 ppm while maintaining product quality and handling convenience
Solution Approach 2:
The patent replaces conventional atmospheric distillation with vacuum distillation, substituting the mechanical approach with a pressure-controlled system that achieves better separation efficiency and lower harmful substance content in the final product
3Object-generated harmful factors
If additional purification steps are added to reduce phthalic acid dialkyl ester content, then the safety and purity of the final product improve, but the process time and complexity increase
Solution Approach 1:
The patent performs preliminary purification during the distillation step itself, where vacuum distillation simultaneously isolates the final product and removes phthalic acid dialkyl ester, achieving less than 20 ppm harmful substance content as an integrated part of the isolation process rather than requiring separate additional steps
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 final product with less than 20 ppm phthalic acid dialkyl ester, improving safety and handling convenience while maintaining high yield and purity.
Implementation Method 1
subjecting crude 2-(4'-diethylamino-2'-hydroxybenzoyl)benzoic acid hexyl ester to a distillation at a temperature in the range of from 100 to 250 °C at a pressure of less than 10 mbar
Implementation Method 2
distillation at a temperature in the range of from 100 to 250 °C at a pressure of less than 10 mbar
Implementation Method 3
evaporation of the solvent after passage through the bed
Data Source
Figure 1~2
AI summary
The present invention relates to a process for purifying 2-(4'-diethylamino-2'-hydroxybenzoyl)benzoic acid hexyl ester providing a high purity and low phthalic acid dialkyl ester content.