Xanthophyll Crystal Purification via Solvent System Optimization
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Solution Overview
Problem
Current methods for producing xanthophyll crystals face challenges such as low purity, low yield, and environmental pollution due to the use of solvents with high boiling points, large water consumption, and inefficient saponification processes, making it difficult to achieve high-quality xanthophyll suitable for human consumption as a food colorant and nutrient supplement.
Innovation Solution
A process involving the dissolution of plant extracts in n-hexane, followed by filtration and treatment with acetone, then saponification using an alkaline solution, followed by acidic pH adjustment and solvent recovery, which includes the use of organic solvents to enhance separation and reduce water usage, ultimately resulting in a high-purity xanthophyll crystal through a mixed solvent purification step.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If propylene glycol is used as solvent for saponification, then the extraction can be performed, but the solvent is difficult to recover and the product purity is low (about 70%)
Solution Approach 1:
The patent changes the solvent system from propylene glycol to a mixture of n-hexane and ethanol, and adjusts the saponification conditions (temperature, alkali concentration) to optimize both purity and yield. This parameter change resolves the contradiction by achieving high purity (90%+) while maintaining ease of manufacture.
Solution Approach 2:
The patent introduces an intermediary step of acidification after saponification, where the alkaline saponified product is treated with acid to precipitate the xanthophyll crystal. This intermediary step enables effective separation and purification, resolving the purity issue while maintaining manufacturing feasibility.
2Ease of manufacture
If large amount of water is used for dilution and extraction, then the extraction can be performed, but environment pollution increases and yield is low
Solution Approach 1:
The patent changes the solvent system from water-based to organic solvent-based (n-hexane and ethanol), which reduces water consumption and environmental pollution while maintaining extraction effectiveness. This parameter change resolves the contradiction between ease of manufacture and environmental harm.
Solution Approach 2:
The patent extracts xanthophyll from the saponified product using organic solvents, separating it from impurities and waste water. This extraction step reduces environmental pollution by minimizing water usage while maintaining high yield and purity.
3Ease of manufacture
If marigold petals are dried before saponification, then the extraction can be performed, but the drying time is too long and affects production scale
Solution Approach 1:
The patent performs preliminary extraction of xanthophyll ester from fresh marigold petals using n-hexane before saponification, avoiding the need for prolonged drying. This preliminary action resolves the time loss issue while maintaining extraction capability.
Solution Approach 2:
The patent changes the processing sequence by performing extraction before drying, and uses optimized saponification conditions (higher temperature, adjusted alkali concentration) to compensate for the skipped drying step, thereby reducing total processing time while maintaining product quality.
4Ease of manufacture
If metallic halide is used to adjust pH, then the extraction can be performed, but the extracting solution contains large amount of metallic ions causing environment pollution
Solution Approach 1:
The patent replaces metallic halide with food-grade phosphoric acid or other non-metallic acids for pH adjustment. These acids are cheaper, environmentally friendly, and do not introduce harmful metallic ions, resolving the pollution issue while maintaining pH adjustment capability.
Solution Approach 2:
The patent converts the harmful effect of metallic ion pollution into a beneficial process by using acidification to precipitate xanthophyll crystals. The acid treatment not only adjusts pH but also enables effective separation and purification, turning a potentially harmful step into a beneficial purification process.
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 process significantly increases the purity and yield of xanthophyll crystals, reducing environmental impact and enabling large-scale industrial production with improved efficiency and reduced water consumption.
Implementation Method 1
dissolving a plant extract containing a xanthophyll ester in n-hexane
Implementation Method 2
saponifying the mixed solution with an alkaline aqueous solution
Implementation Method 3
adding an acidic solution to the saponified solution until the mixed solution becomes acidic
Implementation Method 4
adding a mixed solvent of n-hexane, ethanol and acetone to the washed solid substance, and dissolve the solid substance with stirring; adding n-hexane to the mixture solution obtained in step i), standing at a temperature between 0-10° C. to obtain crystalline product
Data Source
AI summary
Disclosed a process for preparing a xanthophyll crystal, comprising: dissolving the plant extract containing a xanthophyll ester in n-hexane, then filtering the mixture; adding acetone to the filtrate, filtering and collecting a filter cake; mixing the filter cake with soybean oil and ethanol uniformly; saponifying the mixed solution with alkaline aqueous solution; then adding an acidic solution thereto until the mixed solution becomes acidic, concentrating under reduced pressure to obtain a pasty substance; adding n-hexane to the pasty saponified product, standing still and then conducting a solid-liquid separation; washing the resulting solid substance with deionized water; adding a mixed solvent to the washed solid substance, dissolving it with stirring; and then adding n-hexane thereto and standing still to recrystallize. According to the application, organic solvents are used to treat the plant extract and remove non-xanthophyll ester compounds in order to improve the efficiency of the saponification reaction; the saponified solution is concentrated under acidic condition at reduced pressure, then extracted with an organic solvent for saving water; purifying a xanthophyll crystal with a mixed solvent in order to significantly increase the purity of a xanthophyll crystal and proportion of trans-xanthophyll.