Supercritical CO2 Extraction of Non-Volatile Organic Molecules

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Solution Overview

Problem

Current methods for extracting and analyzing organic molecules from solid samples, such as soil, are inefficient, often requiring harsh conditions that lead to molecule degradation, and are not suitable for in situ analysis or low sample quantities, especially for non-volatile molecules.

Innovation Solution

A process involving thermo-desorption, functionalization, and volatilization of organic molecules under controlled temperature and pressure conditions, allowing for rapid extraction and analysis of non-volatile molecules without degradation, using a sample preparation device that can be used in situ.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If traditional solid-liquid extraction methods are used, then extraction completeness is improved, but extraction time increases significantly and equipment complexity increases

Engineering Contradiction:
Improveextraction completenessVSAvoidextraction time
Core Design Contradiction:
Quantity of substanceVSLoss of time

Solution Approach 1:

The patent uses supercritical fluid extraction where CO2 transitions to a supercritical state under high pressure and temperature to extract compounds, then returns to gaseous state for easy removal. This phase transition enables complete extraction without long soaking times required by traditional liquid-solid methods.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent changes physical parameters (pressure and temperature) to create supercritical conditions. By adjusting P>73 atm and T>31°C, the extraction medium achieves enhanced solubility and diffusion properties, enabling rapid and complete extraction without prolonged contact time.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If harsh extraction conditions are applied to strongly bound molecules, then extraction efficiency is improved, but molecule degradation increases

Engineering Contradiction:
Improveextraction efficiencyVSAvoidmolecule degradation
Core Design Contradiction:
ProductivityVSObject-affected harmful factors

Solution Approach 1:

The supercritical fluid provides enhanced penetrability and solubility without requiring harsh chemical conditions. The tunable solvent power of supercritical CO2 allows efficient extraction of strongly bound molecules while maintaining gentle conditions that preserve molecular integrity.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

By precisely controlling pressure and temperature parameters within specific ranges, the patent achieves optimal extraction efficiency while avoiding excessive heat or chemical harshness that would cause degradation. The supercritical state provides enhanced extraction capability without the downsides of traditional harsh methods.

Inventive Principle:
Principle #35Parameter changes

3Quantity of substance

If conventional extraction equipment is used, then extraction capability is improved, but device portability and in situ applicability worsen

Engineering Contradiction:
Improveextraction capabilityVSAvoiddevice portability
Core Design Contradiction:
Quantity of substanceVSEase of operation

Solution Approach 1:

The use of supercritical CO2 enables a compact extraction system because CO2 can be easily pressurized and depressurized in small-scale devices. The phase transition from supercritical to gaseous state allows for simple solvent removal without large evaporation vessels, enhancing device portability.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent employs a disposable or easily replaceable extraction cartridge containing the adsorbent material. This allows the main equipment to remain compact and portable while the consumable component handles the extraction, facilitating in situ applications.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

4Measurement precision

If large sample quantities are processed, then analysis representativeness is improved, but sample preparation complexity and equipment requirements increase

Engineering Contradiction:
Improveanalysis representativenessVSAvoidsample preparation complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The supercritical fluid extraction efficiently processes samples regardless of quantity because the supercritical state provides enhanced mass transfer and penetration. Small samples are adequately represented, and the method scales to larger samples without requiring proportionally larger or more complex equipment.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The extraction system is designed to handle a wide range of sample quantities and types using the same basic apparatus. The supercritical extraction method and adsorbent-based concentration approach provide universal applicability from trace to bulk samples.

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 effectively extracts and volatilizes organic molecules with high recovery yields, preserving their quality and allowing for quantitative analysis, even in low sample quantities, and is suitable for in situ analysis.

Implementation Method 1

raising the temperature of the sample from the environmental temperature to a temperature Td ranging from 250°C to 600°C

Methodology Applied
Scientific EffectThermal energy heating: Heating

Implementation Method 2

adding to the sample at least one functionalization agent and at least one organic solvent, and maintaining the sample at the temperature Tf for a period Df of less than 1 hour

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 3

heating the sample to a temperature Tv ranging from 140°C to 300°C for a duration Dv of less than 1 hour, which causes volatilization of the functionalized organic molecules

Methodology Applied
Scientific EffectVolatilization: Evaporation

Data Source

PatentEP2252886B1Method for the extractive functionalizing of organic compounds
Publication Date: 2017.07.05 CENT NAT DETUD SPATIALES (CNES)
  • EP2252886B1 patent drawingFigure 1
  • EP2252886B1 patent drawingFigure 2~3
  • EP2252886B1 patent drawingFigure 4~5

AI summary

A method for extracting, functionalizing, and volatilizing non-volatile organic molecules present in a solid medium, and which includes the following steps: (a) taking a solid soil sample; (b) placing the sample under a pressure Pd of 0.1 to 200 kPa; (c) raising the temperature of the sample in less than 30 seconds from ambient temperature to a temperature Td of 250°C to 600°C; (d) keeping the sample at the temperature Td during a duration Dd of less than 15 minutes; (e) reducing the temperature of the sample in less than 30 seconds from the temperature Td to the temperature Tf of 50°C to 100°C; (f) adding at least one functionalizing agent and at least one solvent to the sample, and keeping the mixture at the temperature Tf for a duration Dd of less than one hour; and (g) heating the sample to a temperature Tv of 140°C to 300°C for a duration Dv of less than one hour.