Trap Column Solvent Displacement for Rapid Water Removal

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Solution Overview

Problem

Conventional preparative separation/purification systems using liquid chromatographs face inefficiencies due to the long time required for vaporizing and drying processes, primarily because of the presence of water in the eluate, which slows down the solvent removal process.

Innovation Solution

A preparative separation/purification system that uses a trap column with a solvent of higher specific gravity and low solubility to displace and remove the initial solvent, such as water, allowing for efficient elution and collection of the target component without significant water content, utilizing a column-holding means and liquid supply means to manage the solvent exchange.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If water is used as the mobile phase to ensure complete capture of target component, then capture reliability is improved, but the vaporizing and drying process time increases significantly

Engineering Contradiction:
Improvecapture reliabilityVSAvoidvaporizing and drying process time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent segments the solvent removal process into two distinct stages: first removing water from the trap column using an organic solvent, then performing the vaporizing and drying process. This segmentation allows the water removal step to be completed efficiently before the time-consuming vaporizing step, thereby reducing the overall process time while maintaining capture reliability.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent applies preliminary action by removing water from the trap column before the vaporizing and drying process. The organic solvent is introduced to displace and remove water in advance, so that when the vaporizing step occurs, only minimal water remains, significantly reducing the time required for solvent removal while ensuring complete capture of the target component.

Inventive Principle:
Principle #10Preliminary action

2Speed

If organic solvent is used to elute target component quickly, then elution speed is improved, but water content in the eluate increases

Engineering Contradiction:
Improveelution speedVSAvoidwater content in eluate
Core Design Contradiction:
SpeedVSQuantity of substance

Solution Approach 1:

The patent uses an organic solvent as an intermediary substance to remove water from the trap column before elution. This intermediary organic solvent displaces the water through immiscibility and density differences, allowing rapid water removal without contaminating the subsequent eluate with significant water content, thus achieving both fast elution and low water content.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If trap column is washed with water to remove salts, then purity is improved, but the amount of water remaining in the column increases

Engineering Contradiction:
ImprovepurityVSAvoidwater amount in trap column
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent extracts water from the trap column using an organic solvent that is immiscible with water. The organic solvent selectively removes water from the column through displacement, allowing complete water extraction while maintaining the purity benefits of water washing. This extraction process eliminates the trade-off between purity and water content by removing water in a separate, controlled step.

Inventive Principle:
Principle #2Taking out (Extraction)

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 approach significantly reduces the time needed to remove water and other solvents from the trap column, resulting in a water-free eluate that can be quickly vaporized to obtain the target component in solid form, thereby enhancing the process throughput.

Implementation Method 1

the second solvent having a specific gravity greater than the specific gravity of a first solvent remaining in the trap column

Methodology Applied
Scientific EffectDensity gradient: Density Gradient

Implementation Method 2

the first solvent is removed from the trap column by disposing of the first solvent extruded from the discharge end of the trap column by being pushed by the second solvent supplied to the trap column by the liquid supply means

Methodology Applied
Scientific EffectLiquid displacement:

Implementation Method 3

a solution containing a target component is passed through a trap column to capture the target component in the trap column

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 4

These separately collected solutions are then subjected to a vaporizing and drying process to remove the solvent and collect the target components in solid forms

Methodology Applied
Scientific EffectVaporization: Evaporation

Data Source

PatentUS8607620B2Preparative separation/purification system
Publication Date: 2013.12.17 SHIMADZU CORP
  • US8607620B2 patent drawing
  • US8607620B2 patent drawing
  • US8607620B2 patent drawing

AI summary

After a target compound is captured by an adsorbent within a trap column (7) held by a column rack (8) in a substantially vertical position and the column is filled with water to wash its inside, dichloromethane is slowly introduced from an inlet end (7a) on the lower side by a pump (5). The water within the trap column (7) is pushed upward by dichloromethane and exits from an outlet end (7b), to be disposed of via a two-way selector valve (12) and a disposal passage (14). Dichloromethane elutes the captured target compound. Therefore, when the eluate, which initially consists of water, changes via an emulsion to dichloromethane, the eluate contains an adequately high concentration of target compound. At this point, the two-way valve (12) is switched to a preparative separation passage (13). As a result, a solution that is adequately free from water and yet contains the target compound can be collected into a collection container (17), and the target compound in solid forms can be quickly obtained.