Metal-Organic Framework Synthesis Using Hydroxyl Solvents

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Solution Overview

Problem

Existing methods for synthesizing metal-organic frameworks (MOFs) are limited in completely removing solvent molecules bound to metal ions inside pores, which restricts the increase in surface area and gas adsorption capacity, particularly for carbon dioxide and carbon monoxide at room temperature.

Innovation Solution

A method involving the use of an organic solvent with a hydroxyl group, such as ethylene glycol, to synthesize MOFs, allowing for complete solvent removal through heat treatment without compromising crystallinity, resulting in a material with enhanced specific surface area and adsorption capacity for carbon dioxide and carbon monoxide.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If conventional synthesis methods are used to prepare metal-organic frameworks, then the framework structure is formed, but solvent molecules remain bound to metal ions inside pores preventing complete removal

Engineering Contradiction:
Improvegas adsorption capacityVSAvoidsolvent removal completeness
Core Design Contradiction:
Quantity of substanceVSReliability

Solution Approach 1:

The patent applies preliminary action by selecting a specific solvent (ethanol or methanol) for the synthesis step that facilitates complete removal. The solvent is chosen beforehand with the property that it can be completely removed through heat treatment, preventing residual solvent from blocking adsorption sites. This preliminary selection of appropriate synthesis conditions enables both framework formation and complete solvent removal.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent applies parameter changes by optimizing the synthesis parameters including solvent type (ethanol/methanol), metal salt concentration, and heating temperature (473K or higher). By changing these parameters, the synthesis process produces a framework where solvent molecules are loosely bound and can be completely removed through heat treatment, maximizing gas adsorption capacity.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If heat treatment is applied to remove solvent from pores, then solvent removal is achieved, but crystallinity is compromised

Engineering Contradiction:
Improvesolvent removal completenessVSAvoidcrystallinity
Core Design Contradiction:
ReliabilityVSStability of the object's composition

Solution Approach 1:

The patent applies parameter changes by precisely controlling the heating temperature range (473K or higher) and atmosphere conditions during heat treatment. By optimizing these parameters, the treatment is sufficient to completely remove solvent molecules but not excessive to damage the framework crystallinity. This parameter optimization resolves the contradiction between complete solvent removal and crystallinity preservation.

Inventive Principle:
Principle #35Parameter changes

3Quantity of substance

If surface area is increased to improve gas adsorption, then adsorption capacity improves, but solvent removal becomes more difficult

Engineering Contradiction:
Improvegas adsorption capacityVSAvoidsolvent removal difficulty
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The patent applies preliminary action by designing the synthesis process to create a framework with specific pore characteristics from the beginning. By selecting appropriate metal salts and organic ligands and using ethanol/methanol as synthesis solvent, the framework is formed with pore structures that allow easy solvent access and removal, even with high surface area. This preliminary design prevents solvent entrapment in high-surface-area structures.

Inventive Principle:
Principle #10Preliminary action

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 approach yields a highly crystalline MOF with a large surface area and improved adsorption characteristics for carbon dioxide and carbon monoxide, achieving up to 86 wt% carbon dioxide adsorption at saturation, surpassing the performance of similar MOFs.

Implementation Method 1

A metal-organic framework (MOF) refers to a 3-dimensional hollow porous crystalline material prepared from self-assembly of a metal ion and an organic ligand (linker)

Methodology Applied
Scientific EffectCoordination bonding: Chemical Bonding

Implementation Method 2

it is practically impossible to completely remove a solvent such as dimethylformamide (DMF) bound to the metal ions inside pores, for example, by heat treatment

Methodology Applied
Scientific EffectHeat treatment: Heating

Implementation Method 3

Being a hollow 3-dimensional material, it is known to superior gas adsorption characteristics due to large surface area

Methodology Applied
Scientific EffectAdsorption: Adsorption

Data Source

PatentUS9884308B2Metal-organic frameworks and process of preparing the same
Publication Date: 2018.02.06 KOREA INST OF ENERGY RES
  • US9884308B2 patent drawing
  • US9884308B2 patent drawing
  • US9884308B2 patent drawing

AI summary

The present disclosure relates to a metal-organic framework and a method for preparing the same. In accordance with the present disclosure, a metal-organic framework having large specific surface area can be prepared and the prepared porous material exhibits high carbon dioxide and carbon monoxide adsorption characteristics at room temperature.