Cyclodextrin Metal-Organic Framework Rapid Synthesis

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Solution Overview

Problem

The long synthesis time of cyclodextrin-based metal-organic frameworks (CD-MOFs) hinders their large-scale industrial production due to harsh conditions and biotoxicity of traditional methods, limiting their application in biological and medicinal fields.

Innovation Solution

A method involving the formulation of a supersaturated γ-CD alkaline alcohol solution, heating, and controlled cooling to induce rapid crystallization and separation of CD-MOFs, reducing synthesis time from hours to minutes while maintaining biodegradability and high specific surface area.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If traditional self-assembly method is used to prepare CD-MOFs, then good biocompatibility and biodegradability are achieved, but synthesis time is too long (dozens of hours)

Engineering Contradiction:
ImprovebiocompatibilityVSAvoidsynthesis time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent prepares a supersaturated γ-CD alkaline alcohol solution in advance before the actual crystallization process. This preliminary preparation of the supersaturated solution enables the rapid crystallization to proceed much faster than traditional methods, reducing synthesis time from dozens of hours to just a few hours while maintaining the biocompatibility of the final CD-MOFs product

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes key parameters including using alkaline conditions (pH 12-14), supersaturated solution concentration, and alcohol-water mixed solvent system. These parameter changes create optimal conditions for rapid crystallization while preserving the biodegradability and biocompatibility characteristics of cyclodextrin-based materials

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If traditional synthesis conditions are used, then CD-MOFs with good crystallization are obtained, but harsh conditions (high temperature, organic solvents) are required

Engineering Contradiction:
Improvecrystallization qualityVSAvoidharsh synthesis conditions
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The patent uses mild alkaline conditions (pH 12-14) instead of strongly acidic or oxidizing conditions, and employs an alcohol-water mixed solvent system that is less harsh than traditional pure organic solvents. These parameter changes enable good crystallization quality while reducing the harmful effects of harsh synthesis conditions

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses readily available, inexpensive materials such as γ-cyclodextrin, common alcohols (methanol or ethanol), and alkali metal ions. These materials are biodegradable and environmentally friendly, replacing expensive or persistent organic ligands while achieving good crystallization quality

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

3Reliability

If traditional synthesis method is used, then CD-MOFs are prepared, but scale production is limited due to long reaction time

Engineering Contradiction:
ImprovebiodegradabilityVSAvoidscale production capability
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The preparation of supersaturated γ-CD alkaline alcohol solution before crystallization acts as a preliminary action that dramatically accelerates the overall process. This enables scale production by reducing the time bottleneck while maintaining the biodegradability of the CD-MOFs product through the use of cyclodextrin and biodegradable alkali metal ions

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent establishes a continuous process where the supersaturated solution is prepared and then immediately used for crystallization upon cooling. This continuous workflow eliminates idle time between steps, improving productivity for scale production while maintaining the environmentally friendly and biodegradable characteristics of the materials used

Inventive Principle:
Principle #20Continuity of useful 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

This method enables rapid, efficient, and environmentally friendly production of CD-MOFs with perfect crystallization and large specific surface area, suitable for industrial-scale production and broader applications, including biological and medicinal uses.

Implementation Method 1

inducing the γ-CD dissolution and crystallization behavior in solution via simply heating and cooling the γ-CD supersaturated alkaline alcoholic solution

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 2

inducing dissolution and crystallization behaviors of the γ-CD in the alcohol solution via simply controlling heating and cooling processes

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

heating to obtain a hot γ-CD solution; and cooling the hot γ-CD solution of the step (2), and performing crystallization and separation to obtain the CD-MOFs

Methodology Applied
Scientific EffectPhase change: Phase Change

Implementation Method 4

heating to obtain a hot γ-CD solution

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 5

cooling the hot γ-CD solution of the step (2), and performing crystallization and separation to obtain the CD-MOFs

Methodology Applied
Scientific EffectCooling: Cooling

Data Source

PatentUS20220282046A1Cyclodextrin-based metal organic framework material and preparation method therefor
Publication Date: 2022.09.08 SOUTH CHINA UNIV OF TECH
  • US20220282046A1 patent drawing

AI summary

The present disclosure belongs to the field of chemical industry production, and particularly relates to CD-MOFs and a preparation method thereof. The preparation method comprises the following steps: (1) formulating a supersaturated γ-cyclodextrin alkaline alcohol aqueous solution containing an alkali metal ion; (2) heating to obtain a hot γ-cyclodextrin solution; and (3) cooling the hot γ-cyclodextrin solution of the step (2), and performing crystallization and separation to obtain the cyclodextrin-based metal organic framework material. The CD-MOFs has perfect crystallization and large specific surface area, which are similar with those of a material prepared by means of traditional methods. The important thing is that the synthesis operation thereof is simple, green, and environmentally friendly, and the time required is shortened from a few hours or even tens of hours to a few minutes, which significantly improves the synthesis efficiency and is conductive to industrial scale production.