Dehydration-Rehydration Synthesis for Microporous Crystal Membranes

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Solution Overview

Problem

Current hydrothermal processes for synthesizing microporous crystals, such as zeolites, are slow and costly, limiting the feasibility of rapid and cost-effective production of microporous crystal membranes for applications like CO2 capture.

Innovation Solution

A dehydration-rehydration synthesis protocol is employed, where a gel is first dehydrated to induce crystal nucleation and then rehydrated with a controlled water addition rate to accelerate the crystallization of microporous crystals, allowing for the rapid synthesis of microporous crystal membranes compatible with polymer roll-to-roll technology.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional hydrothermal processes are used for synthesizing microporous crystals, then the crystallization can proceed with standard conditions, but the crystallization time is long and production cost is high

Engineering Contradiction:
Improvecrystallization speedVSAvoidcrystallization time
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent applies preliminary action by removing water from the gel before crystallization to pre-concentrate the reactants and create a more favorable environment for rapid crystal growth. This pre-treatment step prepares the system in advance to accelerate the subsequent crystallization process, reducing overall synthesis time from days to hours.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes key parameters of the synthesis process by controlling water removal and addition rates, temperature profiles, and pH conditions. By dynamically adjusting these parameters—particularly the water activity during gel drying and the controlled rehydration rate—the crystallization kinetics are enhanced, achieving faster crystal growth while maintaining quality.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If water is removed rapidly from the gel, then crystallization may be accelerated, but uncontrolled water removal can lead to poor crystal quality and morphology

Engineering Contradiction:
Improvecrystallization speedVSAvoidcrystal quality
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent employs feedback control by monitoring the water removal rate and adjusting the drying conditions accordingly. The controlled water removal process maintains optimal moisture content to prevent premature cracking or deformation of the gel structure, ensuring that crystals develop with good quality and uniform morphology while still achieving accelerated crystallization.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent applies dynamics by using a controlled, dynamic water removal and addition process rather than static conditions. The water is removed at a controlled rate and then added back at a specific rate (0.5-2.0 fold the removal rate) to dynamically adjust the gel's water activity, creating optimal conditions for both rapid crystallization and high crystal quality throughout the process.

Inventive Principle:
Principle #15Dynamics

3Productivity

If the water addition rate during rehydration is too high, then the crystallization process speeds up, but the crystal morphology and quality deteriorate

Engineering Contradiction:
Improvecrystallization speedVSAvoidcrystal morphology
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent optimizes the water addition rate parameter during rehydration to achieve the best balance between crystallization speed and crystal quality. By controlling the water addition rate to be 0.5-2.0 fold the removal rate, the process maintains optimal supersaturation levels that promote rapid yet controlled crystal growth, preserving good morphology while achieving fast production.

Inventive Principle:
Principle #35Parameter changes

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 significantly reduces the crystallization time of microporous crystals, enabling the production of high-quality microporous crystal membranes within the hour time scale, aligning with polymer roll-to-roll fabrication constraints and offering a cost-effective solution for industrial applications.

Implementation Method 1

heating the gel for a first time period, whereupon a first volume of water is removed from the gel

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

heating the gel for a second time period, during which a second volume of water is added to the gel

Methodology Applied
Scientific EffectAbsorption: Absorption (physical)

Implementation Method 3

heating the gel for a first time period, whereupon a first volume of water is removed from the gel and microporous crystal nuclei form

Methodology Applied
Scientific EffectNucleation: Nucleation

Data Source

PatentUS9561477B2Methods for synthesizing microporous crystals and microporous crystal membranes
Publication Date: 2017.02.07 OHIO STATE INNOVATION FOUND
  • US9561477B2 patent drawing
  • US9561477B2 patent drawing
  • US9561477B2 patent drawing

AI summary

A method of making a microporous crystal material, comprising: a. forming a mixture comprising NaOH, water, and one or more of an aluminum source, a silicon source, and a phosphate source, whereupon the mixture forms a gel; b. heating the gel for a first time period, whereupon a first volume of water is removed from the gel and micoroporous crystal nuclei form, the nuclei having a framework; and c.(if a membrane is to be formed) applying the gel to a solid support seeded with microporous crystals having a framework that is the same as the framework of the nuclei; d. heating the gel for a second time period. during which a second volume of water is added to the gel; wherein the rate of addition of the second volume of water is between about 0.5 and about 2.0 fold the rate of removal of the first volume of water.