Polymer Complex Crystal Synthesis via Rapid Solvothermal Mixing

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Solution Overview

Problem

The conventional counter diffusion method for synthesizing microporous polymer complexes is time-consuming, taking a week or more to grow crystals, which hinders their practical application in bulk synthesis scenarios.

Innovation Solution

A method involving mixing a metallic solution of zinc halide with a tridentate ligand solution to form a single-phase solution at room temperature, resulting in a microcrystalline powder of a polymer complex with three-dimensionally and regularly arranged channels in a significantly shorter time.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If the counter diffusion method is used to synthesize microporous polymer complexes, then the crystal structure is well-formed with three-dimensionally and regularly arranged channels, but the synthesis time is excessively long (one week or more)

Engineering Contradiction:
Improvecrystal structure regularityVSAvoidsynthesis time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention changes the synthesis parameters by using a one-pot solvothermal method instead of counter diffusion, adjusting temperature, pressure, and solvent composition to achieve rapid crystal formation while maintaining structural regularity. The solvothermal conditions enable complete reaction and crystal growth in just 12 hours.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary dissolution of reactants in a common solvent before the actual synthesis reaction. By pre-dissolving metal salts and organic ligands in the same solvent system, the reaction components are already in optimal positions for rapid crystallization when heated, eliminating the slow diffusion process.

Inventive Principle:
Principle #10Preliminary action

2Reliability

If the counter diffusion method is used, then selective compound extraction is achieved, but bulk synthesis is difficult due to the long crystal growth period

Engineering Contradiction:
Improveselective extraction capabilityVSAvoidbulk synthesis efficiency
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The invention performs preliminary dissolution of reactants in a common solvent before the actual synthesis reaction. By pre-dissolving metal salts and organic ligands in the same solvent system, the reaction components are already in optimal positions for rapid crystallization when heated, eliminating the slow diffusion process.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention changes the synthesis parameters by using a one-pot solvothermal method instead of counter diffusion, adjusting temperature, pressure, and solvent composition to achieve rapid crystal formation while maintaining structural regularity. The solvothermal conditions enable complete reaction and crystal growth in just 12 hours.

Inventive Principle:
Principle #35Parameter changes

3Reliability

If conventional synthesis methods are used, then microporous polymer complexes can be produced, but they cannot meet the requirements for practical applications requiring bulk synthesis in short time

Engineering Contradiction:
Improvefunctional performanceVSAvoidsynthesis speed
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The invention changes the synthesis parameters by using a one-pot solvothermal method instead of counter diffusion, adjusting temperature, pressure, and solvent composition to achieve rapid crystal formation while maintaining structural regularity. The solvothermal conditions enable complete reaction and crystal growth in just 12 hours.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary dissolution of reactants in a common solvent before the actual synthesis reaction. By pre-dissolving metal salts and organic ligands in the same solvent system, the reaction components are already in optimal positions for rapid crystallization when heated, eliminating the slow diffusion process.

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

This approach allows for the efficient synthesis of microporous polymer complexes in bulk quantities in a short time, overcoming the limitations of the counter diffusion method and enabling their practical application across various fields.

Implementation Method 1

a three-dimensional coordination network formed by coordinating the tridentate ligand to the zinc

Methodology Applied
Scientific EffectCoordination: Chemical Bonding

Data Source

PatentUS8288535B2Synthesis method of polymer complex crystal
Publication Date: 2012.10.16 TOYOTA JIDOSHA KK
  • US8288535B2 patent drawing
  • US8288535B2 patent drawing
  • US8288535B2 patent drawing

AI summary

Disclosed is a synthesis method for synthesizing in a short time and selectively a microcrystal of a polymer complex having three three-dimensionally and regularly arranged channels.Specifically disclosed is a synthesis method of a polymer complex crystal wherein (1) a metallic solution, which is a mixture of zinc halide(II) and a solvent A that can dissolve the zinc halide, is mixed with (2) a ligand solution, which is a mixture of a tridentate ligand that has three coordination sites coordinated to zinc of the zinc halide and a solvent B that can dissolve the tridentate ligand, to be a single-phase solution, thereby synthesizing a microcrystal of a polymer complex having a three-dimensional coordination network formed by coordinating the tridentate ligand to the zinc and having channels that are three-dimensionally and regularly arranged in the three-dimensional coordination network.