High-Entropy COF Synthesis via Disposable Flame-Sealed Tubes
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Solution Overview
Problem
Traditional methods for preparing high-entropy covalent organic framework compounds often result in reduced crystallinity due to repeated container sealing, which affects the material's properties and synthesis efficiency.
Innovation Solution
A flame sealing tube method is used to mix five different monomers with a selected solvent, followed by ultrasound dispersion, vacuum treatment, and high-temperature hydrothermal synthesis in a customized glass tube, maintaining vacuum conditions to enhance crystallinity and slow crystal formation.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If traditional container sealing methods are used for repeated synthesis, then the preparation process can be repeated, but the sealing performance deteriorates and crystallinity is reduced
Solution Approach 1:
The patent employs disposable glass tubes that are sealed once and used for a single synthesis cycle. Each tube is flame-sealed to create a vacuum environment, then discarded after one use. This eliminates the cumulative degradation problem of reusable containers while maintaining high crystallinity throughout multiple synthesis repetitions.
2Productivity
If traditional container sealing methods are used, then the preparation process can be repeated, but the sealing performance and material quality deteriorate
Solution Approach 1:
The patent employs disposable glass tubes that are sealed once and used for a single synthesis cycle. Each tube is flame-sealed to create a vacuum environment, then discarded after one use. This eliminates the cumulative degradation problem of reusable containers while maintaining high crystallinity throughout multiple synthesis repetitions.
3Adaptability or versatility
If five monomers are mixed together, then high-entropy covalent organic framework is formed, but the synthesis complexity increases
Solution Approach 1:
The patent segments the synthesis process into distinct functional zones within a single reactor: monomer mixing zone, ultrasound dispersion zone, vacuum sealing zone, and hydrothermal reaction zone. This spatial and functional segmentation allows complex five-monomer synthesis to be managed through standardized sequential operations rather than complex simultaneous control.
Solution Approach 2:
The patent systematically varies key parameters including monomer ratios (aldehyde:amino = 1-5:1), solvent types, temperature ranges (80-150°C), and time durations (1-7 days) to optimize the high-entropy COF synthesis. These controlled parameter changes enable versatile compound formation through a unified synthesis platform.
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 effectively prepares high-entropy covalent organic framework compounds with high crystallinity, as evidenced by characteristic X-ray powder diffraction peaks and SEM images, demonstrating improved material quality and synthesis efficiency.
Implementation Method 1
vacuum flame sealing the reactor under a condition of vacuuming
Implementation Method 2
quickly sealing the glass tube with a flame gun
Implementation Method 3
performing an ultrasound treatment to make a powder of the trialdehyde phloroglucinol and the phenylenediamine monomers fully dispersed in the solvent
Implementation Method 4
reacting at 80° C.-150° C. for 1-7 d. In this step, exhausting excess air in the glass tube by a vacuum pump, making the material be synthesized under vacuum conditions to improve the crystallinity of the COF material
Implementation Method 5
high-temperature hydrothermal synthesis in a customized glass tube
Data Source
AI summary
A preparation method of a high-entropy covalent organic framework compound (COF) is provided, specifically, at room temperature under ultrasonic conditions, trialdehyde phloroglucinol (Tp), 2,5-dibromo-p-phenylenediamine, 2,5-dichloro-p-phenylenediamine, 2-(trifluoromethyl)-1,4-phenylenediamine and p-phenylenediamine are dispersed in the mixed solution of o-dichlorobenzene and n-butanol; the appropriate amount of acetic acid and deionized water are added to the above solution after ultrasonic dispersion; and vacuuming for 5 min under liquid nitrogen freezing conditions, then thawing, so cycle 3 times, and then reacting in an oven at 120° C. for 72 h. The prepared samples are washed with dichloromethane, and the samples are collected in a vacuum oven at 80° C. overnight. The technical scheme of the present invention is to rapidly generate crystalline substances insoluble in solvents under the condition of acetic acid and to obtain COF materials with high crystallinity and high specific surface area through 3 days of high-temperature preparation.