Preparation method of novel acylhydrazone bond gel through one-step cross-linking polymerization

A technology of cross-linking polymerization and acylhydrazone bond is applied in the field of preparation of new cross-linking polymerization acylhydrazone bond gel to achieve high yield, good physical and chemical properties, cutting-edge design ideas and novel effects

Pending Publication Date: 2022-04-12
ZUNYI MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports in the literature on the rapid and direct synthesis of novel acylhydrazo

Method used

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  • Preparation method of novel acylhydrazone bond gel through one-step cross-linking polymerization
  • Preparation method of novel acylhydrazone bond gel through one-step cross-linking polymerization
  • Preparation method of novel acylhydrazone bond gel through one-step cross-linking polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesis of triethyl trimesate: Weigh 4.53 g (17.0 mmol) of 1,3,5-benzenetricarboxylic acid chloride in a 150 mL round bottom flask, add 50 mL of absolute ethanol and 5-8 drops of triethylamine, The reaction was stirred at room temperature for 6 h, and the reaction was stopped to obtain a white solid, which was filtered with suction, and then recrystallized with absolute ethanol and filtered to obtain white needle-shaped crystals; the synthetic route is as follows.

[0035]

Embodiment 2

[0037] Synthesis of trimesohydrazide: Weigh 1.47 g (5.0 mmol) of triethyl trimesate into a 150 mL round bottom flask, add 20 mL of 80% hydrazine hydrate, 30 mL of absolute ethanol and 30 mL of tetrahydrofuran, stir Heating under reflux for 6 h, distilling off ethanol under reduced pressure, cooling to precipitate a large amount of white solid, suction filtration, and then washing with a large amount of water until neutral, then recrystallizing the solid with absolute ethanol and filtering to obtain a white solid powder; its synthesis The route is shown below.

[0038]

Embodiment 3

[0040] Preparation of a new type of acylhydrazone bonded polymer gel (BTH-BD): Weigh 100.5 mg (0.4 mmol) of trimellitic hydrazide into a 10 mL glass vial, add 4.0 mL of DMSO solvent, and dissolve completely by ultrasonication for 10 min; then weigh Put 80.8 mg (0.6 mmol) of isophthalaldehyde in another 10 mL glass vial, add 4.0 mL DMSO solvent, and dissolve completely. Under ultrasound, the DMSO solution of isophthalaldehyde was slowly added dropwise to the DMSO solution of trimellitic hydrazide, and the mixed solution gradually changed from a cloudy solution to a light green transparent solution. gel state, and then transfer the newly prepared gel to an oven for heating and aging at 80 ºC for 12 h. After aging, take out the solvent in the vial, soak and wash the gel with 15-30 mL tetrahydrofuran for 24 h (3 times, exchange the solvent every 8 h); then soak and wash the gel with 15-30 mL absolute ethanol for 24 h ( 3 times, the solvent was exchanged every 8 h). Finally, free...

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Abstract

The invention provides a preparation method of novel acylhydrazone bond gel through one-step cross-linking polymerization. The method comprises the following steps: by taking 1, 3, 5-benzoyl chloride as an initial raw material, firstly reacting with absolute ethyl alcohol to generate triethyl trimellitate, and then reacting triethyl trimellitate with hydrazine hydrate to generate trimesoyl hydrazine. Finally, trimesoyl hydrazine and aldehyde are adopted as organic monomers to construct a module, and according to the Schiff base reaction principle, an acylhydrazone covalent bond is adopted as a cross-linking point, dimethyl sulfoxide is adopted as a solvent medium, and a series of novel acylhydrazone bond polymer gels are rapidly and directly synthesized at room temperature in one step. Compared with an existing preparation method of an acylhydrazone bond gel material, the novel acylhydrazone bond gel is completed through one-step cross-linking polymerization of organic monomers of hydrazide and aldehyde, the process that a gel factor is designed and synthesized firstly and then a cross-linking group is searched for in the existing acylhydrazone bond gel material is omitted, and the design idea of the novel acylhydrazone bond gel is more advanced and novel. The synthesis method disclosed by the invention is simple, low in cost, mild in condition, high in reaction rate and high in yield, and has good development and application potential in the aspect of intelligent materials.

Description

technical field [0001] The invention relates to a preparation method of a novel acylhydrazone bond gel of one-step cross-linking polymerization, which belongs to the field of polymer materials. Background technique [0002] Polymer gel is a gel system composed of a three-dimensional or interpenetrating network structure with unique physical and chemical properties and a large number of solvents formed by cross-linking polymer macromolecules. According to the cross-linking mode between polymer macromolecules, it can be divided into polymer physical gel and polymer chemical gel. Polymer physical gel is a cross-linked system formed by intermolecular forces (hydrogen bonds, van der Waals forces, etc.) etc.) have good responsiveness, and it is easy to realize the reversible transformation and self-healing process of sol-gel. The polymer chemical gel is a cross-linked structure formed by static covalent bonds between macromolecular chains as cross-linking points. It has high mec...

Claims

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Application Information

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IPC IPC(8): C08G12/08
Inventor 张成江李玉凰袁红梅卢泽毅
Owner ZUNYI MEDICAL UNIVERSITY
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