A kind of preparation method of visible light curing self-healing fluorine-containing polyurethane resin

A polyurethane resin and self-repairing technology, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of carboxylic acid amides, can solve the problems of high brittleness and poor low temperature resistance of polyurethane resin, and achieve enhanced tensile strength and heat resistance performance, improved service life and safety factor, and good self-repair function

Active Publication Date: 2022-03-04
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a preparation method of visible light-cured self-repairing fluorine-containing polyurethane resin, which solves the problems of high brittleness and poor low temperature resistance of polyurethane resin

Method used

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  • A kind of preparation method of visible light curing self-healing fluorine-containing polyurethane resin
  • A kind of preparation method of visible light curing self-healing fluorine-containing polyurethane resin
  • A kind of preparation method of visible light curing self-healing fluorine-containing polyurethane resin

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add 20 mL of dichloromethane into a three-necked flask equipped with nitrogen protection and a magnetic stirring device, and 0.01 mol of 1,1'-(methylenebis-4,1-phenylene)bis[2-hydroxy-2-methyl -1-acetone] and 0.01mol triethylamine were dissolved in dichloromethane, and magnetically stirred at room temperature to make them mix uniformly. After reacting for 2 hours, the temperature was rapidly lowered, and 15 mL of dichloroethane and 0.02 mol of trifluoroacetyl chloride were slowly added to the reaction vessel in an ice-water bath, and the reaction temperature was controlled at 5°C. After reacting for 6 hours, filtered, washed and dried to obtain Fluorinated photoinitiator, the yield is 86%.

[0046]Add 0.01mol oleic acid triglyceride and 0.03mol 10% sodium hydroxide solution to a 100mL round bottom flask, heat to make it fully react for 50min, then separate the liquids, wash the oil layer with excess 0.5mol / L sulfuric acid, and then divide it with 30mL saturated NaCl sol...

Embodiment 2

[0052] Add 30 mL of dichloromethane into a three-necked flask equipped with nitrogen protection and a magnetic stirring device, and 0.02 mol of 1,1'-(methylenebis-4,1-phenylene)bis[2-hydroxy-2-methyl -1-acetone] and 0.02mol n-butylamine were dissolved in dichloromethane, and magnetically stirred at room temperature to mix them evenly. After 2 hours of reaction, the temperature was rapidly lowered, and 20 mL of dichloroethane and 0.04 mol of trifluoroacetyl chloride were slowly added to the reaction vessel in an ice-water bath. The fluorine-containing photoinitiator was obtained with a yield of 88%.

[0053] Add 0.02 mol oleic acid triglyceride and 0.06 mol 10% sodium hydroxide solution to a 100 mL round-bottomed flask, heat to make it fully react for 50 min, then separate the liquids, wash the oil layer with an excess of 0.5 mol / L sulfuric acid, and then separate with 30 mL saturated NaCl solution. After washing three times and drying, unsaturated oleic acid can be obtained (...

Embodiment 3

[0058] Add 35 mL of dichloromethane into a three-necked flask equipped with nitrogen protection and a magnetic stirring device, and 0.03 mol of 1,1'-(methylenebis-4,1-phenylene)bis[2-hydroxy-2-methyl -1-acetone] and 0.03mol trimethylamine were dissolved in dichloromethane, and magnetically stirred at room temperature to make them mix uniformly. After 2 hours of reaction, the temperature was rapidly lowered, and 25 mL of dichloroethane and 0.06 mol of trifluoroacetyl chloride were slowly added to the reaction vessel in an ice-water bath. The fluorine-containing photoinitiator was obtained with a yield of 89%.

[0059] Add 0.03 mol oleic acid triglyceride and 0.09 mol 10% sodium hydroxide solution to a 100 mL round-bottomed flask, heat to make it fully react for 50 min, then separate the liquids, wash the oil layer with an excess of 0.5 mol / L sulfuric acid, and then separate with 30 mL saturated NaCl solution. After washing three times and drying, unsaturated oleic acid can be ...

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Abstract

The invention belongs to the field of light-curing bio-based intelligent materials, and in particular relates to a preparation method of visible light-curing self-repairing fluorine-containing polyurethane resin. First use dichloromethane, dual active functional group photoinitiator, weakly basic acid-binding agent and trifluoroacetyl chloride to react in a nitrogen protection device to prepare a fluorine-containing photoinitiator; Dicarboxylation treatment, under the synergistic action of dihydroxy fluorine-containing monomer, fluorine-containing photoinitiator and diisocyanate, finally prepares self-healing fluorine-containing polyurethane resin cured under visible light conditions. The polyurethane resin of the present invention overcomes the shortcomings of traditional light-curing resins such as high brittleness, easy damage, and poor high temperature resistance. It is cured by visible light that is friendly to the human body, and the material has a self-repairing function, which can prolong the service life of the material and enhance weather resistance and high temperature resistance. properties, the source of the monomer is renewable, and the application prospect is good.

Description

technical field [0001] The invention belongs to the field of light-curing bio-based intelligent materials, and in particular relates to a preparation method of visible light-curing self-repairing fluorine-containing polyurethane resin. Background technique [0002] Photocurable resins are widely used in 3D printing, artificial bones, special coatings, adhesives and other fields because of their fast curing speed, very little organic volatile matter, low cost, and easy operation. However, traditional light-curing resins are cured by ultraviolet light, which requires special equipment to generate ultraviolet radiation, and such equipment is expensive, and the ultraviolet rays produced are harmful to the human body. [0003] Due to its excellent properties such as friction resistance, low temperature resistance, microphase separation, and controllable hardness and softness, polyurethane is widely used in aviation, railways, auto parts, coatings and other fields. However, polyu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/68C08G63/682C08G63/48C08F299/06C08F2/48C07C67/14C07C69/63C07C233/33C07C231/02C07C233/43
CPCC08G18/68C08G63/6828C08G63/48C08F299/06C08F2/48C07C231/02C07C67/14C07C69/63C07C233/33C07C233/43
Inventor 冯苛玉李宁王璐瑶殷鹏李海松樊玲璐张承诺康帝潘雨琪李淼龙
Owner CHANGZHOU UNIV
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