Preparation method of visible light curing self-repairing 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 halides, and can solve problems such as poor low temperature resistance and high brittleness of polyurethane resin

Active Publication Date: 2021-05-14
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Preparation method of visible light curing self-repairing fluorine-containing polyurethane resin
  • Preparation method of visible light curing self-repairing fluorine-containing polyurethane resin
  • Preparation method of visible light curing self-repairing fluorine-containing polyurethane resin

Examples

Experimental program
Comparison scheme
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 photocuring bio-based intelligent materials, and particularly relates to a preparation method of visible light curing self-repairing fluorine-containing polyurethane resin. The preparation method comprises the following steps: firstly, reacting dichloromethane, a double-active-functional-group photoinitiator, a weakly alkaline acid-binding agent and trifluoroacetyl chloride in a nitrogen protection device to prepare a fluorine-containing photoinitiator; and subjecting a hydrolysis product eleostearic acid of eleostearic acid triglyceride to dicarboxylation treatment. Under the synergistic effect of a dihydroxyl fluorine-containing monomer, a fluorine-containing photoinitiator and diisocyanate, the self-repairing fluorine-containing polyurethane resin cured under the visible light condition is finally prepared. The polyurethane resin overcomes the defects that traditional light-cured resin is large in brittleness, easy to damage and poor in high temperature resistance, visible light friendly to the human body is used for curing, the material has a self-repairing function, the service life of the material can be prolonged, the weather resistance and the high temperature resistance are enhanced, the monomer source 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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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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