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Synthesis method and application of unsaturated hyperbranched polyimide resin

A technology of polyimide resin and synthesis method, applied in coating and other directions, can solve the problems of difficulty in reducing the amount of diluent, high molecular weight of polyimide, uncontrollable degree of branching, etc., and achieves excellent processing and molding performance, high Solubility, avoid gelation effect

Inactive Publication Date: 2018-08-24
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are existing synthetic methods about hyperbranched polyimide trees, such as "A" published by Ren Jie et al. 2 +B'B 2 A 2 and B or B 4 As a monomer, a series of hyperbranched polyimides were synthesized through a one-step reaction, but this synthesis method cannot control the degree of branching, and it is easy to gel directly during the preparation process, resulting in too high molecular weight of polyimides, which is difficult to reduce The amount of diluent

Method used

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  • Synthesis method and application of unsaturated hyperbranched polyimide resin
  • Synthesis method and application of unsaturated hyperbranched polyimide resin
  • Synthesis method and application of unsaturated hyperbranched polyimide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Get 2mol 1,3,5-tri(4-aminophenoxy)benzene and 2mol pyromellitic dianhydride and place it in a four-necked flask equipped with a mechanical stirrer, a reflux condenser, a drying tube and an airway tube, and then add 20ml of tetrahydrofuran, stirred and mixed evenly, under nitrogen atmosphere, stirred and heated to 80°C for 2h reaction to obtain triphenoxyphenylenediaminophthalic acid monomer.

[0027] Add 30ml of N-methylpyrrolidone as a solvent and 2ml of pyridine as a catalyst to triphenoxyphenylenediaminophthalic acid monomer, raise the temperature to 120°C in the first stage, reflux for 2 hours, then raise the temperature to 180°C in the second stage for reflux reaction After 5h, the amino terminal hyperbranched resin was obtained. Then, after cooling the entire reaction system to room temperature, add 0.002 mol of free radical inhibitor hydroquinone and 0.2 mol of end-capping agent acryloyl chloride, and then continue to react at room temperature for 2 hours. After ...

Embodiment 2

[0033]Take 2mol melamine and 2mol cyclobutene tetra-acid dianhydride and place in a four-necked flask equipped with a mechanical stirrer, a reflux condenser, a drying tube and an airway tube, then add 10ml of m-cresol, stir and mix evenly, and place the mixture in a nitrogen atmosphere. , stirring and raising the temperature to 120° C. for 1 h to obtain a triazine-based diaminocyclobutenedioic acid monomer.

[0034] Add 1 mL of catalyst quinoline to the triazine-based diaminocyclobutene dioic acid monomer, heat up to 200° C. and reflux for 12 hours to obtain an amino-terminated hyperbranched resin. Then, after the whole reaction system was cooled to room temperature, 0.001 mol of free radical inhibitor p-methylhydroquinone and 0.1 mol of capping agent maleic anhydride were added, and then heated to 120° C. to continue the reaction for 1 h. After the reaction was completed, the The organic solvent was recovered by distillation under reduced pressure (vacuum degree 0.05 MPa) at ...

Embodiment 3

[0039] Take 2.5mol 2,4,6-tris(N-p-aminophenyl)-1,3,5-triazine and 2.5mol4,4'-(hexafluoroisopropylpropyl)-diphthalic anhydride In a four-necked flask equipped with a mechanical stirrer, a reflux condenser, a drying tube and an airway tube, 15ml of N-methylpyrrolidone was then added, and after stirring and mixing evenly, the reaction was stirred at room temperature for 6 hours under a nitrogen atmosphere to obtain triphenyl Triazinyl dihydrophthalic acid monomer.

[0040] Add 0.1 g of catalyst triphenyl phosphite and 0.2 g of calcium chloride to the triphenyltriazine-based dihydrophthalic acid monomer, raise the temperature to 120°C for 12 hours under reflux in the first stage, and raise the temperature in the second stage to Reflux reaction at 180°C for 8 hours, and in the third stage, the temperature was raised to 200°C for reflux reaction for 4 hours to obtain an amino-terminal hyperbranched resin. Then, after the whole reaction system was cooled to room temperature, 0.001 m...

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Abstract

The invention discloses a synthesis method and application of an unsaturated hyperbranched polyimide resin. The synthesis method comprises the following steps: 1) preparing a monomer, namely uniformlymixing raw materials, namely aromatic tertiary amine A3 and a dianhydride compound B2, adding a high-melting point solvent, and performing a reaction under a set condition so as to obtain an A2B typefunctional monomer; 2) performing a polymerization reaction, namely putting a catalyst into the A2B type functional monomer prepared in the step 1), performing a self-polycondensation reaction so asto obtain a yperbranched resin at the tail end of amino, further adding a free radical polymerization inhibitor and an end-capping reagent, performing a quenching reaction, controlling a branching degree, and performing reduced pressure distillation, thereby obtaining the unsaturated hyperbranched polyimide resin HP-PI. The polyimide resin prepared by using the synthesis method is relatively low in viscosity, good in solubleness, capable of effectively reducing the amount of diluents in the process that an insulating impregnating varnish is prepared, the cost can be reduced, and the toxicity can be degraded.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and in particular relates to a synthesis method and application of an unsaturated hyperbranched polyimide resin. Background technique [0002] Insulating impregnating varnish is a kind of impregnation treatment for the electrical coils of motors through infiltration, so that they are filled into the gaps and pores of coils, wire slots or other insulated objects, and after curing, the coil wires are bonded into an insulating whole, so as to A liquid resin system that provides dielectric, mechanical and environmental protection properties. In recent years, as the European Union and the United States have gradually increased their environmental protection requirements for exporting electronic products, my country's solvent-free and less-solvated impregnating varnish industry has gradually grown and has become an important part of the impregnating varnish. [0003] Commercially av...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08G73/12C09D5/25C09D179/08
CPCC08G73/1007C08G73/1067C08G73/1071C08G73/1085C08G73/128C09D5/00C09D179/08C09D179/085
Inventor 喻桂朋张步峰潘春跃
Owner CENT SOUTH UNIV
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