CN-121991397-A - Hyperbranched polyimide embedding material and preparation method and application thereof

CN121991397ACN 121991397 ACN121991397 ACN 121991397ACN-121991397-A

Abstract

The invention belongs to the technical field of high-performance polymer materials and advanced micro-encapsulation, and relates to a hyperbranched polyimide embedding material, a preparation method and application thereof. The method comprises the steps of dripping hyperbranched polyimide solution with the end group as an active group into a functional material to be embedded, and carrying out suction filtration and drying to obtain embedded powder. The obtained embedding powder is placed in a supercritical carbon dioxide device, and the swelling, plasticizing and extremely strong penetrating and diffusing capacities of hyperbranched polyimide with supercritical carbon dioxide as active groups are utilized by regulating temperature, pressure and time, so that a large number of pores are generated in the hyperbranched polyimide embedding material, the specific surface area of the material is increased, and finally the composite material with a porous structure, high embedding rate and well protected activity of functional substances is obtained. The hyperbranched polyimide embedding material prepared by the method can improve the stability of functional substances and the compatibility with an adding system.

Inventors

LI XIAODAN
HUANG WEI
ZHONG HONG
Zhou Chaozhi
JIANG YAO
DAI SHENGPING
LIU YUAN
JI ZHIGANG
LIN JUNCEN
WANG GUANHUI
PENG XUECHAO

Assignees

井冈山大学

Dates

Publication Date: 20260508
Application Date: 20260309

Claims (10)

1. The preparation method of the hyperbranched polyimide embedding material is characterized by comprising the following steps of: Dripping hyperbranched polyimide solution with a terminal group as an active group into an embedding functional material, and performing suction filtration and drying to obtain embedding powder; Placing the embedding powder in supercritical carbon dioxide fluid with the temperature of 31-80 ℃ and the pressure of 8-30 MPa for 0.5-6 hours to obtain a porous structure, regulating the reaction pressure to normal pressure at the depressurization rate of 0.1-2 MPa/min, and drying to obtain the hyperbranched polyimide embedding material; The hyperbranched polyimide with the end group as the active group is at least one of polyimide with hydroxyl group as the end group, polyimide with siloxane end-capped and polyimide with anhydride as the end group.
2. The method for preparing the hyperbranched polyimide embedding material according to claim 1, wherein the hyperbranched polyimide solution with the end group as the active group is prepared by dissolving hyperbranched polyimide with the end group as the active group in an organic solvent, the mass concentration of the hyperbranched polyimide solution with the end group as the active group is 1% -20%, and the organic solvent is at least one of N, N-dimethylacetamide, N-methylpyrrolidone or N, N-dimethylformamide.
3. The preparation method of the hyperbranched polyimide embedding material according to claim 1, wherein the mass percentage of the hyperbranched polyimide with the end group as the active group in the hyperbranched polyimide solution with the end group as the active group to the embedding functional material is 0.08% -1.5%.
4. The preparation method of the hyperbranched polyimide embedding material according to claim 1, wherein the treatment temperature of the embedding precursor in the supercritical carbon dioxide fluid is 35-60 ℃, the treatment pressure is 10-25 mpa, and the treatment time is 1-4 h.
5. The preparation method of the hyperbranched polyimide embedding material according to claim 1, wherein the depressurization rate is 1MPa/min, the drying temperature is 80-100 ℃, and the drying time is 2-5 h.
6. The method for preparing the hyperbranched polyimide embedding material according to claim 1, wherein the embedding functional material is one of a dye, a phase-change material, a catalyst or an antioxidant, wherein the antioxidant is at least one of an antioxidant 245, an antioxidant 1010 or an antioxidant 1076, the phase-change material is at least one of n-octadecane, n-tetracosane, n-eicosane or oxidized polyethylene wax, the catalyst is at least one of ferroferric oxide, vanadium pentoxide or zinc oxide, and the dye is at least one of ferric oxide, lead chromate or chromium oxide.
7. The hyperbranched polyimide embedding material according to any one of claims 1 to 6, which is prepared by a method for preparing the hyperbranched polyimide embedding material.
8. The hyperbranched polyimide embedding material according to claim 7, wherein the hyperbranched polyimide embedding material has a specific surface area of 10m2/g to 500m2/g.
9. The use of the hyperbranched polyimide embedding material according to claim 7 as filler or active ingredient for the preparation of composite films, functional coatings, drug delivery systems or phase change energy storage articles.
10. A composite comprising the hyperbranched polyimide embedding material of claim 7 or 8.

Description

Hyperbranched polyimide embedding material and preparation method and application thereof Technical Field The invention belongs to the technical field of high-performance polymer materials and advanced micro-encapsulation, and relates to a hyperbranched polyimide embedding material, a preparation method and application thereof. In particular to a hyperbranched polyimide embedding material prepared by using supercritical carbon dioxide fluid, a preparation method and application thereof. Background Embedding technology, or microencapsulation technology, is a technology that protects functional substances (e.g., catalysts, dyes, phase change materials, etc.) from environmental factors (e.g., high temperature, oxygen, humidity), and has urgent needs in the fields of electronics, aerospace, military and high-end manufacturing, etc. However, conventional embedding materials, such as conventional linear polymers or the aforementioned hyperbranched polyesters, often have difficulty in meeting the long-term use requirements under extreme conditions of high temperatures above 200 ℃, high mechanical stresses, or strong chemical corrosion. The research shows that the hyperbranched polyimide (HBPI) can meet the long-term use requirements under extreme conditions of high temperature above 200 ℃, high mechanical stress or strong corrosion and the like, is an ideal embedding carrier candidate material with good temperature resistance and processing performance, but the solution blending-evaporation method technology commonly adopted at present for preparing the hyperbranched polyimide (HBPI) material not only has the outstanding problem of solvent residue, but also ensures that the protective functional substance to be protected cannot be fully coated by the hyperbranched polyimide (HBPI) material, thereby influencing the application performance of the composite of the hyperbranched polyimide (HBPI) embedding material prepared by the method and other materials, such as the mechanical performance of the finally prepared composite material. Therefore, it is necessary to explore a preparation method of the hyperbranched polyimide embedding material. Disclosure of Invention Aiming at the defects of the prior art, the invention aims to provide the hyperbranched polyimide embedding material, and the preparation method and application thereof, wherein the preparation method has no outstanding solvent residue problem, so that the hyperbranched polyimide embedding material realizes stable encapsulation without affecting the composite performance of the hyperbranched polyimide embedding material and other materials. In order to solve the technical problems, the invention provides a preparation method of hyperbranched polyimide embedding material, which comprises the following steps of dripping hyperbranched polyimide solution with a terminal group as an active group into embedding functional material, and obtaining embedding powder through suction filtration and drying; Placing the embedding powder in supercritical carbon dioxide fluid with the temperature of 31-80 ℃ and the pressure of 8-30 MPa for 0.5-6 hours to obtain a porous structure, regulating the reaction pressure to normal pressure at the depressurization rate of 0.1-2 MPa/min, and drying to obtain the hyperbranched polyimide embedding material; The hyperbranched polyimide with the end group as the active group is at least one of polyimide with hydroxyl group as the end group, polyimide with siloxane end-capped and polyimide with anhydride as the end group. Preferably, the hyperbranched polyimide solution with the end group as the active group is prepared by dissolving hyperbranched polyimide with the end group as the active group in an organic solvent, the organic solvent is used in an amount that the mass concentration of the hyperbranched polyimide with the end group as the active group in the obtained solution is 1% -20% (namely, the concentration of the hyperbranched polyimide with the end group as the active group in the hyperbranched polyimide solution with the end group as the active group is 1% -20%), and the organic solvent is at least one of N, N-dimethylacetamide, N-methylpyrrolidone or N, N-dimethylformamide. The reason why the use amount of the organic solvent is that the mass concentration of the hyperbranched polyimide with the end group as the active group in the obtained solution is 1% -20% is that the use amount of the organic solvent is lower than 1%, the concentration of the hyperbranched polyimide with the end group as the active group is too high, the viscosity is too high, and the coating effect is too poor. Preferably, the mass percentage of the hyperbranched polyimide with the end group as the active group in the hyperbranched polyimide solution with the end group as the active group and the embedded functional material is 0.08-1.5%. The mass percentage of the hyperbranched polyimide with the end group as the active group in the hyperbranched pol