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Method for preparing polyimide-silicon dioxide composite nanofiber membrane with crosslinking morphology

A technology of composite nanofibers and silica, applied in fiber processing, filament/thread forming, textile and papermaking, etc. Interaction and other issues, to achieve the effects of process-based and industrialized preparation, improved mechanical strength and dimensional stability, and easy operation

Active Publication Date: 2016-09-28
启鼎技术(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, since the polyimide fiber membrane prepared by the traditional electrospinning method is usually a non-woven structure, the fibers of the fiber membrane are only loosely packed together without strong interaction, and the porosity and pore size are relatively large. , so the mechanical properties of the fiber membrane are usually very poor, which does not reflect the excellent properties of polyimide itself, especially the mechanical properties of high strength and high modulus

Method used

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  • Method for preparing polyimide-silicon dioxide composite nanofiber membrane with crosslinking morphology
  • Method for preparing polyimide-silicon dioxide composite nanofiber membrane with crosslinking morphology
  • Method for preparing polyimide-silicon dioxide composite nanofiber membrane with crosslinking morphology

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Effect test

Embodiment 1

[0040] Use pyromellitic dianhydride (PMDA) and 4,4'-diaminodiphenyl ether (ODA) as dibasic anhydride and diamine monomer respectively, and N,N-dimethylformamide (DMF) as solvent , polycondensation to obtain a polyamic acid solution, the solid content is 12%, the quality of the silicon dioxide precursor added is 40% of the quality of the polyimide generated after imidization, and the quality of the silicon dioxide finally generated after all the reactions , the polyamic acid / silicon dioxide precursor nanofiber membrane was prepared by electrospinning method, and the subsequent treatment process was (a) direct high-temperature thermal imidization without hydrolysis treatment, and the temperature was raised from room temperature to 300 ° C at a uniform speed for 120 minutes , and keep it warm for 120min; (b) heat imidization at high temperature first, heat up from room temperature to 300°C at a constant speed for 120min, keep it warm for 120min, hang it in a sealed 650mL container...

Embodiment 2

[0042] Using PMDA and ODA as dibasic anhydride and diamine monomers respectively, and DMF as solvent, polyamic acid solution is polycondensed, with a solid content of 12%. The quality of silicon oxide accounts for 40% of the mass of polyimide after imidization, and the polyamic acid / silicon dioxide precursor nanofiber film is prepared by electrospinning, and the subsequent treatment processes are (a) at 120 ° C Insulate for 60 minutes, hang it in a sealed 650mL container with 40mL of mixed hydrolyzate after cooling, take it out after insulated at 65°C for 12h, heat imidize, heat up from room temperature to 300°C at a constant speed for 120min, and keep warm for 60min; ( b) Insulate at 120°C for 60 minutes, hang it in a sealed 650mL container with 40mL of mixed hydrolyzate after cooling, take it out after heat preservation at 65°C for 36h, heat imidization, and heat up from room temperature to 300°C at a constant speed over 120 minutes , and keep warm for 60min. The morphology...

Embodiment 3

[0044] Using PMDA and ODA as dibasic anhydride and diamine monomers respectively, and DMF as solvent, polyamic acid solution is polycondensed, with a solid content of 12%. The mass of silicon oxide accounts for 40% of the mass of polyimide produced after imidization, and the polyamic acid / silicon dioxide precursor nanofiber film is prepared by electrospinning, and the subsequent treatment processes are (a) at 120 °C Insulate for 60 minutes at low temperature, hang it in a sealed 650mL container with 35mL of mixed hydrolyzate after cooling, take it out after 24 hours of heat preservation at 65°C, heat imidization, and heat up from room temperature to 300°C at a uniform speed for 120 minutes, and hold for 60 minutes; (b) Insulate at 120°C for 60 minutes, hang it in a sealed 650mL container with 40mL of mixed hydrolyzate after cooling, take it out after heat preservation at 65°C for 24h, heat imidization, and heat up from room temperature to 300°C at a constant speed for 120 minut...

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Abstract

The invention discloses a method for preparing a polyimide-silicon dioxide composite nanofiber membrane with crosslinking morphology. The method comprises the steps that firstly, a silicon dioxide precursor with a certain proportion is added into a polyimide precursor-polyamide acid, and a polyimide-silicon dioxide precursor composite nanofiber membrane is prepared through electrostatic spinning; secondly, heat treatment is conducted on the fiber membrane to enable part of the fiber membrane to be imidized, acidic vapor etching and hydrolyzing are conducted, high-temperature imidization treatment is conducted, and then the polyimide-silicon dioxide composite nanofiber membrane with the crosslinking morphology is prepared. The fiber membrane prepared through the method has the advantages of being significant in crosslinking structure, uniform in silicon dioxide coating and high in mechanical property; in addition, the crosslinking degree and the pore structure are adjustable and controllable, process organization of the preparation process is easy to achieve, and a good industrialized application prospect is achieved.

Description

technical field [0001] The invention belongs to the technical field of polyimide nanofiber membranes, and relates to a method for preparing polyimide / silicon dioxide composite nanofiber membranes with crosslinked morphology. Background technique [0002] Electrospinning is a simple and effective method for preparing fiber membranes. It can spin a variety of polymer melts or solutions to obtain continuous fiber non-woven fabrics in submicron or even nanometer scales. It has received extensive attention in recent years. The fiber membrane prepared by electrospinning has the characteristics of large specific surface area, large aspect ratio, high porosity, and strong adsorption force, and the electrospinning technology has the advantages of simple equipment, easy operation, quick preparation, wide application range, and low cost. Therefore, the fiber membrane prepared by electrospinning has great application prospects and significant advantages in the fields of high-performance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D04H1/728D01D5/00
CPCD01D5/00D01D5/003D04H1/728
Inventor 齐胜利林冬燕田国峰武德珍
Owner 启鼎技术(北京)有限公司
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