Polyimide fibrous membrane with crosslinking morphology and preparation method thereof

A technology of polyimide fiber and fiber membrane, which is applied in fiber processing, textiles, papermaking, non-woven fabrics, etc., can solve the problem that the excellent mechanical properties and dimensional stability of polyimide materials cannot be reflected, and the mechanical properties of fiber membranes cannot be realized. Poor performance, limited practical application and other problems, to achieve the effects of process and industrial scale preparation, good dimensional stability and wide application range

Inactive Publication Date: 2015-11-11
北京凯越嘉诚科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the polyimide fiber membrane prepared by the traditional electrospinning method is usually a non-woven structure, the fibers of the fiber membrane are piled up layer by layer, the overlap is loose, and there is no strong interaction, so the mechanical properties of the fiber membrane are usually poor. , so that the excellent properties of the polyimide material itself, especially the mechanical properties and dimensional stability, cannot be reflected, which greatly limits its practical application.

Method used

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  • Polyimide fibrous membrane with crosslinking morphology and preparation method thereof
  • Polyimide fibrous membrane with crosslinking morphology and preparation method thereof
  • Polyimide fibrous membrane with crosslinking morphology and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Using pyromellitic dianhydride (PMDA) and 4,4'-diaminodiphenyl ether (ODA) as the dianhydride and diamine monomers respectively, and DMF as the solvent, polyamic acid solution was polycondensed with a solid content of 12%. , the polyamic acid fiber membrane was prepared by electrospinning, and the subsequent treatment processes were (a) direct high-temperature thermal imidization without solvent treatment, and the temperature was raised from room temperature to 300 ° C at a uniform speed for 120 minutes, and kept for 120 minutes; (b) ) from room temperature to 250°C at a constant speed for 100 minutes, cooled, soaked in DMF for 1 minute, and then thermally imidized, from room temperature to 300°C at a constant speed for 120 minutes, and kept at a constant speed for 120 minutes; (c) from room temperature to 80 minutes at a constant speed 200°C, cool down, soak in DMF for 1min, then thermally imidize, heat up from room temperature to 300°C at a constant speed over 120min, ...

Embodiment 2

[0046] Adopt PMDA, ODA to be dianhydride and diamine monomers respectively, DMF is solvent, polycondensation obtains polyamic acid solution, solid content is 12%, prepares polyamic acid fiber membrane with electrospinning method, and subsequent processing process is respectively (a ) from room temperature to 250°C at a constant speed for 100 minutes, cooled, soaked in DMF for 10 minutes, and then thermally imidized, from room temperature to 300°C at a constant speed for 120 minutes, and kept at a constant speed for 120 minutes; (b) from room temperature to Cool at 250°C, soak in DMF for 20min, then thermally imidize, heat up from room temperature to 300°C at a constant speed over 120min, and keep warm for 120min. The morphologies of the obtained imide fiber membranes are shown in Figure 2(a) and (b). It can be seen from the figure that the polyimide fiber membranes treated with solvent for 10min and 20min have a large number of bonding points, and the longer the solvent treatm...

Embodiment 3

[0049] Using PMDA and ODA as dianhydride and diamine monomers respectively, and DMF as solvent, polyamic acid solution was polycondensed with a solid content of 12%, and polyamic acid fiber membrane was prepared by electrospinning method, and the subsequent treatment process was from room temperature through The temperature was raised to 250°C at a constant speed for 100 minutes, cooled, soaked in DMAc for 20 minutes, and then thermally imidized, and the temperature was raised from room temperature to 300°C at a constant speed for 120 minutes, and kept for 120 minutes. The morphology of the obtained imide fiber membrane is as follows: image 3 shown. It can be seen from the figure that the degree of crosslinking of the polyimide fiber membrane after solvent treatment for 20min is relatively large, and compared with the untreated polyimide fiber membrane, the porosity drops to 65.1% (such as Figure 6 Shown), the mechanical properties are excellent, increased to 51.79MPa (such ...

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Abstract

The invention provides a polyimide fibrous membrane with crosslinking morphology and a preparation method thereof. Binary acid anhydride and diamine are adopted to perform solution condensation polymerization, so as to prepare a precursor of polyimide, i.e. polyamide acid; then a polyamide acid fibrous membrane is prepared by electrostatic spinning. The polyamide acid fibrous membrane is pretreated, and is heated to 200 to 250 DEG C, so as to obtain a partially imidized fibrous membrane, afterwards the partially imidized fibrous membrane is immersed into a soluble solvent of the polyamide acid for performing slightly soluble crosslinking treatment, is dried, and is subjected to high temperature thermal imidization so as to obtain the polyimide fibrous membrane with the crosslinking morphology. The prepared polyimide fibrous membrane has a crosslinking structure, the mechanical property is greatly improved, the pore structure is adjustable, crosslinking degree and pore structure distribution are adjusted by changing pretreatment temperature and solvent treatment time, the preparation process is simple, the process is easy to form, and the industrialized application prospect is very good.

Description

technical field [0001] The invention belongs to the technical field of polyimide fiber membranes, and relates to a polyimide fiber membrane with a cross-linked structure and a preparation method thereof. Background technique [0002] Electrospinning has received extensive attention in recent years because it can spin a variety of polymer melts or solutions to obtain submicron-sized continuous fibers. It is a technique in which the polymer precursor is stretched into fibers under the action of a strong electrostatic field force. Electrospinning can form continuous fibers with diameters ranging from submicron to nanometer. The fibers have the characteristics of large specific surface area, small pore size, high porosity, and strong adsorption force. The electrospinning equipment is simple, the operation time is short, and the preparation is convenient. , so electrospun fiber membranes have great application value in the fields of tissue engineering scaffolds, drug sustained-r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D04H1/728D01D5/00D04H1/4326
Inventor 齐胜利黄素萄田国峰武德珍
Owner 北京凯越嘉诚科技发展有限公司
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