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A kind of preparation method of high specific surface area polyimide precipitated fiber

A technology of polyimide and fibrids, which is applied in the field of preparation of polyimide fibrids with high specific surface area, which can solve problems such as slow addition, difficulty in forming ultra-thin flocculent fibrids, and changes in agglomeration structure , to achieve stable storage, easy control of shape and size, increase in length and specific surface area

Active Publication Date: 2021-11-02
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by this invention is to provide a kind of preparation method of high specific surface area polyimide sedimentation fiber, in order to overcome the easy sedimentation in the process of preparing polyimide by high temperature cyclization of polyamic acid in the prior art Due to the defects of shrinkage, deformation, agglomeration and other structural changes in the fiber and the difficulty in forming ultra-thin flocculent precipitated fibers by direct use of polyimide solution precipitation, the present invention prepares initial fibers by soluble polyimide solution precipitation method. Polyimide precipitated fiber, by slowly adding non-solvent to the coagulant, improves the coagulation performance of the coagulant, improves the formation of the precipitated fiber through the gradual coagulation process, and increases the length and specific surface area of ​​the precipitated fiber

Method used

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  • A kind of preparation method of high specific surface area polyimide precipitated fiber
  • A kind of preparation method of high specific surface area polyimide precipitated fiber
  • A kind of preparation method of high specific surface area polyimide precipitated fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Under the protection of nitrogen, add 1.5L NMP, 30.37g 2,4-TDA, 48.13g MDA to the 5L polymerization kettle, after they are fully dissolved, add 155.35g BTDA to react at room temperature for 8 hours, then drop in 20.1g chemical The cyclization catalyst isocarine is subjected to a stepwise temperature-raising polymerization reaction under a condensing and reflux device, wherein the polymerization is carried out at 100°C for 3 hours, the temperature is raised to 120°C for 3 hours, and the temperature is raised to 180°C for 3 hours to obtain a polyamide with a solid content of 13%. Imine stock solution; filter, defoam, dilute to a concentration of 5wt%, use 10mL of the diluted polyimide solution with a porous syringe containing 1 to 10,000 holes, and the inner diameter of the holes is 0.05 to 1mm, at an injection speed of 5mL / min Inject into a stirred 100mL coagulant, wherein the coagulant is composed of ethanol and NMP with a volume ratio of 2:8, the temperature of the ...

Embodiment 2

[0029](1) Under the protection of nitrogen, add 1.5L NMP, 30.37g 2,4-TDA, 48.13g MDA to the 5L polymerization kettle, after they are fully dissolved, add 155.35g BTDA to react at room temperature for 8 hours, then drop in 20.1g chemical The cyclization catalyst isocarine is subjected to a stepwise temperature-raising polymerization reaction under a condensing and reflux device, wherein the polymerization is carried out at 100°C for 3 hours, the temperature is raised to 120°C for 3 hours, and the temperature is raised to 180°C for 3 hours to obtain a polyamide with a solid content of 13%. Imine stock solution; filter, defoam, dilute to a concentration of 5wt%, use 10mL of the diluted polyimide solution with a porous syringe containing 1 to 10,000 holes, and the inner diameter of the holes is 0.05 to 1mm, at an injection speed of 5mL / min Inject into a stirred 100mL coagulant, wherein the coagulant is composed of ethanol and NMP with a volume ratio of 2:8, the temperature of the c...

Embodiment 3

[0033] (1) Under the protection of nitrogen, add 1.5L NMP, 30.37g 2,4-TDA, 48.13g MDA to the 5L polymerization kettle, after they are fully dissolved, add 155.35g BTDA to react at room temperature for 8 hours, then drop in 20.1g chemical The cyclization catalyst isocarine is subjected to a stepwise temperature-raising polymerization reaction under a condensing and reflux device, wherein the polymerization is carried out at 100°C for 3 hours, the temperature is raised to 120°C for 3 hours, and the temperature is raised to 180°C for 3 hours to obtain a polyamide with a solid content of 13%. Imine stock solution; filter, defoam, dilute to a concentration of 5wt%, use 10mL of the diluted polyimide solution with a porous syringe containing 1 to 10,000 holes, and the inner diameter of the holes is 0.05 to 1mm, at an injection speed of 5mL / min Inject into a stirred 100mL coagulant, wherein the coagulant is composed of ethanol and NMP with a volume ratio of 3:7, the temperature of the ...

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Abstract

The present invention relates to a preparation method of high specific surface area polyimide precipitated fiber. Preparation: add non-solvent to the initial polyimide precipitated fiber suspension, gradually solidify to perfect the shape of precipitated fiber, wash, Filtrate and dry to obtain polyimide precipitated fibers with high specific surface area. The invention adopts a step-by-step coagulation process, continuously adds non-solvent to the initial coagulant, improves the coagulation performance of the coagulant, makes the polyimide diluted and dissolved in the initial coagulant continue to precipitate out, and improves the formation of the initial precipitated fiber. The prepared Polyimide fibrids not only have polyimide high and low temperature resistance, radiation resistance, insulation and other properties, but also have higher specific surface area and more excellent performance.

Description

technical field [0001] The invention belongs to the field of preparation of polyimide fibrids, in particular to a method for preparing polyimide fibrids with high specific surface area. Background technique [0002] High-performance paper has excellent heat resistance, insulation performance, and chemical stability. It is widely used in aerospace, high-speed rail, communications, electrical machinery, cables, and chemical industries. It can also be used to prepare laminated products and composite materials. At present, the high-performance paper on the market is mainly prepared from aramid fiber, and the representative product is DuPont NOMAX paper. This insulating paper has had a huge impact on the high-temperature insulation industry. With the continuous progress of science and technology in our country, the demand for insulating paper is increasing, and new requirements are put forward for its high temperature resistance. At this stage, aramid paper is increasingly unable...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78C08G73/10
CPCC08G73/1007C08G73/1039C08G73/1042C08G73/1067D01F6/78
Inventor 赵昕周建荣张清华董杰吴婷婷李梦洁
Owner DONGHUA UNIV