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Polyimide superfine fiber and preparation method thereof

A polyimide fiber and ultrafine fiber technology, applied in the chemical characteristics of fibers, spinning solution preparation, wet spinning and other directions, can solve the problem of no polyimide ultrafine fibers, etc. The effect of regular chain arrangement and improved mechanical properties

Active Publication Date: 2016-06-08
JIANGSU XIANNUO NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The wet and dry-wet spinning process has the characteristics of high efficiency, low cost, stable spinning process and suitable for industrial production, but there is no use of wet and dry-wet spinning process to obtain polyimide ultrafine fibers Related patents and reports

Method used

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  • Polyimide superfine fiber and preparation method thereof
  • Polyimide superfine fiber and preparation method thereof
  • Polyimide superfine fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Synthesis of polyamic acid solution: according to the molar ratio of PMDA:ODA=1:1, first place ODA diamine monomer in a three-necked flask, add a measured amount of solvent (DMAc), and stir under nitrogen protection to completely dissolve ODA , then add PMDA in batches and stir to make the solid content 9%, and then stir at 0-30°C for 12 hours under the protection of nitrogen to obtain a viscous polyamic acid solution with an intrinsic viscosity of 1.5dL / g.

[0028] Preparation of polyamic acid fiber: The polyamic acid solution is defoamed, and the wet process is used for spinning, the spray ratio is 6, the spinneret is 1000×Φ0.04mm, and the coagulation bath is pure water.

[0029] Thermal imidization of polyamic acid fibers: polyimide fibers are cyclized at high temperatures in stages to obtain polyimide ultrafine fibers.

[0030] The structural formula of the obtained fiber is as follows:

[0031]

[0032] The monofilament linear density is 0.153dtex, the tensile ...

Embodiment 2

[0035] Synthesis of polyamic acid solution: according to the molar ratio of PMDA: ODA: p-PDA = 10: 3: 7, first place ODA and p-PDA diamine monomers in a three-necked flask, and add a measured amount of solvent (DMAc) , stirred under the protection of nitrogen to completely dissolve ODA and p-PDA, then added PMDA in batches and stirred to make the solid content 10%, and then stirred at 0-20°C for 8 hours under the protection of nitrogen to obtain a viscous polyamide The acid solution has an intrinsic viscosity of 1.53dL / g.

[0036] Preparation of polyamic acid fiber: polyamic acid solution is defoamed and spun by wet process, the spray ratio is 5, the spinneret is 800×Φ0.04mm, and the coagulation bath is a mixture of water and DMAc.

[0037] Thermal imidization of polyamic acid fibers: Cyclization of polyimide fibers at high temperatures.

[0038] The structural formula of the resulting fiber:

[0039]

[0040] The monofilament linear density is 0.205dtex, the tensile stre...

Embodiment 3

[0042]Synthesis of polyamic acid solution: according to the molar ratio of BPDA: ODA: p-PDA = 10: 5: 5, first place ODA and p-PDA diamine monomers in a three-necked flask, and add a measured amount of solvent (DMAc) , stirred under the protection of nitrogen to completely dissolve ODA and p-PDA, then added BPDA in batches and stirred to make the solid content 11%, and then stirred at 0-50°C for 10 hours under the protection of nitrogen to obtain viscous polyamide The acid solution has an intrinsic viscosity of 1.6dL / g.

[0043] Preparation of polyamic acid fiber: polyamic acid solution is defoamed and spun by dry-wet process. The spray ratio is 4, the spinneret is 500×Φ0.06mm, the coagulation bath is pure water, and the length of the air layer is It is 1cm.

[0044] Thermal imidization of polyamic acid fibers: Cyclization of polyimide fibers at high temperatures.

[0045] The structural formula of the resulting fiber:

[0046]

[0047] The bundle linear density is 0.245d...

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Abstract

The invention discloses a polyimide superfine fiber and a preparation method thereof. The method includes the steps of adding solvent to dissolve diamine under protection of nitrogen, adding dianhydride to make the solid content of the solution be 9-20%, conducting reaction for 3-12 hours at a temperature of 0-50 DEG C to obtain a polyimide spinning solution, conducting spinning through the polyimide spinning solution according to a wet method or dry method spinning process, and conducting imidization on polyamide acid protofilament through the thermal amidation or chemical imidization process. The minimum monofilament density of the prepared polyimide superfine fiber can reach 0.153 dtex, the raw materials are wide in source and low in cost, the spinning process is stable, and industrial production can be achieved.

Description

Technical field: [0001] The invention belongs to the technical field of ultrafine fibers and preparation methods thereof, and in particular relates to a polyimide ultrafine fiber and a preparation method thereof. Background technique: [0002] Polyimide fiber is a high-performance organic fiber with high strength and high modulus, high temperature resistance, low temperature resistance and radiation resistance, and also has biocompatibility and dielectric properties. It is one of the indispensable polymer materials with broad development prospects in industry, aerospace and other fields. [0003] There are two types of wet spinning of polyimide. One is a one-step technical route: the spinning stock solution used is a soluble polyimide solution, and the polyimide primary fiber is obtained by spinning the soluble polyimide solution without thermal cyclization or chemical A cyclization treatment step, which avoids defects such as micropores inside the fiber that may be caused...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F6/78C08G73/10D01D1/02D01D5/06
CPCC08G73/1007C08G73/1067D01D1/02D01D5/06D01F6/74D01F6/78
Inventor 武德珍牛鸿庆韩恩林于文骁俞建刚
Owner JIANGSU XIANNUO NEW MATERIAL TECH
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