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A method for preparing polyimide fibers based on imidization of o-methyl aramid

A technology of o-methyl aramidimide and polyimide fibers, which is applied in the field of high-performance fiber preparation, can solve problems such as weak strength, achieve dense fiber structure, high strength modulus, and overcome spinning processing difficulties Effect

Active Publication Date: 2017-01-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although there are a few industrialized polyimide fibers, they are mainly used for heat resistance and radiation resistance, and their strength has always been weaker than other high-strength and high-performance fibers.

Method used

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  • A method for preparing polyimide fibers based on imidization of o-methyl aramid
  • A method for preparing polyimide fibers based on imidization of o-methyl aramid
  • A method for preparing polyimide fibers based on imidization of o-methyl aramid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) In a three-necked flask with nitrogen, add 150ml NMP, add 10% CaCl 2 , stirred for 2 hours, added 10% diamine monomer, stirred at 10°C for 1.5 hours, then added an equimolar mass of o-methyl aromatic dichloride, stirred for 3 hours, added 0.5% dibenzoyl peroxide, as the reaction proceeded, The polymer is gradually precipitated, then washed and dried with water, and then dissolved and mixed with concentrated sulfuric acid to obtain anisotropic solute liquid crystal polyamide spinning solution.

[0033] (2) After degassing the above-mentioned liquid crystal polyamide spinning liquid, it is transported to the spinning assembly through a metering pump, and is spun by a dry-wet method. The height of the air layer is 1cm, the number of spinneret holes is 50, the diameter of the spinneret holes is 0.02mm, and the spinneret speed is 2m / min. , the temperature of the coagulation bath is 20°C. The obtained fiber enters into a water bath at 20°C, the winding speed is 80-90m / m...

Embodiment 2

[0037] (1) In a three-necked flask with nitrogen gas, add 150ml NMP, add 20% CaCl 2 , stirred for 3h, added 20% diamine monomer, stirred at 20°C for 1.5h, then added equimolar mass o-methylaromatic dichloride, added 1% isoquinoline, stirred for 4h, as the reaction proceeded, the polymer gradually Precipitate, then wash and dry with water, and then dissolve and prepare slurry with concentrated sulfuric acid to obtain anisotropic solute-type liquid crystal polyamide spinning solution.

[0038] (2) After degassing the above-mentioned liquid crystal polyamide spinning liquid, it is transported to the spinning assembly through a metering pump, and is spun by a dry-wet method. The height of the air layer is 2cm, the number of spinneret holes is 300, the diameter of the spinneret holes is 1.0mm, and the spinneret speed is 50m / min. , the temperature of the coagulation bath was 30°C. The obtained fiber enters into a water bath at 30°C, the winding speed is 80-90m / min, and dried to ob...

Embodiment 3

[0042] (1) In a three-necked flask with nitrogen gas, add 150ml NMP, add 30% CaCl 2 , stirred for 4 hours, added 40% diamine monomer, stirred at 60°C for 1.5 hours, then added an equimolar mass of o-methyl aromatic dichloride, added 0.5% acetic anhydride, stirred for 5 hours, as the reaction progressed, the polymer gradually precipitated , then washed with water and dried, and then dissolved in concentrated sulfuric acid to prepare the slurry to obtain anisotropic solute-type liquid crystal polyamide spinning solution.

[0043] (2) After degassing the above-mentioned liquid crystal polyamide spinning liquid, it is transported to the spinning assembly through a metering pump, and is spun by a dry-wet method. Among them, the height of the air layer is 40cm, the number of spinneret holes is 100, the diameter of the spinneret holes is 0.04mm, and the spinneret speed is 20m / min. , the temperature of the coagulation bath is 60°C. The obtained fiber enters a 60°C water bath, the wi...

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Abstract

The invention provides a method for preparing polyimide fibers based on imidization of o-methyl aryl amide. The method comprises the following steps that (1) an ortho-methyl aromatic polyamide liquid crystal spinning solution is prepared according to a low temperature solution polycondensation method; (2) after the prepared polyamide liquid crystal spinning solution is deaerated, spray water washing is carried out according to a dry-jet wet-spinning method, and then polyamide spun fibers are prepared; (3) the polyamide spun fibers are treated by high temperature, ortho-methyl is activated under the action of a catalyst, and reacts with amide groups to form imide rings, so that polyamide fibers are converted into the polyimide fibers; (4) molecular chain orientation and fiber axial tensile strength are increased to prepare high strength and high modulus polyimide fibers. According to the invention, rigid macromolecular chains in the spinning solution are in shapes of straight rods, thereby being beneficial to obtaining fibers with high degree of orientation, so that disadvantages of the conventional polyimide such as difficulties in spinning processing and multiple defects of the fibers are overcome, and the prepared fibers are compact in structure, and high in intensity modulus.

Description

technical field [0001] The invention belongs to the field of preparation of high-performance fibers, in particular to a method for preparing polyimide fibers based on the imidization of o-methyl aramid. Background technique [0002] Polyimide is a polymer containing five-membered imide rings in its molecular chain. It has excellent mechanical properties, heat resistance, good impact resistance, radiation resistance and solvent resistance. It is used in many fields It has a wide range of applications, and can be widely used in aerospace, military materials, electronics industry and special civil fields. Polyimide fiber is one of the common polyimide materials, and it is also a research hotspot in recent years. It has the advantages of high strength, high modulus, and high temperature resistance. However, due to the relatively large rigidity of the polyimide molecular chain, the characteristics of insoluble and infusible, the processing is difficult. The research on polyimid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/74D01F6/78C08G73/10D01D1/02D01D5/04D01D5/06D01D11/00D01D5/12D01D10/02
Inventor 张清华张殿波谭文军董杰赵昕李振涛尹朝青陈大俊
Owner DONGHUA UNIV
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