Method for preparing polyamide-imide copolymer fibers

A technology of imide copolymer fiber and polyamide, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, stretch spinning, etc., can solve the problems of fiber performance degradation, achieve high modulus, process Simple, efficient effect

Active Publication Date: 2016-01-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional improvement method is to introduce flexible groups, such as ether bonds, into the p...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of spinning dope: Use p-phenylenediamine (referred to as PDA), terephthaloyl chloride (referred to as TPC), 3,3',4,4'-biphenyltetracarboxylic dianhydride (referred to as BPDA) as monomers , wherein the molar ratio of terephthaloyl chloride and 3,3',4,4'-biphenyltetracarboxylic dianhydride is 1:3. Add 40.0g p-phenylenediamine into 640g N,N-dimethylacetamide solvent, stir for 2 hours under nitrogen protection, cool to 8°C, and then add 81.6g BPDA. After reacting for 3 hours, 18.8 g of terephthaloyl chloride was added to the system and reacted for 1 hour to obtain a polymer stock with a solid content of 18 wt%, ie a spinning stock solution.

[0026] Dry spinning forming: After the prepared spinning precursor solution is degassed for 12 hours under the protection of nitrogen, it is extruded into the spinning tunnel through a metering pump and a spinneret. The length of the tunnel is 12m, and the upper and middle sections of the tunnel are , and the lower end te...

Embodiment 2

[0029] Preparation of spinning dope: Use p-phenylenediamine (abbreviated as PDA), terephthaloyl chloride (abbreviated as TPC), and pyromellitic dianhydride (abbreviated as PMDA) as monomers, of which terephthaloyl chloride and pyromellitic The molar ratio of formic dianhydride is 1:2. Add 50g of p-phenylenediamine into 616g of N,N-dimethylacetamide solution, stir for 2 hours under nitrogen protection, cool to 5°C, and then add 72.8g of PMDA. After reacting for 2 hours, 31.28 g of terephthaloyl chloride was added to the system, and reacted for 2 hours to obtain a polymer stock with a concentration of 20%, that is, a spinning stock solution.

[0030] Dry spinning forming: After the prepared spinning precursor solution is left to defoam under the protection of nitrogen for 12 hours, it is extruded into the spinning tunnel through the metering pump spinneret. The length of the tunnel is 10m. The temperature at the lower end is 330 / 330 / 330°C respectively, and the spinning speed is...

Embodiment 3

[0033] Preparation of spinning dope: 2-(4-aminophenyl)-5-aminobenzimidazole (BIA for short), terephthaloyl chloride (TPC for short), 3,3',4,4'-diphenyl Ether tetracarboxylic dianhydride (s-ODPA for short) is a monomer, in which the molar ratio of terephthaloyl chloride and 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride is 2:5. Add 80g BIA to 982g N,N-dimethylacetamide solution, stir for 2 hours under nitrogen protection, cool to 5°C, and then add 80gs-ODPA. After reacting for 24 hours, 20.7 g of terephthaloyl chloride was added to the system and reacted for 1.5 hours to obtain a polymer stock with a concentration of 17%, that is, a spinning stock solution.

[0034] Dry spinning: put the prepared spinning precursor solution under the protection of nitrogen for 12 hours, and then extrude it into the spinning tunnel through a metering pump and spinneret. The length of the tunnel is 10m, and the upper and middle sections of the tunnel are , the lower end temperature is 220 / ...

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Abstract

The invention relates to a method for preparing polyamide-imide copolymer fibers. The method comprises the steps that diamine monomers are added to an aprotic polar solvent, stirring is carried out at the temperature of -5 DEG C to 100 DEG C under nitrogen protection, dianhydride monomers are added for reacting, then paraphthaloyl chloride is added at the temperature of -10 DEG C to 20 DEG C, and reacting is carried out to obtain polyamide-polyamide acid polymer spinning solution; the spinning solution stands still for deaeration, and enters an inert gas channel of 140 DEG C to 380 DEG C after passing through a filtering and spinning assembly, cured raw yarn is obtained, and partially-cyclized precursor nascent fibers are obtained through winding; the nascent fibers are cyclized and drafted through the process of cyclizing and drafting integration. The method for preparing the polyamide-imide copolymer fibers is simple in process and high in efficiency, the obtained polyamide-imide copolymer fibers have the advantages of being high in strength and modulus, and resistant to irradiation and high temperature, and a new thought is provided for preparation of polyamideimide fibers.

Description

technical field [0001] The invention belongs to the field of fiber preparation methods, in particular to a preparation method of polyamide-imide copolymer fibers. Background technique [0002] Aramid fiber is a typical representative of high-performance fibers, such as Russia's Armos fiber (known as aramid III in China), whose tensile strength is greater than 4.5GPa, which exceeds the Kevlar fiber produced by DuPont in the United States, and has high strength, high modulus and high temperature resistance. characteristic. Due to the strong hydrogen bonding in the molecule, aromatic polyamide has poor solubility and is difficult to dissolve in aprotic solvents, which brings great troubles to the spinning process. In order to make it dissolve, patent CN101921395A and patent CN101787582A mention that lithium chloride or calcium chloride co-solvent is added to N-methylpyrrolidone or N,N-dimethylacetamide to form a composite solvent. However, the polymer stock solution obtained ...

Claims

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Application Information

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IPC IPC(8): D01F6/74C08G73/10D01D10/02D01D5/12
Inventor 张清华方玉婷吴婷婷董杰李振涛谭文军甘锋张殿波赵昕陈大俊
Owner DONGHUA UNIV
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