Method for synthesizing nomex resin containing fluorine and synthesized resin thereby and application

Abstract

The invention discloses a method for synthesizing nomex resin containing fluorine and synthesized resin thereby and an application thereof, and belongs to the technical field of macromolecule polymerization. The nomex resin containing fluorine of the invention is prepared by hypothermia pre-polycondensation of paraphthaloyl chloride and fluoric diamine in strong polar solvent and / or inorganic salt solution thereof at the temperature of -15-20 DEG C and then heating to 40-95 DEG C for polymerization. The intrinsic viscosity of the nomex resin containing fluorine prepared by the invention is 5-10; the resin has high fire resistance, the limited oxygen index can be 45-50; and the resin also has the characteristics of small hygroscopicity (0.6-1.5%), low surface energy, high dielectric strength and the like. The nomex resin containing fluorine of the invention can obtain nomex fiber containing fluorine by spinning, and can be processed into film, coating or coordination compound of the nomex resin containing fluorine for using.

Description

technical field

[0001] The present invention relates to a method for synthesizing polyaramid resin and the synthesized polyaramid resin and its application, in particular to a method for synthesizing high molecular weight fluorine-containing polyaramid resin and the synthesized high molecular weight fluorine-containing aramid resin and The application thereof belongs to the technical field of polymer polymerization. Background technique

[0002] Polyaramid resin is a type of polymer whose repeating structural units on the molecular main chain are amide groups and aromatic rings. The nitrogen atom and carbonyl group in the amide group of each repeating structural unit are directly connected to the carbon atoms in the aromatic ring. connect. Because the molecular main chain contains aromatic rings and the conjugated structure formed by aromatic rings and amide chains, polyaramid has excellent mechanical properties, heat resistance, good chemical stability and dielectric prope...

Examples

example 1

[0051] Put 600g of anhydrous NMP into a three-necked glass bottle, then add 28g of anhydrous calcium chloride at 30-60°C to dissolve, add 14.4g of 2,5-difluoro-p-phenylenediamine and 2 at 15-30°C, 11.2g of 5'-diaminobenzimidazole, then add 30.4g of TPC at -15°C to 10°C at one time, remove the heat of chemical reaction with ice water under strong stirring, and then raise the temperature to 40°C after 2 hours The reaction was continued for 1 hour at ℃~70℃ to obtain a fluorine-containing aramid resin solution, and 44.8 g of fluorine-containing aramid resin was isolated. The intrinsic viscosity of the resin was 6.7 g / dl after testing.

example 2

[0053] Put 600g of anhydrous DMAC in a three-neck glass bottle, add 8.1g of PPDA and 10.8g of 2,5-bisfluoro-p-phenylenediamine at 15-30°C, stir to dissolve, and then put it at -15°C-5°C once more Add 21.5g of TPC, remove the heat of chemical reaction with ice water under strong stirring, and then raise the temperature to 50°C-80°C for 2 hours to continue the reaction for 1 hour to obtain a fluorine-containing aramid resin solution. The intrinsic viscosity of the resin is tested. It is 7.3g / dl.

[0054] Coat the resin on a 200mm×50mm polypropylene template with an applicator, volatilize at 20°C to 60°C to form a film, wash with water, and dry at 100°C to 130°C and 150°C to 180°C for 1 hour respectively. into a film of 30-50 μm. After testing, its dielectric strength reaches 80-105MV / m, and its surface energy is 21.5mJ / m 2 , The water absorption rate in boiling water for 1h is 0.8%.

example 3

[0056] Put 577g of anhydrous NMP into a three-neck glass bottle, then add 43g of anhydrous calcium chloride at 30-50°C to dissolve, add 11.3g of PPDA and 2,2'-trifluoromethylbiphenyl diphenylene at 15-30°C 14.4g of amine, and then add 30.4g of TPC at one time at -15°C to 5°C for reaction, use ice water to remove the heat of chemical reaction under strong stirring, and then raise the temperature to 50°C to 80°C to continue the reaction 1 hours, a fluorine-containing aramid resin solution was obtained, and the intrinsic viscosity of the resin was detected to be 8.9 g / dl.

[0057] After vacuum defoaming the resin solution, it is wet-spun in a coagulation bath composed of NMP, water and calcium chloride; then plasticized and stretched, the filaments are washed with water, and dried at 110-130°C to obtain fluorine-containing aromatic resin. Amid fiber precursors. The strength of the monofilament is 8.6cN / dtex, and the limiting oxygen index is 48.

technical field

[0001] The present invention relates to a method for synthesizing polyaramid resin and the synthesized polyaramid resin and its application, in particular to a method for synthesizing high molecular weight fluorine-containing polyaramid resin and the synthesized high molecular weight fluorine-containing aramid resin and The application thereof belongs to the technical field of polymer polymerization. Background technique

[0002] Polyaramid resin is a type of polymer whose repeating structural units on the molecular main chain are amide groups and aromatic rings. The nitrogen atom and carbonyl group in the amide group of each repeating structural unit are directly connected to the carbon atoms in the aromatic ring. connect. Because the molecular main chain contains aromatic rings and the conjugated structure formed by aromatic rings and amide chains, polyaramid has excellent mechanical properties, heat resistance, good chemical stability and dielectric prope...

Examples

example 1

[0051] Put 600g of anhydrous NMP into a three-necked glass bottle, then add 28g of anhydrous calcium chloride at 30-60°C to dissolve, add 14.4g of 2,5-difluoro-p-phenylenediamine and 2 at 15-30°C, 11.2g of 5'-diaminobenzimidazole, then add 30.4g of TPC at -15°C to 10°C at one time, remove the heat of chemical reaction with ice water under strong stirring, and then raise the temperature to 40°C after 2 hours The reaction was continued for 1 hour at ℃~70℃ to obtain a fluorine-containing aramid resin solution, and 44.8 g of fluorine-containing aramid resin was isolated. The intrinsic viscosity of the resin was 6.7 g / dl after testing.

example 2

[0053] Put 600g of anhydrous DMAC in a three-neck glass bottle, add 8.1g of PPDA and 10.8g of 2,5-bisfluoro-p-phenylenediamine at 15-30°C, stir to dissolve, and then put it at -15°C-5°C once more Add 21.5g of TPC, remove the heat of chemical reaction with ice water under strong stirring, and then raise the temperature to 50°C-80°C for 2 hours to continue the reaction for 1 hour to obtain a fluorine-containing aramid resin solution. The intrinsic viscosity of the resin is tested. It is 7.3g / dl.

[0054] Coat the resin on a 200mm×50mm polypropylene template with an applicator, volatilize at 20°C to 60°C to form a film, wash with water, and dry at 100°C to 130°C and 150°C to 180°C for 1 hour respectively. into a film of 30-50 μm. After testing, its dielectric strength reaches 80-105MV / m, and its surface energy is 21.5mJ / m 2 , The water absorption rate in boiling water for 1h is 0.8%.

example 3

[0056] Put 577g of anhydrous NMP into a three-neck glass bottle, then add 43g of anhydrous calcium chloride at 30-50°C to dissolve, add 11.3g of PPDA and 2,2'-trifluoromethylbiphenyl diphenylene at 15-30°C 14.4g of amine, and then add 30.4g of TPC at one time at -15°C to 5°C for reaction, use ice water to remove the heat of chemical reaction under strong stirring, and then raise the temperature to 50°C to 80°C to continue the reaction 1 hours, a fluorine-containing aramid resin solution was obtained, and the intrinsic viscosity of the resin was detected to be 8.9 g / dl.

[0057] After vacuum defoaming the resin solution, it is wet-spun in a coagulation bath composed of NMP, water and calcium chloride; then plasticized and stretched, the filaments are washed with water, and dried at 110-130°C to obtain fluorine-containing aromatic resin. Amid fiber precursors. The strength of the monofilament is 8.6cN / dtex, and the limiting oxygen index is 48.

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