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Preparation method of p-aramid nanofiber

A nanofiber, para-aramid fiber technology, applied in fiber processing, fiber chemical characteristics, spinning solution preparation, etc., can solve the problems of destroying the properties of aramid fiber, long production cycle, complex production technology, etc., to reduce the post-processing process. , the effect of reducing production costs and improving safety performance

Active Publication Date: 2015-12-16
SHANDONG JUFANG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN104562650A, CN104480702A, CN103146007A, CN103937237A, CN103537198A, CN103824988, etc. have adopted similar alkali dissolution method to prepare nanoscale para-aramid fiber, but the preparation method has long reaction time, low effective concentration, and the obtained ionized structure is not Stable, low production efficiency, and chemical reactions often destroy the original properties of aramid fiber
However, the traditional sulfuric acid dissolution method has serious cutting damage, uneven microfiber size, sulfuric acid will corrode the machine, and has more stringent requirements on the production process. Therefore, the preparation method is costly, long production cycle, and complex production technology.

Method used

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  • Preparation method of p-aramid nanofiber

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preparation example Construction

[0015] The preparation method of the para-aramid nanofiber proposed by the inventive method comprises the following steps:

[0016] (1) Modified polymerization:

[0017] Under the protection of nitrogen, add the solvent that has been dewatered into the reaction vessel, add the solubilizing salt and surfactant under stirring, and heat to 80-100°C to dissolve the solubilizing salt and surfactant to obtain the solubilizing salt and surfactant solution, the heating time is 45-60min, and z is cooled in a cold water bath for 10min to 0-15°C, and p-phenylenediamine (PPD) is added to the reaction vessel, after the p-phenylenediamine is dissolved, the reaction vessel is cooled To -15 ~ 0 ℃, then add terephthaloyl chloride (TPC), increase the stirring speed to 1000 ~ 2500r / min, continue the reaction, the reaction time is 5 ~ 10 minutes, the reaction temperature is -15 ~ 0 ℃, wait for the above Stop stirring after gelation occurs in the reaction system to obtain a jelly body, wherein th...

Embodiment 1

[0025] (1) Under the protection of nitrogen, add 100mL of N-methylpyrrolidone (NMP) that has undergone water removal treatment into the reaction vessel, and add the solubilizing salt CaCl under stirring. 24.844g, LiCl1.157g and surfactant PEG-2000 (polyethylene glycol of molecular weight 2000) 3g, and be heated to 100 ℃ and make solubilizing salt and tensio-active agent dissolve, obtain the solution of solubilising salt and tensio-active agent, The heating time was 45 minutes, and then cooled in a cold water bath for about 10 minutes to 15°C, and 4.326g of p-phenylenediamine (PPD) was added to the reaction vessel, and the reaction vessel was cooled to 0°C after the p-phenylenediamine was dissolved. Add terephthaloyl chloride (TPC) again, increase the stirring speed to 2000r / min, continue to react for 5 minutes, the reaction temperature is 0°C, stop stirring after gelation occurs in the above reaction system, and obtain a jelly body;

[0026] (2) Add 1L of dispersant N-methylpy...

Embodiment 2

[0030] (1) Under the protection of nitrogen, add 100mL of solvent N,N-dimethylformamide (DMF) and N,N-dimethylacetamide (DMAc) (volume ratio 1:1) after water removal treatment In the reaction vessel, add the solubilizing salt CaCl under stirring 2 6g and 3g of surfactant mPEG (polyethylene glycol monomethyl ether with a molecular weight of 2000), and heated to 80°C to dissolve the solubilizing salt and the surfactant to obtain a solution of the solubilising salt and the surfactant, and the heating time is 60min , and then cool in a cold water bath for about 10 minutes to 10°C, add 4.326g of p-phenylenediamine (PPD) into the reaction vessel, and cool the reaction vessel to -5°C after the p-phenylenediamine is dissolved. Add terephthaloyl chloride (TPC) again, increase the stirring speed to 2500r / min, continue to react for 8 minutes, the reaction temperature is -5°C, stop stirring after gelation occurs in the above reaction system, and obtain a jelly body;

[0031] (2) Add 2L o...

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Abstract

The invention relates to a preparation method of p-aramid nanofiber, and belongs to the technical field of polymer new materials. The diameter of the prepared p-aramid nanofiber ranges from tens of nanometers to hundreds of nanometers, and the length of the prepared p-aramid nanofiber ranges from hundreds of nanometers to tens of micrometers. According to the preparation method, a certain amount of surface active agents are added in the PPTA low-temperature polymerization process, aggregation of PPTA molecules is controlled while PPTA molecule chains are lengthened, and the p-aramid nanofiber which is uniform in size and has the diameter capable of being regulated within the range between nanometer and submicron can be prepared under the auxiliary effect of other means (for example, precipitator and high-speed shearing and dispersing). The preparation method is short in production flow, devices are simple, batched and stable production can be achieved, and therefore the requirement for industrially producing the p-aramid nanofiber on a large scale is met; the preparation method has wide application prospects and can be used for preparing lithium-ion battery separators and high-performance composites.

Description

technical field [0001] The invention relates to a method for preparing para-aramid nanofibers, belonging to the technical field of new polymer materials. Background technique [0002] Poly-p-phenylene terephthalamide (PPTA) is a high-performance material. Its molecular chain contains rigid benzene rings and strong polar amide bonds. There are strong hydrogen bonds between molecular chains, and its structure is simple. Symmetrical, regular arrangement, high strength, high modulus and high temperature resistance and other excellent properties. Moreover, its density is not high, and the fiber prepared from it is a high-performance fiber (para-aramid, aramid 1414 or aramid II), which is widely used in special clothing, aerospace, sporting goods, cables and composite materials, etc. field. [0003] Aramid nanofibers have a special molecular structure, are easy to disperse, and are easy to compound with other materials. They have good heat insulation and oxidation resistance, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28D01F6/60
CPCC08G69/28C08G69/32D01D1/02D01D5/40D01F6/605D01D5/38D01D10/06D01F1/10D01F11/08D01F13/04
Inventor 庹新林李京龙闫鸿琛
Owner SHANDONG JUFANG NEW MATERIAL CO LTD
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