A method for preparing aramid paper with para-aramid nanofibers
A technology of nanofibers and para-aramid fiber, applied in the direction of synthetic cellulose/non-cellulose material pulp/paper, fiber raw material treatment, papermaking, etc. Requirements for high-precision products, unstable PAP performance and other issues, to achieve good industrial application prospects, excellent mechanical properties and electrical insulation properties, and excellent uniformity
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[0019] The preparation method of the para-aramid fiber paper that the present invention proposes comprises the following steps:
[0020] (1) Preparation of slurry:
[0021] (1-1) Add the solvent N-methylpyrrolidone into the reactor, add the solubilizing salt while stirring under the protection of nitrogen, and heat to 80-100°C to completely dissolve the solubilizing salt to obtain the first solution. The dissolved salt is one or more mixtures in any proportion among calcium chloride, lithium chloride and magnesium chloride, and the mass concentration of the dissolved salt is (2-12)%; the first solution is reduced to 10-25°C, Add p-phenylenediamine and auxiliary agent in the first solution, obtain the second solution, the molar concentration of p-phenylenediamine in the second solution is (0.05-0.5) mol / L, auxiliary agent is polyoxyethylene ether polymer, The molecular weight of the polyoxyethylene ether polymer is 500-6000, and one or both ends of the polyoxyethylene ether po...
Embodiment 1
[0039] (1) Add 100L N-methylpyrrolidone to a 500L reactor, add 10kg of polymerization aid CaCl under nitrogen protection and stirring 2 , heated to 100°C to dissolve completely. Then the solution was lowered to 15°C with an ice-water bath, and then 4.326kg of p-phenylenediamine (PPD) and 8kg of polyethylene glycol (PEG) with a molecular weight of 2100 were added for dissolution. After the two were completely dissolved, the solution was further cooled to 0°C. Then add 8.178kg terephthaloyl chloride powder and high-speed stirring (500r / min) to carry out polymerization, keep ice-water bath in the polymerization process, keep system temperature no more than 70 ℃; Add 200L N-methylpyrrolidone / water (7:3, mass ratio) mixed solution into the reactor, stir rapidly for 5 minutes to break up the jelly, and form a uniform and stable para-aramid nanofiber dispersion;
[0040]The prepared nanofibers have a diameter of about 20nm and an average length of about 100um. In order to remove im...
Embodiment 2
[0047] (1) Add 100L of N-methylpyrrolidone into a 500L reactor, add 8kg of solubilizing salt LiCl under nitrogen protection and stirring, and heat to 100°C to completely dissolve it. Then use an ice-water bath to lower the system to 10°C, and then add 4.326kg of p-phenylenediamine (PPD) and 5kg of polyethylene glycol (PEG-DME) with a molecular weight of 2000 and methoxy double-capped to dissolve, and wait until the two are completely dissolved. Further cool down the solution to -5°C, add 8.160kg of terephthaloyl chloride melt (85°C) and high-speed stirring (1000r / min) for polymerization, keep an ice-water bath during the polymerization, and maintain the system temperature not exceeding 90°C; the above When the polycondensation reaction proceeds until the system forms a jelly body, stop stirring, add 200L of ethanol to the reactor, stir rapidly for 10 minutes to break the jelly body, and form a uniform and stable para-aramid nanofiber dispersion;
[0048] The prepared nanofiber...
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