A preparation method of para-meta-position copolymerized aramid paper
The technology of para-aramid fiber and aramid fiber paper is applied in the field of preparation of para-meta-co-aramid fiber paper, which can solve the problem that the addition amount of fibrids cannot be too high, the preparation path of aramid fibrids is long, and the aramid paper Dimensional stability decline and other problems, to achieve the effect of improving structural uniformity and mechanical properties, improving structural and mechanical properties, tensile strength and elongation at break
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[0024] The preparation method of para-position meta-position copolymerized aramid fiber paper that the present invention proposes comprises the following steps:
[0025] (1) Preparation of aramid para-meta-position copolymer:
[0026] Under the protection of nitrogen, mix the dewatered polymerization solvent with the solubilizing salt, the mixing ratio is: the mass of the solubilizing salt is 5-10% of the mass of the polymerization solvent, heat to 80-100°C to dissolve the solubilizing salt, and cool the water Cool the bath to 5-15°C to obtain the first solution; add the diamine monomer to the first solution, the molar concentration of the diamine monomer in the first solution is 0.1-0.5mol / L, and wait for the diamine monomer to dissolve After cooling to -5 ~ 5 ° C, add diacid chloride monomer, the molar ratio of diacid chloride monomer and diamine monomer is (0.09 ~ 1.01): 1, high-speed stirring for polymerization reaction, stirring speed is 500 ~ 2000rpm , the reaction time...
Embodiment 1
[0042] Under the protection of nitrogen, 100mL NMP was added to the reaction vessel, and the solubilizing salt CaCl was added under stirring. 2 6g, and heated to 100°C to dissolve it for 60 minutes, then cooled to 15°C in a cold water bath. 2.163 g of diamine monomer was added to the reaction vessel. The diamine monomer consists of 50% p-phenylenediamine and 50% m-phenylenediamine by mass. After the diamine monomer was dissolved, the reaction vessel was cooled to 0° C. with an ice-water bath. 4.101 g of another monomer terephthaloyl chloride (TPC) was added, and the stirring speed was increased to 2500 r / min to continue the reaction. Stop stirring for a period of time after the rod-climbing phenomenon occurs in the above reaction system to obtain jelly. Add 2L of NMP to the jelly to swell the jelly. Then transfer the swollen product to a homogeneous emulsification disperser for high-speed stirring, shearing, breaking and dispersing into a macroscopically uniform system. ...
Embodiment 2
[0045] Under the protection of nitrogen, 100mL NMP was added into the reaction vessel, 8g of the solubilizing salt LiCl was added under stirring, and heated to 80°C to dissolve it for 60min, and then cooled to 10°C in a cold water bath. 4.326 g of p-phenylenediamine monomer was added to the reaction vessel. After p-phenylenediamine was dissolved, the reaction vessel was cooled to 0°C with an ice-water bath. Polymerization was carried out by adding 8.178 g of another monomer, diacid chloride. The diacid chloride monomer consists of 50% by mass of terephthaloyl chloride and 50% of isophthaloyl chloride. Increase the stirring speed to 1500r / min to continue the reaction. Stop stirring for a period of time after the rod-climbing phenomenon occurs in the above reaction system to obtain jelly. Add 2L of DMF to the jelly to swell the jelly. Then transfer the swollen product to a homogeneous emulsification disperser for high-speed stirring, shearing, breaking and dispersing into a ...
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