High-performance fluorine-containing polyimide nanofiber separation diaphragm, preparation method thereof, and application thereof
A technology of fluorine-containing polyimide and nanofiber membrane, which is applied in the direction of nanotechnology, fiber chemical characteristics, single-component synthetic polymer rayon, etc., can solve the problem of large pore size of electrospun nanofiber membrane, poor mechanical strength of diaphragm, Precursor storage instability and other issues, to achieve excellent cycle performance and energy density, low internal corrosion resistance, superior thermal stability
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[0034] The preparation method of the above-mentioned high-performance fluorine-containing polyimide nanofiber diaphragm comprises the following steps:
[0035] 1) Preparation of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene:
[0036] a) Dissolve hydroquinone, anhydrous potassium carbonate, and 2-chloro-5-trifluoromethylnitrobenzene in DMF, stir at room temperature for 20 minutes, then heat to 130° C., and keep the temperature for 18 hours;
[0037] b) Cool the mixed solution obtained in step a) to room temperature, add it to deionized water, then drop concentrated hydrochloric acid, wash and filter the precipitate obtained by filtration, and dry it in vacuum at 80°C for 12 hours to obtain a white crystal dinitro compounds;
[0038] c) heating the dinitro compound, catalyst, ethanol, and hydrazine hydrate obtained in step b) to reflux for 5 hours, filtering while hot to remove the catalyst, and then removing the solvent by rotary evaporation, and recrystallizing the crude p...
Embodiment 1
[0052] The preparation method of high-performance fluorine-containing polyimide nanofiber diaphragm, the steps are as follows:
[0053] 1) Preparation of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene (6FAPB):
[0054] a) Add 0.03mol of hydroquinone, 0.066mol of anhydrous potassium carbonate, and 0.061mol of 2-chloro-5-trifluoromethylnitrobenzene into a dry 250mL three-necked flask, and dissolve them in 80mL of DMF with magnetic stirring. After stirring at room temperature for 20 minutes, heat to 130°C and keep the temperature for 18 hours;
[0055] b) The mixed solution obtained in step a) is cooled to room temperature, then the reaction mixture is poured into 300 mL of deionized water, and then 10 mL of concentrated hydrochloric acid with a concentration of 37 wt% is slowly added dropwise to the mixture for more than 10 min. The precipitate was collected by filtration, washed and filtered with deionized water several times, and vacuum-dried at 80°C for 12 hours to obtain ...
Embodiment 2
[0062] The difference with embodiment 1 is as follows:
[0063] In step 1), 0.03mol hydroquinone, 0.06mol anhydrous potassium carbonate, 0.06mol 2-chloro-5-trifluoromethylnitrobenzene; the catalyst is palladium carbon catalyst; 1.6g catalyst, 3.2g dinitro compound, 5.76g hydrazine hydrate,
[0064] Step 2) in 5.00mmol 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene, 5.00mmol 4,4'-biphenyl ether dianhydride, 1.29g isoquinoline;
[0065] The concentration of fluorine-containing polyimide polymer in the spinning solution in step 3) is 25wt%; the process parameters of the electrospinning method are: spinneret aperture 0.6mm, voltage 15kv, feed rate 0.45mL / h, fiber receiving The distance is 15cm;
[0066] The rest is exactly the same.
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