Condensation washing method for fluorinated ethylene-propylene resin
A technology of polyperfluoroethylene propylene and washing method, which is applied in the field of post-processing of polymer emulsions, can solve the problems of small particle size and low bulk density of polyperfluoroethylene propylene powder, and achieves high bulk density, large particle size, Easy to use effect
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preparation example Construction
[0031] The preparation process of polyperfluoroethylene propylene resin emulsion is as follows:
[0032] Add 250-300L deionized water and 150-500g perfluorooctanoic acid sodium dispersant into a 500L high-pressure reactor, fill it with nitrogen to test the pressure without leaking, and add a certain amount of initial monomer (by weight TFE:HFP) from the initial tank after the oxygen content is qualified. =20~50:50~80), and heating up, when reaching reaction temperature 70~120 ℃ and pressure 2~4.5MPa, add initiator ammonium persulfate (APS) and potassium persulfate (KPS) mixture with metering pump 150 ~ 200g (weight ratio APS: KPS = 1: 1), start the reaction, and use a membrane press to add additional monomers (by weight TFE: HFP = 95 ~ 70: 5 ~ 30) into the autoclave to maintain the reaction pressure No change, when the amount of added monomer reaches the specified value, stop the reaction.
[0033] The solid content of the obtained polymeric emulsion is 25-30%, the specific g...
Embodiment 1
[0035] The polyperfluoroethylene propylene emulsion has a solid content of 28% and a specific gravity of 1.18.
[0036]Put 500ml of polyperfluoroethylene propylene emulsion at 80°C for 8 hours, add a certain amount of hot deionized water to make the specific gravity of the emulsion 1.15, and control the temperature of the diluted emulsion at 60±2°C. Start stirring at 800rpm, stir for 2 minutes, add 20ml of 10% (wt) nitric acid solution and continue stirring for 15 minutes, add 135ml of trichlorotrifluoroethane (F113), and stop stirring for 5 minutes to release water. Add 500ml of 80°C water, adjust the stirring speed to 450rpm, wash for 4-5min, and wash 3 times, and measure the conductivity of the water after washing to be less than 5μs / cm. The washed resin was dried in a vacuum oven at 160° C. for 5 hours.
[0037] Its particle size was determined to be 20 μm, and its bulk density was 423 g / l.
Embodiment 2
[0039] The polyperfluoroethylene propylene emulsion has a solid content of 26% and a specific gravity of 1.19.
[0040] Put 500ml of polyperfluoroethylene propylene emulsion at 80°C for 8 hours, add a certain amount of hot deionized water to make the specific gravity of the emulsion 1.15, and control the temperature of the diluted emulsion at 60±2°C, start stirring at 800rpm After stirring for 2 minutes, add 15ml of 25% (wt) ammonium bicarbonate aqueous solution, continue to stir for 15min, add 135ml of F113, stop after stirring for 5min, and emit water. Add 500ml of 80°C water, adjust the stirring speed to 450rpm, wash for 4-5min, and wash 3 times, and measure the conductivity of the water after washing to be less than 5μs / cm. The washed resin was dried in a vacuum oven at 160° C. for 5 hours.
[0041] Its particle size was determined to be 18 μm, and its bulk density was 399 g / l.
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