Fluoric polymer and preparing method thereof
A high polymer and fluorinated technology, which is applied in the direction of final product manufacturing, electrochemical generator, sustainable manufacturing/processing, etc., can solve the problem of insufficient molecular weight of resin
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[0042] The following examples are further illustrations of the present invention, but the present invention is not limited thereto. Unless otherwise specified, the reaction kettles used in each embodiment are all 101 stainless steel high-pressure reaction kettles, and are equipped with temperature sensors, pressure sensors, heating circulation systems, cooling circulation systems, stirring motors, internal cooling water pipes, liquid metering pumps, gas Feed valve, liquid feed valve, material discharge valve in the reactor.
[0043] The perfluoroalkyl initiator used in the synthesis process of the present invention can be prepared according to known techniques in the art, and the recommended preparation method of the present invention can be found in J.Org.Chem., 1982, 47(11):2009-2013.
[0044] Potassium persulfate, ammonium persulfate or N used in the synthesis process of the present invention 2 f 2 Initiators such as gases are all commercially available. High-purity nitr...
Embodiment 1
[0047] Embodiment 1, r=2
[0048] Reactor is cleaned and adds 4.0L deionized water, 1000ml contains 550g cerium sulfonate pendant vinyl ether monomer (1) (F 2 C=CF-O-CF 2 CF 2 -SO 3 - ) 4 Ce 4+ And 450g cerium sulfonate pendant vinyl ether monomer (2) (F 2 C=CF-O-CF 2 -CF(CF 3 )-O-CF 2 CF 2 -SO 3 - ) 3 Ce 3+ The aqueous solution, start the stirring device, vacuumize and replace with high-purity nitrogen for three times, after testing that the oxygen content in the reactor is below 1ppm, vacuumize, fill the reactor with tetrafluoroethylene monomer to a pressure of 2.2MPa, and raise the temperature to 25 ℃, add 2.15g perfluorobutyryl compound (CF 3 CF 2 CF 2 CO-OO-CCF 2 CF 2 CF 3 ) to initiate the polymerization reaction, continue to feed tetrafluoroethylene monomer to keep the reaction pressure at 2.2MPa, add 0.62g of initiator to the system every 15min, after reacting for 2h, stop adding the initiator, let the reaction continue for 15min, then stop adding ...
Embodiment 2
[0051] Embodiment 2, r=2
[0052] Reactor is cleaned and adds 4.0L deionized water, 1000ml contains 500g cerium sulfonate pendant vinyl ether monomer (1) (F 2 C=CF-O-CF 2 CF 2 -SO 3 - ) 3 Ce 3+ And 350g manganese sulfonate pendant vinyl ether monomer (2) (F 2 C=CF-O-CF 2 -CF(CF 3 )-O-CF 2 CF 2 -SO 3 - ) 2 mn 2+ The aqueous solution, start the stirring device, vacuumize and replace with high-purity nitrogen for three times, after testing that the oxygen content in the reactor is below 1ppm, vacuumize, fill the reactor with tetrafluoroethylene monomer to a pressure of 2.5MPa, and raise the temperature to 35 ℃, add 8.4g perfluoropropoxypropyl peroxide (CF 3 CF 2 CF 2 OCF (CF 3 )CO-OO-CCF(CF 3 )OCF 2 CF 2 CF 3) to initiate the polymerization reaction, continue to feed tetrafluoroethylene monomer to keep the reaction pressure at 2.5MPa, add 2.5g of initiator to the system every 25min, stop adding the initiator after reacting for 2.5h, let the reaction continue...
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