Fluorine-containing material preparation method, and application of fluorine-containing material prepared through using method
A technology of reaction kettle and oxygen content, applied in the direction of coating, etc., can solve the problems of unable to meet the requirements of coating viscosity, low intrinsic viscosity, etc., and achieve the effect of preventing sedimentation and sagging, and high fluorine content
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[0034] The present invention provides a method for preparing a fluorine-containing material. In one embodiment, the method for preparing the fluorine-containing material includes the following steps:
[0035] S1. Add deionized water into the reactor, and reserve 1 / 3-1 / 2 of the space; wherein, the volume of the deionized water is 1 / 2-2 / 3 of the reaction volume in the reactor.
[0036]S2. Control the oxygen content in the reactor to less than 30ppm, and raise the temperature in the reactor to 30-65°C; specifically, deoxygenation can be carried out by means of vacuuming and / or nitrogen replacement.
[0037] S3. Add part of the polymerized monomers into the reactor, and raise the pressure in the reactor to 2.5-4.5 MPa.
[0038] S4. In parts by weight, add 0.01 to 1 part of emulsifier, 0.015 to 0.3 part of pH regulator and 0.001 to 0.02 part of initiator to every 100 parts of deionized water in order to start polymerization; wherein, after adding emulsifier, After the pH regulator...
Embodiment 1
[0060] Batch radical emulsion polymerization was carried out in a 50L autoclave to prepare fluorine-containing materials. Add 32L of deionized water into the reactor, replace the oxygen in the reactor with nitrogen, make the oxygen content less than 30ppm, and raise the temperature in the reactor to 55°C;
[0061] Use a diaphragm compressor to add part of the polymerized monomers to the reactor so that the pressure in the reactor rises to 4MPa; after reaching 4MPa, the pressure controller of the reactor is set to an automatic operating state at 4MPa;
[0062] Use a metering pump to add 80g of 5wt% ammonium perfluorooctanoate aqueous solution and 20g of pH regulator disodium hydrogen phosphate in sequence; when the pressure in the reactor reaches 4MPa, start stirring, fully mix the mixture in the reactor, and then add 0.5g of dicarbonic acid peroxide The solution (5wt%, solution is 10g) of diisopropyl ester initiator, starts polyreaction;
[0063] During the reaction process, ...
Embodiment 2
[0066] Batch radical emulsion polymerization was carried out in a 50L autoclave to prepare fluorine-containing materials. Add 32L of deionized water into the reactor, replace the oxygen in the reactor with nitrogen, make the oxygen content less than 30ppm, and raise the temperature in the reactor to 58°C;
[0067]Use a diaphragm compressor to add part of the polymerized monomers to the reactor to raise the pressure in the reactor to 3.5MPa. After reaching 3.5MPa, the pressure controller of the reactor is set to an automatic operation state at 3.5MPa;
[0068] Use a metering pump to add 75g of 5wt% ammonium perfluorooctanoate aqueous solution and 18g of pH regulator disodium hydrogen phosphate in sequence; when the pressure in the reactor reaches 3.5MPa, start stirring, fully mix the mixture in the reactor, and then add 5g of potassium persulfate to trigger The solution (3wt%, solution is 166.67g) of agent and the solution (5wt% that contains 2.5g sodium metabisulfite initiator...
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