Preparation method for fluorine-contained emulsifier
A technology of emulsifiers and fluorine-containing solvents, applied in chemical instruments and methods, chemical/physical processes, dissolution, etc., can solve problems such as high risk and easy out-of-control production of fluorine-containing emulsifiers
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Embodiment 1
[0062] A stainless steel reactor with a built-in ultraviolet lamp (wavelength 200nm) in a volume of 2L, with a reflux facility at -70°C; add perfluorodimethyl ether (solvent) that has been precooled to -30°C into the precooled reactor 0.5L; into the bottom of the reactor metered oxygen (O 2 ) 20L / h (standard state) and hexafluoropropylene (monomer) 2.5L / h (standard state) (purity 99.5%) mixed gas, keep the reaction phase at a temperature of about -45 ° C, maintain 8h, the bottom product take out. After the product was hydrolyzed in deionized water at 90°C for 6 hours, 565 g of the oil layer was obtained by static layering. After testing, the acid value of the product was 80.5 mgNaOH / g, and the peroxide content was 28 ppm. The product was formulated into an ammonium salt solution with a surface tension of 12.9mN / m.
Embodiment 2
[0064] A stainless steel reactor with a built-in ultraviolet lamp (wavelength 300nm) in a volume of 2L, with a reflux facility at -70°C; add 0.5L of hexafluoropropylene precooled to -40°C into the precooled reactor; The metered oxygen (O 2 ) 20L / h (standard state) and perfluoromethyl ethyl ether 2.5L / h (standard state) (purity 99.0%) mixed gas, keep the reaction phase at about -45 ℃ of temperature, maintain 8h, the bottom product take out. After the product was hydrolyzed in deionized water at 90°C for 6 hours, 580 g of the oil layer was obtained by static layering. After testing, the acid value of the product was 75.5 mgNaOH / g, and the peroxide content was 25 ppm. The product is formulated into an ammonium salt solution with a surface tension of 21.2mN / m.
Embodiment 3
[0066] A stainless steel reactor with a built-in ultraviolet lamp (wavelength 380nm) in a volume of 2L, with a reflux facility at -70°C; add 0.5L of hexafluoropropylene precooled to -40°C into the precooled reactor; The metered oxygen (O 2 ) 20L / h (standard state) and chlorotrifluoroethylene 2.5L / h (standard state) (purity 99.4%) mixed gas, keep the reaction phase at about -45 ℃ of temperature, maintain 8h, the bottom product is taken out. After the product was hydrolyzed in deionized water at 90°C for 6 hours, 572 g of the oil layer was obtained by static layering. After testing, the acid value of the product was 65.5 mgNaOH / g, and the peroxide content was 52 ppm. The product was formulated into an ammonium salt solution with a surface tension of 17.2mN / m.
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