Method for preparing fluroxene by vertical-tube type catalytic reaction
A fluoroalkenyl ether and riser-type technology, which is applied in the field of fluorine-containing fine chemicals, can solve the problems of chlorine gas and caustic soda current efficiency drop, etc., and achieve the effect of improving product purity, meeting the demand of output and improving utilization rate
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Embodiment 1
[0042] The vertical tube reactor that is equipped with circulating cooling / heating system, temperature control system and is filled with activated carbon catalyst is vacuumized inside the system by the decompression system at the top, (the inner diameter of the vertical tube reactor is 170mm, and the length is 3600mm, Hastelloy material) filled with nitrogen for three times until the oxygen content is controlled below 10ppm, vacuumed to -0.1MPa, closed the pressure reducing valve, and adjusted the temperature of the circulating water to keep the internal temperature of the reactor at 1°C. From the lower part of the tubular reactor Slowly add 3-methoxycarboxypropionyl fluoride (molecular formula: CH 3 OOCCF 2COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:6, and the residence time of the liquid materials in the reactor is controlled by a feed flowmeter to be 10min to maintain continuous feeding and discharging. ...
Embodiment 2
[0045] A vertical pipe reactor equipped with a circulating cooling / heating system and a temperature control system filled with activated carbon, macroporous molecular sieves, and a mixed catalyst with a mass ratio of porous alumina of 2:1:1 is used to pump the inside of the system through the top decompression system. Vacuum, (the inner diameter of the vertical pipe reactor is 185mm, the length is 4100mm, made of Hastelloy alloy) filled with nitrogen and replaced three times until the oxygen content is controlled below 10ppm, then vacuumed to -0.1MPa, closed the pressure reducing valve, and adjusted the circulating water The temperature is controlled at 4°C inside the reactor, and 4-methoxymethyl fluorine-containing butyryl fluoride (molecular formula: CH 3 OOCCF 2 CF 2 COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:9, and the residence time of the liquid materials in the reactor is controlled by a feed flowm...
Embodiment 3
[0048] A vertical tube reactor equipped with a circulating cooling / heating system and a temperature control system filled with activated carbon and a mixed catalyst with a mass ratio of porous alumina of 2:3 will evacuate the inside of the system through the top decompression system, (vertical tube type The inner diameter of the reactor is 200mm, the length is 4100mm, and the Hastelloy material) is filled with nitrogen for three times until the oxygen content is controlled below 10ppm, then vacuumed to -0.1MPa, the pressure reducing valve is closed, and the temperature of the circulating water is adjusted to control the internal temperature of the reactor. Temperature at 5°C, slowly add 6-methoxycarboxypropoxy propionyl fluoride (molecular formula: CH 3 OOCCF 2 CF 2 OCF (CF 3 )COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:10, and the residence time of the liquid materials in the reactor is controlled by a f...
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