Method for resource utilization of fluoroform
A technology of trifluoromethane and fluorodichloromethane, applied in chemical instruments and methods, chlorodifluoromethane production, organic chemistry, etc., can solve the problems of many by-products, serious carbon deposition, high reaction temperature, etc. Effects of cost, life extension, and product selectivity improvement
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Embodiment 1
[0029] Pass trifluoromethane and fluorodichloromethane at a ratio of 1:1 (molar ratio) into a reactor containing 50ml of pretreated chromium trioxide catalyst, at a temperature of 350°C, a pressure of 2bar, and a space velocity of 2000h -1 react under the conditions. The pretreatment process of chromium trioxide is fluoridation treatment at 400°C for 2 hours in a mixed atmosphere of 10% hydrogen fluoride and 90% nitrogen, and finally 5 hours at 400°C with hydrogen fluoride. The conversion rate of trifluoromethane is 89%, and the selectivity of difluorochloromethane is 98%. In addition to some unreacted trifluoromethane and monofluorodichloromethane, there are traces of methane and CO in the tail gas. 2 Wait for gas. After the tail gas separates and collects difluorochloromethane, the remaining gas circulates into the reactor to continue to react with trifluoromethane.
Embodiment 2
[0031] Pass trifluoromethane and trichloromethane at a ratio of 2:1 (molar ratio) into a reactor containing 50ml of pretreated chromium trioxide catalyst, at a temperature of 350°C, a pressure of 2bar, and a space velocity of 2000h -1 react under the conditions. The pretreatment process of chromium trioxide is fluoridation treatment at 400°C for 2 hours in a mixed atmosphere of 10% hydrogen fluoride and 90% nitrogen, and finally 5 hours at 400°C with hydrogen fluoride. The conversion rate of trifluoromethane is 95%, and the selectivity of difluorochloromethane is 95%. In addition to some unreacted trifluoromethane and monofluorodichloromethane, there are traces of methane and CO in the tail gas. 2 Wait for gas. After the tail gas separates and collects difluorochloromethane, the remaining gas circulates into the reactor to continue to react with trifluoromethane.
Embodiment 3
[0032] Example 3 catalyst preparation
[0033] 10.09g Sm(NO 3 ) 3 Dissolve in 205ml of distilled water to make impregnating solution, impregnate on 100g of MgO carrier with high specific surface area, age for 12h after impregnating for 5 hours, dry the water in an oven at 110°C for 12h, and dry at 400°C N 2 Roasting under the atmosphere for 5h, the prepared 5.2wt%Sm 2 o3 / MgO catalyst. The prepared catalyst was evaluated according to the raw material composition, pretreatment process and reaction conditions of Example 1, and the evaluation results are shown in Table 1.
[0034] 14.04g La(NO 3 ) 3 6H 2 O was dissolved in 225ml of distilled water to make a solution, and 100g of high specific surface area Al 2 o 3 Dispersed in La(NO 3 ) 3 solution, a suspension was formed, to which 20% NH 3 water solution, and at the same time turn on the magnetic stirring until the pH = 9~11, stop the reaction, let it stand for aging for 12 hours, then carry out suction filtration, dr...
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