Nano-catalyst for preparing methyl formate by one-step oxidation of methanol and preparation method thereof
A nano-catalyst and catalyst technology, applied in the nano field, can solve the problems of short catalyst life, complex catalyst preparation process, generation of a large amount of irritating gas, etc., and achieve the effects of good dispersion, easy molding and good sintering resistance.
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Embodiment 1
[0072] 6.0 g of vanadyl sulfate, 15.0 g of titanium sulfate, 9.0 g of sulfuric acid and 680 ml of deionized water were stirred in a three-necked flask to obtain solution A. Dissolve 80ml of ammonia water (25%) in 720ml of deionized water to form an ammonia solution with a volume fraction of 10%. Under the condition of ice-water bath, the ammonia solution was dripped into the solution A at a speed of 10ml / min (equivalent to 110r / min) until the pH=10, and a slurry containing a yellow-brown precipitate was obtained. Continue to stir for 0.5h and then leave it to age for 3h. Suction filter to obtain a yellow-brown solid. After washing with deionized water, dissolve the obtained yellow-brown solid in a solution of 15ml of water and 35ml of n-butanol, disperse for 6h, and then suction-filter to obtain cake, and then dried at 120°C for 8 hours to obtain solid B. Then solid B was calcined at 600° C. for 4 h to obtain solid C, namely the vanadium-titanium catalyst. Take 5 g of the ob...
Embodiment 2
[0075] 4.5g of vanadyl sulfate, 18.0g of titanium sulfate, 4.3g of sulfuric acid and 680ml of deionized water were stirred and fully mixed in a three-necked flask to obtain solution A. Dissolve 80ml of ammonia water (25%) in 720ml of deionized water to form an ammonia solution with a volume fraction of 10%. Under the condition of ice-water bath, the ammonia solution was dripped into the solution A at the speed of 10ml / min (equivalent to 110r / min) until the pH=9.0, and a slurry containing yellow-brown precipitate was obtained. Continue to stir for 0.5h and then leave it to age for 4h. Suction filter to obtain a yellow-brown solid. After washing with deionized water, dissolve the obtained yellow-brown solid in a solution of 15ml of water and 35ml of n-butanol, disperse for 6h, and then suction-filter to obtain cake, and then dried at 105°C for 7 hours to obtain solid B. Then solid B was calcined at 450° C. for 8 h to obtain solid C, namely the vanadium-titanium catalyst. Take ...
Embodiment 3
[0078] 7.5g of vanadyl sulfate, 15.0g of titanium sulfate, 2.5g of sulfuric acid and 680ml of deionized water were stirred in a three-necked flask to obtain solution A. Dissolve 80ml of ammonia water (25%) in 720ml of deionized water to form an ammonia solution with a volume fraction of 10%. Under the condition of ice-water bath, the ammonia solution was dripped into the solution A at the speed of 10ml / min (equivalent to 110r / min) until the pH=8.5, and a slurry containing yellow-brown precipitate was obtained. Continue to stir for 0.5h and then leave it to age for 5h. Suction filter to obtain a yellow-brown solid. After washing with deionized water, dissolve the obtained yellow-brown solid in a solution of 15ml of water and 35ml of n-butanol, disperse for 6h, and then suction-filter to obtain cake, and then dried at 95°C for 12h to obtain solid B. Then solid B was calcined at 500° C. for 5 h to obtain solid C, namely the vanadium-titanium catalyst. Take 5 g of the obtained s...
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