Vanadium-titanium-based catalyst for synthesizing n,n-dimethylformamide from methanol, oxygen and dimethylamine and preparation method thereof
A technology of dimethylformamide and catalyst, which is applied in the field of vanadium-titanium-based catalyst and its preparation, which can solve the problems of catalyst instability, high reaction temperature, and short life, and achieve good dispersion, high porosity, and good sintering resistance performance effect
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Embodiment 1
[0036] Dissolve 5.0 g of vanadyl sulfate and 20.0 g of titanium sulfate in 500 ml of deionized water, stir fully in a three-necked flask to mix the solution evenly, place the above solution in an ice-water bath, and use ammonia (25%) solution at 40 r / min Velocity titration to pH = 8 gave a slurry containing a tan precipitate. Continue to stir for 0.5h to allow it to fully react, then leave it to age for 2h. The aged slurry was separated by filtration and washed with 100 mL of deionized water to obtain a tan solid; the obtained solid was dried at 100°C for 2 hours, and calcined at 400°C for 5 hours to obtain a vanadium-titanium-based catalyst.
[0037] figure 1 Shown as the XRD spectrum of the catalyst, it can be seen that the catalyst support titanium is anatase TiO 2 form, vanadium is highly dispersed on the surface of the carrier.
[0038] figure 2 It is a transmission electron microscope photograph of the catalyst, and it can be seen that the particle size of the catal...
Embodiment 2
[0043] Dissolve 0.895g of vanadyl sulfate and 28.5g of titanium sulfate in 500ml of deionized water, fully stir in a three-necked flask to mix the solution evenly, place the above solution in an ice-water bath, and use ammonia (5%) solution at 40r / min Velocity titration to pH = 7 gave a slurry containing a tan precipitate. Continue to stir for 0.5h to make it fully react, then let it stand for aging for 1h. The aged slurry was separated by filtration and washed with 100 mL of deionized water to obtain a yellow-brown solid; the obtained solid was dried at 60°C for 10 hours and calcined at 300°C for 8 hours to obtain a vanadium-titanium-based catalyst.
[0044] The prepared catalyst is pressed into tablets, crushed and sieved to get 20-40 mesh particles, the prepared catalyst 0.1g is filled into the reactor, and the oxygen content is 10% ( vol.) inert gas, activated at 500°C for 1h. The catalytic reaction temperature was controlled at 120°C, methanol was passed in at a flow ra...
Embodiment 3
[0046] Dissolve 7.16g of vanadyl sulfate and 18.0g of titanium sulfate in 500ml of deionized water, stir fully in a three-necked flask to mix the solution evenly, place the above solution in an ice-water bath, and use ammonia (28%) solution at 40r / min Velocity titration to pH = 10 yielded a slurry containing a tan precipitate. Continue to stir for 0.5h to allow it to fully react, then leave it to age for 12h. The aged slurry was separated by filtration and washed with 100 mL of deionized water to obtain a tan solid; the obtained solid was dried at 120°C for 2 hours and calcined at 600°C for 4 hours to obtain a vanadium-titanium-based catalyst.
[0047] The prepared catalyst is pressed into tablets, crushed and sieved to get 20-40 mesh particles, the prepared catalyst 1.0g is filled into the reactor, and the oxygen content is 30% ( vol.) inert gas, activated at 300°C for 5h. The catalytic reaction temperature was controlled at 150°C, methanol was passed in at a flow rate of 0...
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