VPO catalyst and preparation and application thereof in preparation of acrolein by reaction of methanol and ethanol
A catalyst and acrolein technology, applied in the preparation of carbon-based compounds, organic compounds, physical/chemical process catalysts, etc., can solve problems such as difficult large-scale commercialization, unstable raw material prices, and scale-up, and achieve good hydrothermal Stability, the reaction process is simple, controllable and easy to operate, and the effect of good stability
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Embodiment 1
[0021] Vanadium pentoxide is placed in the mixed alcohol solution of benzyl alcohol and isobutanol (5g V 2 o 5 and 100mL alcohol solution), the volume ratio of benzyl alcohol to isobutanol is 3:1, heat and reflux at 120°C for 3h, then add phosphoric acid with a mass fraction of 85% and continue to reflux for 12h, the amount of phosphoric acid added is based on phosphoric acid and di Vanadium was added at a P / V molar ratio of 1.0. At the same time, surfactant PVP-K30 (concentration: 10 mg / mL) was added. The obtained solid was suction-filtered, air-dried at 100°C for 6 hours, calcined in air at 400°C for 12 hours, and activated in 0.5% butane-air mixture for 4 hours before use.
[0022] The obtained sample was pressed into tablets to 20-40 mesh, mechanically mixed with the same mass of silicon dioxide of the same mesh, and then loaded into a stainless steel tube fixed bed reactor (fixed bed inner diameter 8mm). Methanol-ethanol mixture (molar ratio 1:1), reaction temperature ...
Embodiment 2
[0024] Vanadium pentoxide is placed in the mixed alcohol solution of benzyl alcohol and isobutanol (10g V 2 o 5 and 100mL alcohol solution), the volume ratio of benzyl alcohol to isobutanol is 1:1, heat and reflux at 130°C for 3h, then add phosphoric acid with a mass fraction of 45% and continue to reflux for 12h, the amount of phosphoric acid added is based on phosphoric acid and di The P / V molar ratio in vanadium is 1.2. At the same time, surfactant PVP-K90 (concentration: 10 mg / mL) was added. The obtained solid was suction-filtered, air-dried at 120°C for 6 hours, roasted in nitrogen at 600°C for 12 hours, activated in 1.5% butane-air mixture for 4 hours before use.
[0025] The obtained sample was pressed into tablets to 40-60 mesh, mechanically mixed with the same mass of silicon dioxide of the same mesh, and then loaded into a stainless steel tube fixed bed reactor (fixed bed inner diameter 8mm). Methanol-ethanol mixture (molar ratio 5:1), reaction temperature 300°C, ...
Embodiment 3
[0027] Vanadium pentoxide is placed in the mixed alcohol solution of benzyl alcohol and isobutanol (5g V 2 o 5 and 100mL alcohol solution), the volume ratio of benzyl alcohol to isobutanol is 1:3, heat and reflux at 140°C for 3h, then add phosphoric acid with a mass fraction of 85% and continue to reflux for 12h. The P / V molar ratio of vanadium is added at 1.6. At the same time, surfactant PVP-K150 (concentration: 10 mg / mL) was added. The obtained solid was suction-filtered, vacuum-dried at 140°C for 6 hours, calcined and reduced with hydrogen at 800°C for 4 hours, activated in 3.0% butane-air mixture for 4 hours before use.
[0028] The obtained sample was pressed into tablets to 60-80 mesh, mechanically mixed with the same mass of silicon dioxide of the same mesh, and then loaded into a stainless steel tube fixed bed reactor (fixed bed inner diameter 8mm). Methanol-ethanol mixture (molar ratio 10:1), reaction temperature 400°C, pressure 0.1MPa, methanol: ethanol: oxygen: ...
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