A kind of method by acetic acid synthetic acrylic acid
A technology of acrylic acid and acetic acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., to achieve good hydrothermal stability, good stability, controllable and easy-to-operate preparation process
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Embodiment 1
[0056] 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 The P / V molar ratio of vanadium is added at 0.5. At the same time, surfactant PVP-K30 (final 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.
[0057] The resulting sample was pressed into tablets to 20-60 mesh, and then added to a fixed-bed reactor. After 5 wt% acetic acid aqueous solution was vaporized at 200°C, 2 Dilute, wherein the volume fraction of acetic acid in the gas phase is 5%, and the molar ratio of acetic acid to oxygen i...
Embodiment 2
[0059] 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, and then add phosphoric acid and SiO with a mass fraction of 85%. 2 Continue to reflux for 12 hours, and add phosphoric acid according to the P / V molar ratio of phosphoric acid and vanadium pentoxide being 1.2. At the same time, surfactant PVP-K90 (final 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. SiO 2 The mass fraction in the catalyst is 80%.
[0060] The resulting sample was pressed into tablets to 20-60 mesh, and then added to a fixed-bed reactor. After the 20 wt% acetic acid acetonitrile solution was vaporized at 300 ° C, it was diluted with oxygen-containing Ar, wherein the v...
Embodiment 3
[0062] 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 85% phosphoric acid, SiO 2 Continue to reflux with scandium oxide for 12 hours, and add phosphoric acid according to the P / V molar ratio of phosphoric acid and vanadium pentoxide being 3. At the same time, surfactant PVP-K150 (final 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. SiO 2 The mass fraction in the catalyst is 50%, and the mass fraction of scandium oxide in the catalyst is 1%.
[0063] The resulting sample was pressed into tablets to 20-60 mesh, and then added to a fixed-bed reactor. After 100 wt% acetic acid was gasified at 400°C, it was diluted wi...
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