Method for preparing acrylic acid from propane under the condition of free-dioxygen
A technology of acrylic acid and molecular oxygen, which is applied in the direction of oxidative preparation of carboxylic acid, carboxylate preparation, organic chemical methods, etc., to achieve the effect of improving selectivity
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Embodiment 1
[0068] Formula Mo 1 V 0.33 Nb 0.11 Te 0.22 Si 1.08 o x Preparation of Catalyst A
[0069] a) Preparation of niobium solution
[0070] Add 80 grams of distilled water to a 600-ml beaker, and then add 6.4 grams (0.038 moles) of niobic acid. Then 12.9 grams (0.102 moles) of oxalic acid dihydrate were added.
[0071] The oxalic acid / niobium molar ratio is therefore 2.69.
[0072] The above solution was heated to 60°C for 2 hours 19 minutes with stirring and covered to prevent evaporation. A white suspension was obtained which was cooled to 30° C. with stirring for about 2 hours.
[0073] b) Preparation of Mo, V and Te solutions
[0074] Add 265 grams of distilled water, 61 grams (0.346 moles) of ammonium heptanomolybdate, 13.3 grams (0.114 moles) of ammonium metavanadate NH in a 600-ml beaker 4 VO 3 and 17.4 g (0.076 mol) telluric acid (supplier: FLUKA).
[0075] The above solution was heated to 60°C for 1 hour and 35 minutes with stirring and covered to prevent evapo...
Embodiment 2
[0084] Formula Mo 1 V 0.33 Nb 0.11 Te 0.22 o x Preparation of Catalyst B
[0085] The procedure performed was as described in Example 1, parts a) and b).
[0086] The niobium solution was then added to the Mo, V and Te solutions. After stirring for several minutes, a fluorescent orange gel was obtained. The solution was then placed in an oven at 130°C overnight.
[0087] 88.8 g of precursor were thus recovered.
[0088] The procedure as described in Example 1, part d) was then followed.
[0089] 20.8 g of Catalyst B were thus obtained.
Embodiment 3
[0091] Catalyst A test
[0092] a) Test according to the pulse mode
[0093] a1) Operation mode
[0094] The detailed operation performed is as follows.
[0095] In a vertical reactor, fill from bottom to top: 2 ml (2.346 g) of silicon carbide particles with a particle size of 1.19 mm (mesh opening 1-1.25 mm) from the first height, 5 ml (5.458 g) from the second height g) catalyst particles with a particle size of 0.25-1 mm, and a third height of the same silicon carbide as above (19.547 g).
[0096] Then, the reactor was heated to 250°C and the evaporator was heated to 200°C. Electricity to start the water pump.
[0097] Once the reactor and evaporator reached the indicated temperature, the water pump was started and the temperature of the reactor was raised to 350°C. The temperature of the reactor was then further raised to 380°C at a rate of 10°C every 10 minutes.
[0098] Then, the reactor was stabilized for 30 minutes.
[0099] Next, oxygen was fed in 10 pulses of ...
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