A kind of unsaturated aldehyde selective oxidation method
An aldehyde selective, unsaturated technology, applied in the field of selective oxidation of unsaturated aldehydes, can solve the problems of huge energy consumption, huge economic losses, difficult to control accurately, etc., to suppress hot spots, avoid the drop of bed temperature, long-term The effect of cycle stable production
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Embodiment 1
[0040] Preparation of Catalyst 1
[0041] Step 1: Prepare catalyst inner layer matrix
[0042] (1) Preparation of active ingredient slurry (a)
[0043] Under stirring conditions, take 211.9 grams of ammonium molybdate and 46.8 grams of ammonium metavanadate and dissolve them in 500ml of pure water (water temperature above 65°C) to obtain slurry (1), then take 52.2 grams of ammonium paratungstate, 127.9 grams of copper nitrate, 14.5 grams Dissolve nickel nitrate, 48 grams of sodium stannate, and 5.8 grams of cesium nitrate in 1000 ml of pure water (water temperature above 65°C), stir well and mix evenly to obtain slurry (2). Then, the slurry (1) is mixed with the slurry (2) to obtain the slurry (3) to obtain the active ingredient slurry (a).
[0044] (2) Preparation of catalyst inner layer matrix
[0045] Add 90 grams of silicon dioxide and 1.4 grams of graphite to the active component slurry (a), stir vigorously at 80°C for co-precipitation reaction, heat and dry, heat-trea...
Embodiment 2
[0059] Preparation of Catalyst 2
[0060] Same as the preparation steps and the main raw materials of the catalyst 1 in Example 1, just add 16.2 grams of lanthanum nitrate, add 162 grams of silicon dioxide and 2.3 grams of silicon carbide in the inner layer, and extrude and roll granulate into a diameter of 2mm through an extruder. Spherical shape, adding 13.2 grams of silicon dioxide to the outer layer. The thickness of the coating is 0.5-2.0mm, and the catalyst 2 is obtained by roasting at 450° C. for 3 hours. The main composition of catalyst 2 inner layer matrix is: Mo 12 V 5 W 4 Cu 2 Ni 3.7 sn 0.6 La 0.5 Si 25.2 o x , the main composition of the outer layer is: Mo 12 V 5 W 4 Cu 2 Ni 3.7 sn 0.6 La 0.5 Si 2.2 o x , the element content of the outer layer is 0.8%~17.4% higher than that of the inner layer.
Embodiment 3
[0067] Same as the preparation steps and main raw materials of the catalyst 1 in Example 1, just add 11.8 grams of potassium manganate, add 174.6 grams of silicon dioxide and 1.6 grams of aluminum oxide in the inner layer; add 4.2 grams of silicon dioxide in the outer layer. The main composition of the catalyst 3 inner layer matrix is: Mo 12 V 2 W 6.7 Cu 1 Ni 1.2 sn 1.0 Si 20.5 mn 0.6 o x , the main composition of the outer layer is: Mo 12 V 2 W 6.7 Cu 1 Ni 1.2 sn 1.0 Si 0.7 mn 0.6 o x
[0068] The inner diameter of the fixed-bed single-tube reactor is 25 mm, and a thermocouple is installed inside, and 13 ml of CN201110265250.4 catalyst 3 (S 1 paragraph), 17ml of the above catalyst (S 2 section), heated in a salt bath, and the temperature of the salt bath was 253°C. From the entrance of the above reaction tube at a space velocity of 2000h -1 A mixed gas of 11% by volume of acrolein, 15% by volume of oxygen, 15% by volume of water vapor, and 59% by volume of...
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