Method for recovering heteropoly acid from deactivated supported type heteropoly acid catalyst
A heteropolyacid and catalyst technology, which is applied in chemical recovery, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of undisclosed heteropolyacid recovery and purity, and achieve high purity, single structure, and high yield. high rate effect
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Embodiment 1
[0042] Take by weighing 20 grams of deactivated supported phosphotungstic acid catalyst in the alkylation reaction of isobutane and butene, the active component of this catalyst is H 3 PW 12 o 40 , the carrier is silicon oxide SiO 2 , 25% by weight of phosphorus-containing tungstic acid, adding this catalyst and the concentration of equal volume in the crucible is 35% by weight of HClO 4 25.1 grams of aqueous solution makes the catalyst just wet completely, makes HClO 4 The amount of the catalyst is 44% of the dry weight of the catalyst. After standing for 0.5h, the above system is put into a muffle furnace and burned for 1h (air atmosphere) at 230°C. After cooling, the catalyst treated in this way is put into an Erlenmeyer flask , add 40g of water, fully stir on a magnetic stirrer, control the temperature of the system at 25°C, and process for 1 hour. Suction filtration to remove the carrier; at 55°C, depressurize to 15.75×10 3 Under the condition of Pa, the solution is ...
Embodiment 2
[0052] The deactivated loaded phosphotungstic acid catalyst is the same as that in Example 1, with an amount of 50 grams. In crucible, add this catalyst and 16.3g concentration respectively and be the HClO of 15% by weight 4 solution, and 15.0 g of HNO at a concentration of 15% by weight 3 solution, stirred evenly and left for 0.5h, put the above system into a muffle furnace and burn at 120°C for 3h (oxygen atmosphere), take it out and add 16.3g of HClO with a concentration of 15% by weight in the catalyst after cooling 4 solution and 15.0 g of HNO at a concentration of 15% by weight 3 solution, placed in a muffle furnace for 30 minutes and then burned at 120°C for 3h (oxygen atmosphere), the catalyst treated in this way was put into a conical flask, 50g of methanol was added, fully stirred, and the temperature of the control system was 50 °C, reflux for 5 hours. Then suction filtration to remove the carrier, distill methanol at 85°C to obtain a distillate containing hetero...
Embodiment 3
[0054] Weigh 2 grams of supported heteropolyacid catalyst deactivated in the alkylation reaction of isobutane and butene, the active component of the catalyst is phosphotungstic acid H 3 PW 12 o 40 , the content is 25% by weight, and the carrier is a silica-alumina mixture, namely SiO 2 -Al 2 o 3 . Add this catalyst and 2g concentration in crucible and be the HNO of 40% by weight3 Aqueous solution, stirred evenly and left for 0.5h, put the above system into a muffle furnace and burn at 175°C for 2.5h (oxygen atmosphere), repeat 3 times. After taking out and cooling, put the catalyst into an Erlenmeyer flask, add 20 g of methanol, fully stir on a magnetic stirrer, control the temperature of the system at 10° C., and process for 24 hours. Then the carrier is removed by suction filtration, methanol is steamed out at 85°C to obtain a residue containing heteropolyacid; add 6g of water to dissolve the residue of heteropolyacid, then add 2 grams of 65% by weight nitric acid and ...
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