Preparation method for substituted molybdophosphate crystal catalyst
A technology of phosphate crystals and catalysts, which is applied in the chemical field, can solve the problems of difficult recovery of catalysts, harsh reaction conditions, and easy pollution, and achieve the effects of low cost, mild reaction process conditions, and easy recovery
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Embodiment 1
[0021] A kind of preparation method of substituted molybdophosphate crystal catalyst, this method is divided into two steps, the first step, sodium molybdate Na 2 MoO 4 2H 2 O, transition metal sulfate, phosphoric acid H3PO4 and 1,3-2 (4-pyridyl)-propane or ethylenediamine are mixed in water with a mole fraction of 2000 in a ratio of 6:2.9:30:2.6 , and stirred for 30 minutes to obtain a mixed solution; in the second step, the mixed solution obtained in the first step was sealed in a stainless steel reactor lined with polytetrafluoroethylene, and the filling degree was 60-70%, and then the reactor was placed in 165°C Heating and crystallizing in an oven for 7 days, and then naturally cooling to room temperature, the dark red polyacid crystal catalyst was obtained.
Embodiment 2
[0023] The preparation method of the substituted type molybdophosphate crystal catalyst described in embodiment 1, with 1.45 gram of sodium molybdate Na 2 MoO 4 2H 2 O, 0.52 g zinc sulfate ZnSO 4 ·H 2 O, 2 mL H 3 PO 4 , 0.38 grams of 1,3-2 (4-pyridyl)-propane was mixed in 36 milliliters of water, stirred at room temperature for 30 minutes, and the resulting mixed solution was sealed in a stainless steel reactor lined with polytetrafluoroethylene, and the filling degree was 65%. Then put the reaction kettle into a 165°C oven and heat it for 7 days, then cool it naturally to room temperature to obtain a deep red massive polyacid crystal catalyst; the polyacid crystal catalyst is a pure compound, and its chemical formula is
[0024] (H 2 bpp) 3 [Zn 3 Mo 12 VO 24 (OH) 8 (HPO 4 ) 6 (PO 4 ) 2 ]·2H 2 O) bpp = 1,3-2(4-pyridyl)-propane).
Embodiment 3
[0026]The preparation method of the substituted type molybdophosphate crystal catalyst described in embodiment 1, with 1.45 gram of sodium molybdate Na 2 MoO 4 2H 2 O, 0.56 g ferrous sulfate FeSO 4 ·H 2 O, 2 mL phosphoric acid H 3 PO 4 , 0.32 g of ethylenediamine was mixed in 36 ml of water, stirred at room temperature for 30 minutes, the resulting mixture was sealed in a stainless steel reactor lined with polytetrafluoroethylene, and the filling degree was 65%, and then the reactor was placed in a 165°C oven Heating at a constant temperature for 7 days, and then naturally cooling to room temperature, obtained the dark red massive polyacid crystal catalyst; the polyacid crystal catalyst is a pure compound, and its chemical formula is
[0027] (H 2 en) 3 (Hen)[Fe III 3 Mo 12 V o 24 (OH) 8 (HPO 4 ) 4 (PO 4 ) 4 ]·3H 2 O (en = ethylenediamine).
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