Nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst and preparing method and application thereof
A tungsten carbide catalyst and co-doping technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of active center trouble synthesis, complicated manufacturing process, low yield, etc., and achieve structural Controllable, clear structure, good dispersion effect
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[0032] Example 1
[0033] A method for preparing a carbon-supported molybdenum carbide catalyst supported by co-doped nitrogen and phosphorus includes the following steps:
[0034] (1) Heteropoly acid (NH 4 ) 4 [NiMo 6 O 24 H 6 ](NiMo 6 ) Synthesis: 5.00g (4.2mmol) (NH 4 ) 6 Mo 7 O 24 Dissolve in 80ml of deionized water, stir and heat the solution to boiling, then add 20ml containing 0.76g (3.0mmol) NiSO 4 ·7H 2 The aqueous solution of O was slowly added dropwise to the boiling aqueous solution of ammonium molybdate, and recrystallized twice in water to obtain colorless crystals, namely (NH 4 ) 4 [NiMo 6 O 24 H 6 ](NiMo 6 ).
[0035] (2) Preparation of SEP (Surfactant encapsulate polyoxometalate) composite material: 1.08g (1.0mmol) (NH 4 ) 3 [NiMo 6 O 24 H 6 ] Dissolved in 80mL deionized water (A solution), 2.20g (10.0mmol) cetyltrimethylammonium bromide (surfactant) dissolved in 20mL ethanol (B solution); at a temperature of 85 ℃, vigorously Under stirring, add B solution to A solut...
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[0041] Example 2
[0042] A method for preparing a carbon-supported molybdenum carbide catalyst supported by co-doped nitrogen and phosphorus includes the following steps:
[0043] (1) Heteropoly acid (NH 4 ) 4 [(HPO 3 ) 2 Mo 5 O 15 ]·4H 2 Synthesis of O: Dissolve 4.1g of phosphorous acid (50mmol) in 70mL of water, then add 7mL of 15mol / L ammonia (105mmol), heat the solution to boiling, add 14.4g of MoO to the solution several times 3 (100mol), the powder is dissolved after 40~45min, the solution is filtered, the filtrate is boiled and evaporated to reduce the volume to 20~25mL, and then cooled to room temperature, the crystalline powder is collected by filtration, washed with 7mL ice water, dried in the air to obtain colorless The crystal is (NH 4 ) 4 [(HPO 3 ) 2 Mo 5 O 15 ]·4H 2 O.
[0044] (2) Preparation of SEP (Surfactant encapsulate polyoxometalate, surfactant-coated heteropoly acid) composite material: 0.54g (0.5mmol) (NH 4 ) 4 [(HPO 3 ) 2 Mo 5 O 15 ]·4H 2 O was dissolved in 8...
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[0048] Example 3
[0049] A method for preparing a carbon-supported molybdenum carbide catalyst supported by co-doped nitrogen and phosphorus includes the following steps:
[0050] (1) Heteropoly acid (NH 4 ) 6 [NiMo 9 O 32 ]·6H 2 Synthesis of O: 10mL of Ni(NO) with a concentration of 0.01mol / L 3 ) 2 And 0.1mol / L (NH 4 ) 2 Mo 7 O 24 The mixed solution was heated to 70°C, and then 10mL of ammonium persulfate solution with a concentration of 0.01mol / L was added, and 0.1mol / L of H 2 SO 4 Adjust the pH of the reaction system to 4.4, and then boil the solution for half an hour. Finally, the solution was slowly cooled overnight to obtain black-red crystals. The crude product is obtained by suction filtration, and then the crude product is recrystallized 3-5 times and dried at 60°C. The colorless crystals obtained are (NH 4 ) 6 [NiMo 9 O 32 ]·6H 2 O.
[0051] (2) Preparation of SEP (Surfactant encapsulate polyoxometalate) composite material: 1.08g (1.0mmol) (NH 4 ) 3 [NiMo 6 O 24 H 6 ] Dis...
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