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A kind of preparation method of trinuclear nickel-vanadium oxide cluster catalyst and use thereof
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A catalyst, vanadium oxide technology, applied in the preparation of organic compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problem of difficult recovery of catalysts
Active Publication Date: 2021-05-25
LIAOCHENG UNIV
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[0010] The purpose of this invention is to solve the problems such as the difficult recovery of the catalyst during the Knoevenagel condensation reaction catalyzed by the polymetallic oxygen cluster catalyst
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Embodiment 1
[0030] Embodiment 1: Compound [Ni(1-mIM) 4 ][Ni(H 2 O) 5 ] 2 V 10 o 28 4H 2 Preparation of O
[0031] Add vanadium pentoxide (5mmol), tetramethylammonium hydroxide (10mmol), distilled water 2000mmol, Ni(NO 3 ) 2 (1mmol) and 1-methylimidazole (6mmol), stirred vigorously for 10h, then raised the temperature to 40°C, reacted for 30min, cooled to room temperature after the reaction, filtered, stood still, the filtrate slowly volatilized, and a red substance was obtained after 4 days. Yield about 34%.
Embodiment 2
[0032] Embodiment 2: Compound [Ni(1-mIM) 4 ][Ni(H 2 O) 5 ] 2 V 10 o 28 4H 2 Preparation of O
[0033] Add vanadium pentoxide (5mmol), tetramethylammonium hydroxide (20mmol), distilled water 3000mmol, Ni(NO 3 ) 2 (1mmol) and 1-methylimidazole (10mmol), stirred vigorously for 16h, then raised the temperature to 30°C, reacted for 50min, cooled to room temperature after the reaction, filtered, stood still, the filtrate slowly volatilized, and a red substance was obtained after 4 days. Yield about 39%.
Embodiment 3
[0034] Embodiment 3: Compound [Ni(1-mIM) 4 ][Ni(H 2 O) 5 ] 2 V 10 o 28 4H2 Preparation of O
[0035] Add vanadium pentoxide (10mmol), tetramethylammonium hydroxide (20mmol), distilled water 3000mmol, Ni(NO 3 ) 2 (2mmol) and 1-methylimidazole (15mmol), stirred vigorously for 20h, then raised the temperature to 40°C, reacted for 60min, cooled to room temperature after the reaction, filtered, stood still, the filtrate slowly volatilized, and a red substance was obtained after 5 days. Yield about 57%.
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Abstract
The invention discloses a preparation method of a single-component three-center catalyst of a trinuclear nickel-vanadium oxygen cluster. In the method, vanadium pentoxide, tetramethylammonium hydroxide, distilled water, Ni(NO 3 ) 2 And 1-methylimidazole is placed in the reactor, vigorously stirred, then heated up, reacted, cooled to room temperature after the reaction, filtered, left to stand, the filtrate slowly volatilized, and a single-component three-center catalyst of the trinuclear nickel-vanadium oxide cluster was obtained. Catalyst crystals. The method of the invention has the advantages of fast reaction speed, simple reaction process, high purity of the obtained product and simple aftertreatment. In the Knoevenagel condensation reaction, the yield is as high as 99%.
Description
[0001] Summary [0002] This patent relates to a technical method for preparing a trinuclear nickel-vanadium oxide cluster catalyst by using an imidazole nickel complex and two water nickel complexes to interact with vanadium oxide clusters. The novel trinuclear nickel-vanadium oxycluster catalyst in the present invention has better catalytic activity in the Knoevenagel condensation reaction. technical field [0003] The invention belongs to the technical field of catalyst material preparation, and relates to the preparation technology of a tri-nuclear nickel-vanadium oxygen cluster catalyst. [0004] technical background [0005] Polyoxometallic clusters, also known as polyacids or polyoxometallates, are metal oxygen cluster compounds containing transition elements such as molybdenum, tungsten, vanadium, niobium and tantalum in their structures. In polymetallic oxygen clusters, because they can be designed and synthesized at the molecular level, and have a variety of metal ...
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