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Preparation method and application of Pb complex-vanadate substituted phosphomolybdic acid one-component dual-active-center catalyst

A technology of palladium complex and monophosphate is applied in the field of preparation of palladium complex-polymetallic oxygen cluster binary catalyst, can solve the problems of large amount of catalyst, low activity and the like, achieves good catalytic activity, simple preparation method, and is beneficial to The effect of industrial production

Active Publication Date: 2014-01-01
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Palladium complex-polymetallic oxygen cluster binary catalysts can solve the problems of low activity and large catalyst dosage in the selective oxidation of alcohols under ambient pressure when molecular oxygen is the oxidant of pure polymetallic oxygen cluster catalysts

Method used

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  • Preparation method and application of Pb complex-vanadate substituted phosphomolybdic acid one-component dual-active-center catalyst
  • Preparation method and application of Pb complex-vanadate substituted phosphomolybdic acid one-component dual-active-center catalyst
  • Preparation method and application of Pb complex-vanadate substituted phosphomolybdic acid one-component dual-active-center catalyst

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Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: compound [Pd (dpa) (DMSO) 2 ] 2 [HPMo 10 V 2 o 40 ] The preparation of 4DMSO: 2,2'-dipyridylamine, Pd(OAc) 2 and H 5 PV 2 Mo 10 o 40 Join in the reactor that fills dimethyl sulfoxide (control the ratio of the amount of raw material 2,2'-dipyridylamine: Pd(OAc) 2 : H 5 PV 2 Mo 10 o 40 2:3.5:1.5), stirred and reacted at room temperature for 20 minutes, filtered, and the filtrate was slowly evaporated at room temperature, and a rod-shaped single crystal was obtained after 7-9 days. The yield is about 82%.

Embodiment 2

[0029] Embodiment 2: compound [Pd (dpa) (DMSO) 2 ] 2 [HPMo 10 V 2 o 40 ] Preparation of 4DMSO: In a clean beaker, 2,2′-dipyridylamine (3 mmol), Pd(OAc) 2 (3 mmol) and H 5 PMo 10 V 2 o 40 (1 mmol), Pd(dpa)(OAc) 2 (1 mmol) was added to 15 mL dimethyl sulfoxide, mixed and stirred, the resulting solution was stirred at room temperature for 30 min, filtered, and the filtrate was slowly evaporated at room temperature, and a rod-shaped single crystal was obtained after 7 days. The yield is about 84%.

Embodiment 3

[0030] Embodiment 3: compound [Pd (dpa) (DMSO) 2 ] 2 [HPMo 10 V 2 o 40 ] The preparation of 4DMSO: 2,2'-dipyridylamine, Pd(OAc) 2 and H 5 PV 2 Mo 10 o 40 Join in the reactor that fills dimethyl sulfoxide (control the ratio of the amount of raw material 2,2'-dipyridylamine: Pd(OAc) 2 : H 5 PV 2 Mo 10 o 40 2.5:3:1), stirred and reacted at room temperature for 30 minutes, filtered, and the filtrate was slowly evaporated at room temperature, and a rod-shaped single crystal was obtained after 9 days. The yield is about 88%.

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Abstract

The invention relates to a preparation method and application of a Pb complex-vanadate substituted phosphomolybdic acid one-component dual-active-center catalyst. Pb complexes and vanadate substituted phosphomolybdic acid are combined via electrostatic force, and a Pb complex-vanadate substituted phosphomolybdic acid binary catalyst is prepared in a one-pot way. The preparation method is based on coordination substitution and an ion exchange reaction, and has the characteristics of high simplicity, easiness in implementation, operation controllability and the like. The Pb complex-vanadate substituted phosphomolybdic acid one-component dual-active-center catalyst represents better catalytic activity in the selective oxidation of alcohol, and the transformation ratio and selectivity are respectively 92.8 percent and 93.2 percent.

Description

technical field [0001] The invention belongs to the technical field of catalyst material preparation, and relates to the preparation technology of a palladium complex-polymetallic oxygen cluster binary catalyst. Background technique [0002] The selective oxidation of alcohols is an important transformation in the laboratory and chemical industry. The essence of this process is oxidative dehydrogenation. The corresponding products aldehydes or ketones are widely used in the production of chemical industry and the synthesis of fine chemicals. At present, in the industrial production of alcohol oxidation catalysis, stoichiometric or even superstoichiometric metal oxides or metal salts are used as oxidants ((a) G. Cainelli, G. Cardillo, Chromium Oxidants in Organic Chemistry , Springer Press: Berlin, 1984; (b) F. M. Menger, C. Lee, Tetrohedron Lett ., 1981, 22 , 1655-1662.), these substances inevitably produce a large amount of heavy metal pollutants. In recent years, as en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07B41/06C07C45/38C07C45/39C07C47/54C07C47/542C07C47/575C07C47/55C07C49/78C07C49/786C07C201/12C07C205/44C30B7/14C30B29/54
Inventor 迟瑛楠黄现强胡长文张小梅王博
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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