Hydrotalcite-like in situ assembled nano multiple-metal oxygen-containing cluster catalyst and application

An in-situ assembly, hydrotalcite technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. The problem of polymetallic oxygen-containing clusters loading and other problems can be avoided, and the preparation method is simple and the structure stability is good.

Inactive Publication Date: 2011-06-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

However, this goal has not been achieved, mainly because there is a complex chemical equilibrium closely related to the pH value in the self-assembled polyoxometallic cluster solution, in which there are not only target polyoxometallic anions, but also a variety of by-products and Impurity anions, these coexisting anions will seriously affect the loading of target polyoxometallic clusters, and lead to impure products and reduced catalytic performance

Method used

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  • Hydrotalcite-like in situ assembled nano multiple-metal oxygen-containing cluster catalyst and application
  • Hydrotalcite-like in situ assembled nano multiple-metal oxygen-containing cluster catalyst and application
  • Hydrotalcite-like in situ assembled nano multiple-metal oxygen-containing cluster catalyst and application

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preparation example Construction

[0029] The preparation of nanometer polymetallic oxygen-containing cluster refers to the method of the following documents:

[0030] [WZn 3 (H 2 O) 2 (ZnW 9 o 34 ) 2 ] 12- , [WCo 3 (H 2 O) 2 (CoW 9 o 34 ) 2 ] 12- See [J. Chem. Soc., Dalton Trans. (1991), 143];

[0031] [Ni 3 (H 2 O) 3 (PW 10 o 39 )H 2 O] 7- , [Ni 4 (H 2 O) 2 (PW 9 o 34 ) 2 ] 10- , [Ni 9 (OH) 3 (H 2 O) 6 (HPO 4 ) 2 (PW 9 o 34 ) 3 ] 16- Refer to [Inorg.Chem.38(1999), 55];

[0032] [Mn 4 (H 2 O) 2 (PW 9 o 34 ) 2 ] 10- See [Polyhedron 15 (1996), 917];

[0033] [Co 4 (H 2 O) 2 (PW 9 o 34 ) 2 ] 10- ,.[Zn 4 (H 2 O) 2 (PW 9 o 34 ) 2 ] 10- Refer to [J.Chem.Soc.,.Dalton Trans.(1986), 2699];

[0034] [Ti 2 W 10 PO 40 ] 7- Refer to [Inorg.Chem.22(1983), 818];

[0035] [NaP 5 W 30 o 110 ] 14- Refer to [Inorg. Chem. 32(1993), 1573].

Embodiment 1

[0037] Preparation of Hydrotalcite-like In Situ Assembled Nanoscale Polymetallic Oxygen Cluster Catalysts (I)

[0038] (1)[WZn 3 (H 2 O) 2 (ZnW 9 o 34 ) 2 ] 12- (abbreviated as ZnWO) self-assembly. With reference to the method in the literature, 1.9mol Na 2 WO 4 2H 2 O (635g) and 1.75mol HNO 3 (125ml) was dissolved in 1000ml distilled water, poured into the flask, and the flask was placed on a water bath, the temperature of the water bath was 85°C; 0.5mol Zn(NO 3 ) 2 ·6H 2 O (149g) was dissolved in 500ml distilled water and placed in the dropping funnel; the temperature of the water bath was raised to 95°C, and Zn(NO 3 ) 2 Solution, keep stirring vigorously; After the dropwise addition, the translucent or slightly turbid mixed solution is settled to 2000ml with distilled water for later use, and its pH=7.5 is measured, thus a self-assembled ZnWO solution with a molar concentration of 0.05M is prepared.

[0039] (2) 0.6mol Mg(NO 3 ) 2 ·6H 2 O(153.8g) and 0.2mo...

Embodiment 2

[0042] Preparation of Hydrotalcite-like In Situ Assembled Nanoscale Polymetallic Oxygen Cluster Catalysts (II)

[0043] (1)[Ni 4 (H 2 O) 2 (PW 9 o 34 ) 2 ] 10- (abbreviated as NiPWO) self-assembly. With reference to the method of literature, 72mmol Na 2 WO 4 2H 2 O (24g) was dissolved in 60ml distilled water, and 8mmolNa 2 HPO 4 (1.13g), adjust the pH=7.1 of the solution with acetic acid; 16mmol Ni(OAc) 2 4H 2 O (4.02g) was dissolved in 30ml of distilled water and placed in the dropping funnel, and Na was added dropwise at a rate of 2ml / min. 2 WO 4 / Na 2 HPO 4 Mix the solution; after the dropwise addition, dilute the yellow solution to 100ml with distilled water and heat to reflux for 2 hours to obtain a self-assembled NiPWO solution with a molar concentration of 0.04M.

[0044] (2) 0.04mol Zn(NO 3 ) 2 ·6H 2 O(11.9g) and 0.02mol Al(NO 3 ) 3 9H 2O (7.5g) is made into a mixed salt solution with a concentration of 2M with freshly boiled deionized water; 0.1...

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Abstract

The invention relates to a method for preparing a hydrotalcite-like in-situ assembled nanometer polyoxometalate clustering catalyst, and application of the catalyst to liquid phase olefin epoxidation reaction. The method for preparing the catalyst is to directly mix a self-assembled nanometer polyoxometalate clustering solution and an in-situ generated hydrotalcite-like serous fluid under the conditions of a proper temperature and acidity, so that the hydrotalcite-like can selectively assemble nanometer polyoxometalate clustering anions without influence of other co-existing anions, and the hydrotalcite-like in-situ assembled nanometer polyoxometalate clustering catalyst is obtained. The catalyst can be used in the olefin epoxidation reaction taking an aqueous hydrogen peroxide solution as an oxidizing agent, has high catalytic activity and stability, and is applicable to fixed bed continuous reaction.

Description

technical field [0001] The invention relates to a nanometer polymetallic oxygen-containing cluster catalyst assembled by hydrotalcites, specifically a hydrotalcite-like in-situ assembled nanometer polymetallic oxygen-containing cluster catalyst and its preparation. The catalyst can be used in liquid-phase epoxidation reactions . Background technique [0002] Polyoxometallic clusters (also known as polyoxometalates, or heteropolyacids) are an important class of catalytic materials, which can be widely used in reactions such as acid catalysis and redox catalysis. In order to make the catalyst easy to separate from the reaction product and reuse it, the preparation of nanoscale multimetallic oxygen-containing clusters as a supported heterogeneous catalyst is a major approach. Commonly used heterogeneous methods are impregnation and ion exchange. The supported catalyst obtained by the impregnation method is only suitable for non-polar catalytic reaction systems, and the active...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/188B01J23/888B01J21/16C07D301/06
Inventor 李灿刘鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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