Metal carbonyl cobalt cluster and Ti bridged complex, preparation method and application

A technology of cobalt carbonyl and complexes, which is applied in the field of synthesis gas-to-oil catalyst preparation, and can solve problems such as inhomogeneity and random distribution of additive components

Inactive Publication Date: 2012-12-19
INNER MONGOLIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a bridging cobalt carbonyl heterometallic cluster complex, in which cobalt The cobalt atom of the cluster is in the zero oxidation state and is the active component of the FT reaction catalyst, while the rare earth or transition metal (Ti, Zr) exists in the normal valence state and is the auxiliary component of the FT reaction catalyst

Method used

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  • Metal carbonyl cobalt cluster and Ti bridged complex, preparation method and application
  • Metal carbonyl cobalt cluster and Ti bridged complex, preparation method and application
  • Metal carbonyl cobalt cluster and Ti bridged complex, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] ln 2 {OOCμ 3 -CCo 3 (CO) 9} 2 {μ-OOCCF 3} 4 {(CO) 9 co 3 mu 3 -CCOOH} 4 Synthesis of (Ln=La, Ce, Eu) (I)

[0050]

[0051] Will (CO) 9 co 3 CCOOH (0.500g, 1.0mmol) and Ln(OOCCF 3 ) 3 (0.5mmol) dissolved in THF solvent, in 50mL Schlenk bottle N 2 React under protection, stir at 30°C for 1 h to obtain a purple-black solution, and remove the solvent in vacuo. The solid was extracted with hot toluene, and the extract was left at room temperature for 2 days to obtain about 400 mg of black crude crystals, with a yield of about 80% (calculated as Ln).

[0052] Elemental analysis (%, calculated value in brackets), C 74 h 4 co 18 f 12 o 74 Eu 2 : C24.35 (24.22), H 0.43 (0.11), Co 27.96 (28.91), Eu 7.97 (8.28); IR (KBr, cm -1 )2111(m), 2054(vs), 1708(m), 1678(m), 1608(m), 1479(w), 1466(w), 1407(w), 1368(w), 1337(w) , 1265(w), 1205(m), 1155(w), 1062(w), 1028(w), 781(w), 723(w), 528(w), 504(m).

[0053] C 74 h 4 co 18 f 12 o 74 La 2 : C 24.80 (24.40...

Embodiment 2

[0056] Ti 4 (μ 3 -O) 4 (OCH 2 CH 3 ) 4 {μ-[(CO) 9 co 3 (μ 3 -CCO 2 )]} 4 Synthesis of (II)

[0057]

[0058] Will (CO) 9 co 3 CCOOH (0.9700g, 2.0mmol) and liquid Ti(OCH 2 CH 3 ) 4 (0.22mL, 1.0mmol) with THF as solvent, in 50mL Schlenk bottle N 2 React under protection, stir at room temperature for 12h to obtain a purple-black solution, and remove the solvent in vacuo. The obtained solid was washed with ethanol until the solution was almost colorless, and then the washed solid was dissolved in 20 ml of dichloromethane, placed at 4° C. for one week, and 350 mg of crystals were collected. Yield 70% (as Ti).

[0059] Elemental analysis (%, calculated value in brackets), C 52 h 20 co 12 Ti 4 o 52 : C: 26.18 (26.29), H: 1.12 (0.85); IR (KBr, cm -1 )2109(m), 2054(vs), 1633(m), 1490(w), 1382(m), 1338(w), 1120(w), 1073(w), 1030(m), 927(w) , 727(w), 618(w), 553(m), 535(m), 502(m).

Embodiment 3

[0061] Yb 4 -O{μ-[Co 3 (CO) 9 mu 3 -CCOO]} 6 Synthesis of (IV)

[0062]

[0063] Will (CO) 9 co 3 CCOOH (0.500g 1.0mmol) and Yb (CF 3 COO) 3 2H 2 O (0.1263g 0.2467mmol) with THF as solvent, in 50mL Schlenk bottle N 2 React under protection, stir at 30°C for 9h to obtain a purple-black solution, and remove the solvent in vacuo. The solid was extracted with hot toluene, and the extract was placed in dichloromethane solvent at room temperature for one week to obtain black crystals.

[0064] Elemental analysis (%, calculated value in brackets): C 67 co 18 o 69 Yb 4 , C: 21.90 (21.85), O: 30.08 (30.12), Co: 28.90 (28.81), Yb: 18.85 (18.79); IR (KBr, cm -1 ): 2109(m), 2011(vs), 1708(m), 1678(m), 1619(m), 1456(w), 1386(w), 1203(m), 1152(w), 1086(w ), 791(w), 752(w), 727(w), 554(w), 502(m).

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Abstract

The invention discloses a metal carbonyl cobalt cluster and Ti bridged complex, a preparation method and an application of the complex in fixed bed or slurry bed catalytic reaction of production of fuel from syngas (F-T reaction). The complex has a structural formula as shown in specification. The catalyst of the invention has simple and convenient preparation method and adjuvant elements and active components in a molecular form are introduced at the same time, wherein, an adjuvant and the active components are distributed uniformly, and the adjuvant has obvious effects, thus effectively improving activity and selectivity of the catalyst.

Description

[0001] This application is a divisional application with the patent application number 201010166936.3, the filing date is 2010.05.10, and the invention title is "A Class of Cobalt Cluster-Heterometallic Bridging Complex and Its Preparation and Application as a Syngas-to-oil Catalyst". technical field [0002] The invention relates to a preparation method and structural characteristics of a metal carbonyl cobalt cluster and other heterometallic bridging complexes, as well as a preparation method and application as a synthesis gas-to-oil (F-T synthesis reaction) catalyst. Background technique [0003] Cobalt-based catalysts are a class of catalysts with excellent performance for Fischer-Tropsch (F-T) synthesis and processing of hydrocarbon products. They have high CO hydrogenation activity, strong F-T chain growth ability, CO 2 It has the advantages of low selectivity, less generation of oxygen-containing compounds, stable reaction process and less carbon deposition and poisoni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00B01J31/26B01J31/22C10G2/00
Inventor 苏海全白凤华曾尚红杜东平王晶李雪芬张银霞
Owner INNER MONGOLIA UNIVERSITY
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