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Novel epoxidation catalyst, preparation method and applications

A technology for epoxidation and catalysts, which is applied in the field of preparation of new epoxidation catalysts, can solve the problems of unstable transition metal complexes, difficulty in catalyst recycling, difficult recovery of ligand synthesis, etc., and achieves strong substrate universality, Effect of constant conversion and selectivity, high stability

Inactive Publication Date: 2012-09-12
HENAN VOCATIONAL COLLEGE OF CHEM TECH
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Problems solved by technology

[0004] In order to solve the problems that the transition metal complexes used as epoxidation catalysts are unstable, easy to decompose, difficult to recycle, complex ligand synthesis, or difficult to recycle the catalyst, the purpose of the present invention is to provide a stable performance, easy The recovery and synthesis method are simple, the synthesis process is easy to operate, and the preparation method and use of a new type of epoxidation catalyst with good epoxidation catalytic effect

Method used

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  • Novel epoxidation catalyst, preparation method and applications
  • Novel epoxidation catalyst, preparation method and applications
  • Novel epoxidation catalyst, preparation method and applications

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preparation example Construction

[0026] Preparation of molybdenum dioxide adduct:

[0027] ①According to the molar ratio, add 0.01 molar parts of sodium molybdate to 20 mL of concentrated hydrochloric acid, stir and dissolve at room temperature, extract three times with 300 parts of ether, dry overnight with anhydrous sodium sulfate, and remove the solvent by rotary evaporation to obtain dichlorodioxygen Molybdenum crystals, dissolved molybdenum dichloride crystals in tetrahydrofuran and rotary evaporation in the dark, to obtain flaky light yellow molybdenum dichloride and tetrahydrofuran solvent adduct MoO 2 Cl 2 (THF) 2 .

[0028] ② Dissolve 0.1 mole part of molybdenum trioxide in 30 mL of hydrochloric acid with a concentration of 6 mol / L under heating, add acetylacetone after cooling, and precipitate white crystals as molybdenum dioxide acetylacetonate adduct MoO 2 (acac) 2 .

Embodiment 1

[0030] The preparation of chlorotetrahydrofuran dioxy molybdenum 8-hydroxyquinoline salt (a): under stirring, the solvent adduct MoO 2 Cl 2 (THF) 2 (0.5mmol) in tetrahydrofuran (THF) 20mL was added to ligand 8-hydroxyquinoline (0.5mmol) in 20mL THF solution. The color of the solution immediately changed to yellow. After stirring at room temperature for 30 minutes, a straight yellow microcrystalline precipitate formed. The precipitate was separated, washed three times with n-hexane, and dried to obtain molybdenum dioxymolybdenum monochlorotetrahydrofuran 8-hydroxyquinoline salt complex (a) as a solid with a yield of 87%.

Embodiment 2

[0032] O-phenanthroline dichlorodioxymolybdenum complex (b) preparation: under stirring, the solvent adduct MoO 2 Cl 2 (THF) 2 (0.5mmol) of tetrahydrofuran (THF) solution 20mL was added in 20mL THF solution of ligand o-phenanthroline (0.5mmol), and the color of the solution immediately turned into light pink. After stirring at room temperature for 50 minutes, a pale pink precipitate formed. The precipitate was separated and washed three times with n-hexane to obtain pale pink microcrystalline complex (b) with a yield of 90%.

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Abstract

The invention discloses a novel epoxidation catalyst, a preparation method and applications. The novel epoxidation catalyst adopts molybdenum dioxide adduct and 8-hydroxyquinoline or 1, 10-phenanthroline as bidentate ligand to synthesize four types of molybdenum (VI) complexes which are monochloro tetrahydrofuran dioxo-molybdenum 8-tumex, 1, 10-phenanthroline dichloro-dioxo molybdenum complex, di (8-tumex) dioxo-molybdenum complex and 1, 10-phenanthroline acetylacetone dioxo molybdenum complex. The structural formulas are shown in the specification. The molybdenum (VI) complexes containing 8-hydroxyquinoline or 1, 10-phenanthroline ligand has the advantages that the properties are stable, the recovery is easy, the synthetic method is simple, the synthetic process is easy to operate, and the epoxidation catalytic effect is good; and the substrate of the epoxidation catalyst is strong in universality, and the epoxidation catalyst is high in activity and good in selectivity, so that the production efficiency of the epoxidation industry is improved, and the cost is reduced.

Description

technical field [0001] The invention relates to a class of epoxidation catalysts, in particular to a preparation method and application of a class of novel epoxidation catalysts. Background technique [0002] Epoxides are important organic synthesis intermediates, widely used in petrochemical, fine chemical, organic synthesis and other industries, and play an important role in the national economy. At present, the domestic demand for epoxides is large, but it mainly depends on imports, which are expensive. The epoxidation of alkenes is one of the important organic synthesis reactions for the preparation of epoxides. Epoxide preparation methods include chlorohydrin method, organic peracid method and hydrogen peroxide method, etc., but the epoxidation reactions such as organic peracid method and hydrogen peroxide method are used in industrial production, and there are still many problems to be solved urgently. At present, the production of large-scale epoxides mainly adopts ...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07F11/00C07D301/19C07D303/04C07D303/08C07D303/48
Inventor 柴凤兰李敬董玉涛赵玉奇朱东方刘新奇
Owner HENAN VOCATIONAL COLLEGE OF CHEM TECH
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