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Preparation method and application of metal oxygen cluster catalyst with stable organic acid

An organic acid and catalyst technology, applied in clean catalysis and green fields, can solve the problems of difficult catalyst separation and recovery, poor stability, etc.

Inactive Publication Date: 2021-05-18
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These homogeneous catalysts face common problems, such as their poor stability under catalytic oxidation reaction conditions and difficulties in catalyst separation and recovery, which limit their applications.

Method used

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  • Preparation method and application of metal oxygen cluster catalyst with stable organic acid
  • Preparation method and application of metal oxygen cluster catalyst with stable organic acid
  • Preparation method and application of metal oxygen cluster catalyst with stable organic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 2.65g niobium oxide (Nb 2 o 5 ) and 5.62g of potassium hydroxide (KOH) were placed in a mortar, ground evenly, transferred to a nickel crucible, roasted at 550°C for 5h, dissolved in water after cooling, and filtered to obtain a clear solution, and then added acetic acid to adjust the pH to about 5, resulting in a large amount of The white precipitate was filtered by suction for 0.5h and dried at 60°C for 0.5h to finally obtain hydrated niobium oxide with a water content of about 70%. The same method can be used to obtain other hydrated metal oxides (V, Ta, Mo, W).

[0038] The above-mentioned hydrated niobium oxide (2.24g, 2.50mmol) and tetrabutylammonium hydroxide (0.65g, 2.50mmol) were mixed and stirred in 20mL ethanol according to the molar ratio of 1:1, and 30% hydrogen peroxide (11.00g, 30mmol) was added, and stirred After clarification, lactic acid (0.23g, 2.50mmol) was added, stirred for 6h, and then heated and evaporated to dryness at 60°C to obtain a reddish-...

Embodiment 2

[0046] 2.65g niobium oxide (Nb 2 o 5 ) and 5.62g of potassium hydroxide (KOH) were placed in a mortar, ground evenly, transferred to a nickel crucible, roasted at 550°C for 5h, dissolved in water after cooling, and filtered to obtain a clear solution, and then added acetic acid to adjust the pH to about 5, resulting in a large amount of The white precipitate was filtered by suction for 0.5h and dried at 60°C for 0.5h to finally obtain hydrated niobium oxide with a water content of about 70%. The same method can be used to obtain other hydrated metal oxides (V, Ta, Mo, W).

[0047] The above-mentioned hydrated niobium oxide (2.24g, 2.50mol) and tetrabutylammonium hydroxide (0.65g, 2.50mol) were mixed and stirred in 20mL ethanol according to the molar ratio of 1:1, and hydrogen peroxide (11.00g, 30mol) was added, and after stirring and clarification Lactic acid (0.23g, 2.50mmol) was added, stirred for 6h, and then heated and evaporated to dryness at 60°C to obtain a reddish-bro...

Embodiment 3

[0051] 2.65g niobium oxide (Nb 2 o 5 ) and 5.62g of potassium hydroxide (KOH) were placed in a mortar, ground evenly, transferred to a nickel crucible, roasted at 550°C for 5h, dissolved in water after cooling, and filtered to obtain a clear solution, and then added acetic acid to adjust the pH to about 5, resulting in a large amount of The white precipitate was filtered by suction for 0.5h and dried at 60°C for 0.5h to finally obtain hydrated niobium oxide with a water content of about 70%. The same method can be used to obtain other hydrated metal oxides (V, Ta, Mo, W).

[0052] The above-mentioned hydrated niobium oxide (2.24g, 2.50mol) and tetrabutylammonium hydroxide (0.65g, 2.50mol) were mixed and stirred in 20mL ethanol according to the molar ratio of 1:1, and hydrogen peroxide (11.00g, 30mol) was added, and after stirring and clarification Lactic acid (0.23g, 2.50mmol) was added, stirred for 6h, and then heated and evaporated to dryness at 60°C to obtain a reddish-bro...

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Abstract

The preparation method comprises the following steps: carrying out high-temperature melting roasting on a metal oxide and potassium hydroxide in a molar ratio of 1:(8-12) for 2-8 hours at 300-800 DEG C, adding water for dissolving and filtering the material, adding acetic acid to adjust the pH value to 4-6, and carrying out suction filtration and drying to obtain a hydrated oxide; then dissolving a hydrated oxide and a cation precursor in ethyl alcohol, adding hydrogen peroxide, stirring and mixing the components, and adding organic acid for coordination, wherein the molar ratio of the hydrated oxide to the cation precursor to the organic acid is (0.5-2):1:1, and the molar ratio of the hydrogen peroxide to the hydrated oxide is 12:1; and evaporating the mixture to dry to prepare the metal oxygen cluster catalyst with the stable organic acid. The metal oxygen cluster catalyst with stable organic acid has the advantages of simple preparation method, cheap and easily available raw materials, high catalytic activity, good stability and recyclability.

Description

technical field [0001] The invention belongs to the technical field of green and clean catalysis, in particular, it relates to a metal oxygen cluster catalyst with a stable structure, which reduces the electron cloud density of the metal center through the coordination of an organic acid, and applies the prepared metal oxygen cluster catalyst to propylene And other selective epoxidation of olefins to prepare epoxy compounds. Background technique [0002] The epoxidation of alkenes and enols plays an important role in industrial and synthetic chemistry. Epoxy compounds are important intermediates in the synthesis of fine chemicals, especially for the manufacture of surfactants, polymers and epoxy resins. However, epoxidation reactions usually use peroxyacids and hazardous organic solvents, which are expensive and environmentally harmful. From both environmental and economical considerations, hydrogen peroxide may be the best oxidizing agent besides oxygen. Also, there are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/04C07D303/04C07D301/12
CPCB01J31/04C07D301/12
Inventor 侯震山丁炳杰周青青
Owner EAST CHINA UNIV OF SCI & TECH