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Preparation method and application of amine functional mesoporous silica-gel-loaded gold catalyst

A technology of mesoporous silica gel and amine functionalization, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of difficult practical application, complicated preparation and increased cost, and achieves high feasibility and simple process. , the effect of low equipment requirements

Inactive Publication Date: 2014-04-09
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the above-mentioned preparation method is concerned, the actual loading amount of gold in the deposition-precipitation method is usually 55-75% of the designed amount, and the remaining Au 3+ The recovery of the material greatly increases the cost, and this method is only suitable for oxide carriers with an isoelectric point ≥ 6
However, the immobilization of organic complexes and the construction of core-shell nanoreactors have the disadvantages of high cost, complicated preparation, and difficulty in practical application, and the catalysts obtained by these methods are mostly used in the fields of CO oxidation and gas purification.

Method used

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  • Preparation method and application of amine functional mesoporous silica-gel-loaded gold catalyst
  • Preparation method and application of amine functional mesoporous silica-gel-loaded gold catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In a mixed solvent composed of 70 mL of water and 20 mL of n-octanol, add 0.5 g of cetyltrimethylammonium bromide, and stir vigorously for 1 h at a controlled temperature of 45 ° C; add 0.8 mL of concentrated ammonia water, and continue stirring for 0.5 h; Add 3.0mL tetraethyl orthosilicate, continue to stir for 5h; filter with suction, dry at 90°C for 12h; then bake at 500°C to obtain mesoporous silica gel nanospheres; weigh 2.0g of silica gel nanospheres, add 80ml of toluene, 2.0ml3- Aminopropyltriethoxysilane, reflux at 110°C for 16h, filter with suction, wash with ethanol, and dry at 90°C for 12h to obtain amine-functionalized mesoporous silica gel; weigh 0.4g of amine-functionalized mesoporous silica gel, and add 20ml of deionized water in turn , 0.4 mL of 0.1 M chloroauric acid solution, centrifuged, and dried at 90° C. for 12 hours to obtain a nano-gold catalyst with a gold content of 2.5 wt%. The finished product is nano-spherical and uniformly pink in color.

...

Embodiment 2

[0042] Catalyst preparation method is the same as embodiment 1.

[0043] In a 100mL round bottom flask, 20mg of catalyst, 5mL of acetonitrile, 2mL of hydrogen peroxide, and 12mmoL of diphenyl sulfide were added, and the reaction was carried out at 60°C for 3h. The conversion of diphenyl sulfide was 97.6%, and the selectivity of sulfoxide was 89.2%.

Embodiment 3

[0045] In the mixed solvent composed of 50mL water and 20mL ethanol, add 4ml nonylphenol polyoxyethylene ether, under the control temperature of 35°C, stir vigorously for 1h; add concentrated ammonia water 0.8mL, continue stirring for 0.5h; add tetraethyl orthosilicate Esters 3.0mL, continue stirring for 4h; filter with suction, dry at 90°C for 12h; then roast at 600°C to obtain mesoporous silica gel nanospheres; weigh 1.0g silica gel nanospheres, add 60ml toluene, 1.0ml 3-aminopropyltriethoxy base silane, reflux at 110°C for 18h, filter with suction, wash with ethanol, and dry at 90°C for 12h to obtain amine-functionalized mesoporous silica gel; weigh 0.4g of amine-functionalized mesoporous silica gel, add 20ml of deionized water, 0.1M [Au (en) 2 ] Cl 3 0.5 mL of the solution was centrifuged and dried at 90° C. for 12 hours to obtain a nano-gold catalyst with a gold content of 3.0 wt %. The finished product is nano-spherical and uniformly pink in color.

[0046] In a 100mL...

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Abstract

The invention discloses a nano gold catalyst and a preparation method, in particular to a preparation method of an amine functional mesoporous silica-gel-loaded gold catalyst. The amine functional mesoporous silica-gel-loaded gold catalyst consists of Au, Si, C, O, N and the like, wherein Au is used as a catalyst active component, and the content of Au is 0.1 to 10 percent. The preparation method of the catalyst is processed in two steps and comprises the following steps of adding a silicon source into a water-ammonia water-organic solvent consolute system to obtain a mesoporous silica-gel nano-ball; carrying out amine functionalization on the mesoporous silica-gel nano ball by utilizing the 3-amino propyl triethoxysilane, and finally loading the nano gold. The nano gold catalyst and the preparation method have the advantages that the load rate of the gold is high, the dispersion property is good, and the catalyst is simple to prepare and good in stability. The catalyst has excellent catalytic property in the olefin epoxidation reaction and oxidation reaction of thioether to sulfoxide, the conversion rate of the catalyst for the styrene oxidation reaction can reach up to 96.8 percent, and the oxidation selectivity is stabilized at 83.7 percent; the conversion rate of the thioether in the oxidation reaction to sulfoxide is 100 percent, and the selectivity of the methyl phenyl sulfoxide is 89.5 percent.

Description

technical field [0001] The invention relates to a preparation method and application of a high-performance amine-functionalized mesoporous silica gel-loaded nano-gold catalyst. The catalyst is used for the epoxidation of olefins and the selective oxidation of sulfides to sulfoxides, and can also be used for other catalytic oxidations reaction. Background technique [0002] Olefin epoxides are a class of organic raw materials and intermediates with a wide range of uses, and are widely used in petrochemical, fine chemical and organic synthesis fields. Among them, epoxides of low-carbon olefins, such as ethylene oxide and propylene oxide, are raw materials or semi-finished products for the synthesis of polyurethane, polyester, amino alcohol, and surfactants; and cyclohexane oxide can participate in Many reactions generate many derivatives, which are raw materials for the production of pesticides, medicines, paints, dyes and vulcanizing agents for rubber products; as an importa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52C07D303/04C07D301/19C07C317/14C07C317/04C07C315/02
Inventor 王芳
Owner NANJING UNIV OF TECH
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