Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Silicon oxide-loaded ruthenium catalyst modified or unmodified with organic functional group and containing nickel or no nickel, and preparation method and application thereof

A technology of ruthenium catalyst and silica carrier, which is applied in the preparation of organic compounds, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of inability to achieve catalyst reaction activity, substrate universality, harsh reaction conditions, etc., and achieve good The effect of industrial application prospect

Active Publication Date: 2016-01-27
EAST CHINA NORMAL UNIV
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There is no shortage of catalysts with ruthenium as the active component in the current published literature patents, but the content of ruthenium in the active component is relatively high, such as 5-10wt.%; the reaction conditions are harsh, and the temperature is 80-150 ° C; ~5MPa, the reactivity of the catalyst of the present invention and its universality to the substrate in the hydrogenation reaction cannot be achieved

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Silicon oxide-loaded ruthenium catalyst modified or unmodified with organic functional group and containing nickel or no nickel, and preparation method and application thereof
  • Silicon oxide-loaded ruthenium catalyst modified or unmodified with organic functional group and containing nickel or no nickel, and preparation method and application thereof
  • Silicon oxide-loaded ruthenium catalyst modified or unmodified with organic functional group and containing nickel or no nickel, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0104] In a specific embodiment, the preparation method of the organic functional group modified nickel-containing silicon oxide supported ruthenium catalyst of the present invention comprises the following steps:

[0105] (1) Preparation of Ni-containing mesoporous silica:

[0106] Ni(NO 3 ) 2 ·6H 2 O was melted at 60-80°C for 0.5-2 hours, then added solvent ethanol and ground to a paste, and added dried silicon oxide into the paste and ground continuously until uniform, wherein the mass ratio of solvent ethanol to silicon oxide was 0.3~0.6:1. Calcining the obtained green powder at 350-550° C. for 1-4 hours to obtain Ni-containing mesoporous silicon oxide, wherein the mass percentage of nickel is 20-40 wt.%.

[0107] In the above steps, the solvent can also be a low-boiling-point solvent that can dissolve nickel salts such as methanol, isopropanol, and acetone.

[0108] (2) Preparation of nickel-containing silicon oxide nanoparticles wrapped by silicon oxide:

[0109] D...

Embodiment 1

[0118] 2.973g of Ni(NO 3 ) 2 ·6H 2 O was melted at 80°C for 1 hour, then 0.5ml of ethanol was added as a solvent and ground to a paste, and 1.4g of dried SBA-15 was added to the paste and ground continuously until uniform. The resulting green powder was calcined at 550°C in air for 2h. 1 g of the obtained nickel-containing SBA-15 was dispersed in 50 ml of water, 120 ml of ethanol was added to the mixed liquid, and 2 ml of 28% ammonia water was added dropwise. After stirring for 12 h, the collected carrier was filtered and dried at 120° C. for 4 h. Dissolve 0.5 g of dried nickel-containing SBA-15 coated with silicon oxide in anhydrous acetonitrile as a solvent, and after stirring to disperse evenly, add 0.38 ml of trimethylchlorosilane. Stirring was continued for 12 h, the turbid solution was filtered, and dried at 120° C. for 12 h. The resulting product was reduced with hydrogen at 400°C for 2 hours to obtain nickel-containing SBA-15 coated with silicon oxide. Weigh 0.29...

Embodiment 2

[0122] Catalyst preparation is the same as in Example 1.

[0123] The prepared nickel-containing SBA-15 catalyst loaded with ruthenium, coated with silicon oxide and modified with methyl groups, is used for the liquid-phase hydrogenation catalytic reaction of levulinic acid. Take 20mg of the catalyst and put it into the autoclave, add 10ml of 0.25M levulinic acid aqueous solution, fill with 0.5MPa hydrogen, seal the autoclave, control the reaction temperature at 20°C, the speed at 600rpm, and react for 60min to obtain the target product 4-hydroxyvaleric acid, because 4-hydroxyvaleric acid is unstable at room temperature, placed at 80°C for 4 hours to obtain the product γ-valerolactone. The product analysis was carried out by gas chromatography, and the results are shown in Table 1. The steps of magnetic separation application are as follows: figure 2 shown.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle diameteraaaaaaaaaa
particle sizeaaaaaaaaaa
sizeaaaaaaaaaa
Login to View More

Abstract

The invention discloses a silicon oxide-loaded ruthenium catalyst modified or unmodified with an organic functional group and containing nickel or no nickel and a preparation method thereof; the catalyst takes ruthenium as an active component, and ruthenium particles are loaded on a carrier; ruthenium includes metal ruthenium or oxidation-state ruthenium; the weight percentage of the contained ruthenium is 0.5-5 wt.%, the content of the surface organic group is 0.5-10 wt.%, and the loading amount of contained nickel in the nickel-containing silicon oxide-loaded ruthenium catalyst accounts for 10.0-70.0 wt.% of the silicon oxide mass. The particle size of the active component ruthenium nanoparticles is 1-5 nm. Efficient catalytic hydrogenation of carbonyl or other unsaturated bonds is achieved under conditions of the temperature of 20-50 DEG C and low pressure, and the catalyst has the catalytic hydrogenation generality and appropriate hydrophilicity and hydrophobicity, and improves the safety and economical efficiency of a common hydrogenation catalytic reaction system. Moreover, the catalyst has magnetism, is easy to recycle and regenerate, still remains relatively high activity after repeated use, and shows good industrial application value on hydrogenation of a variety of unsaturated functional bonds.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical industry, and relates to a low-temperature, low-pressure, high-efficiency, magnetically-separated hydrogenation catalyst and a preparation method thereof, in particular to a nickel-containing or nickel-free silicon oxide-supported ruthenium catalyst modified or unmodified by an organic functional group and Its preparation method, and its application to the hydrogenation reaction of unsaturated functional groups in biomass-based derivatives (including levulinic acid, ethyl levulinate, furfural, and aromatic hydrocarbons). Background technique [0002] γ-valerolactone is recognized as a versatile platform compound for the preparation of liquid fuels, pharmaceuticals, and chemical synthesis intermediates. As far as it is concerned, its natural fruit flavor is widely used in food additives; in addition, it has the characteristics of low melting point (-31 ° C), high boiling point (207 ° C)...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035C07C69/675C07C67/31C07C59/01C07C51/367C07C35/08C07C29/20C07D307/44C07C13/18C07C5/10
Inventor 关业军叶飞洋孙兴王一萌
Owner EAST CHINA NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products