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Silicon dioxide loaded copper-dipyridyl catalyst and its preparation method

A technology of silicon dioxide and bipyridine, applied in the field of copper-bipyridine catalyst and preparation thereof, can solve the problems of difficult separation and recovery, equipment corrosion, large feeding amount of organic ligands, etc., so as to overcome the problems of large feeding amount and easy separation. Effect

Active Publication Date: 2017-09-19
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN1197792A (1998) is based on cuprous chloride, magnesium chloride, calcium chloride etc. are auxiliary agents, prepares composite catalyst, improves the solubility and catalyst activity of cuprous chloride in the reaction solution, but there are still equipment Corrosion problems
However, the non-solid-phase catalysts used in the above-mentioned systems, in addition to the central element copper, have a large amount of organic ligands, high value and difficult to separate and recover.

Method used

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  • Silicon dioxide loaded copper-dipyridyl catalyst and its preparation method
  • Silicon dioxide loaded copper-dipyridyl catalyst and its preparation method
  • Silicon dioxide loaded copper-dipyridyl catalyst and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Take 1.000g of dry nano-silica (50nm diameter) and 1.105g of 3-aminopropyltriethoxysilane into 30mL of dry toluene, keep stirring and heating to 120°C under nitrogen protection, and reflux for 24h. After cooling, the reaction mixture was separated by filtration, and the filter cake was washed three times with 150 mL of toluene, and the solid was vacuum-dried at 50° C. for 3 h to obtain surface-aminated silica.

[0024] Heat 0.070g of 4-formaldehyde-2,2'-bipyridine and 1.000g of surface aminated silicon dioxide in 25mL of toluene solvent under the protection of nitrogen to 120°C and reflux for 20h. After cooling to room temperature, add 6mL of ethanol, 0.072g of sodium borohydride and 0.25mL of glacial acetic acid, and stir for 3 hours. The reaction mixture is separated by filtration, and the filter cake is washed with 100mL of water and ethanol several times in sequence. Dry under vacuum for 3 hours to obtain the surface-modified bipyridyl silica.

[0025] Dissolve 0.0...

Embodiment 2

[0027] Take 1.500g of dry nano-silica (50nm diameter) and 1.265g of 3-aminopropyltriethoxysilane into 30mL of dry toluene, keep stirring and heating to 120°C under nitrogen protection, and reflux for 24h. After cooling, the reaction mixture was separated by filtration, and the filter cake was washed three times with 200 mL of toluene, and the solid was vacuum-dried at 50° C. for 1 h to obtain surface-aminated silica.

[0028] Heat 0.070g of 4-formaldehyde-2,2'-bipyridine and 1.020g of surface aminated silicon dioxide in 30mL of toluene solvent under the protection of nitrogen to 122°C and reflux for 18h. After cooling to room temperature, add 6 mL of ethanol, 0.072 g of sodium borohydride and 0.25 mL of glacial acetic acid, stir for 4 h, filter and separate the reaction mixture, and wash the filter cake with 100 mL of water and ethanol several times in sequence, and place the solid at 50 °C After vacuum drying for 4 hours, the surface-modified bipyridyl silica was obtained.

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Abstract

The invention relates to a silicon dioxide loaded copper-dipyridyl catalyst and its preparation method. The catalyst carrier is dipyridyl modified silicon dioxide, and the active component is copper; the mole ratio of the dipyridyl modified silicon dioxide to copper is 0.3-3.5: 1 and weight of Cu of catalyst is 4-6 wt% of the total weight of catalyst. In application of preparing dimethyl carbonate, the selectivity of dimethyl carbonate reaches 99.9%, and yield of dimethyl carbonate exceeds 53%.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a silica-loaded copper-bipyridine catalyst and a preparation method thereof. Background technique [0002] Dimethylcarbonate (Dimethylcarbonate, DMC for short) is an important class of carbonates with wide application prospects. It contains active reactive groups such as alkyl, alkoxy, carbonyl and alkylcarbonyl in its molecule, so it can react with alcohols, phenols, amines and esters, and can be used as an alkylation, carbonylation and alkylcarbonylation reagent , is an important organic synthesis intermediate, widely used in medicine, pesticide and other industries; secondly, dialkyl is a solvent with excellent performance, and has good compatibility with many solvents, and can be used as paint, cellulose and resin and other solvents are used; the battery with carbon material as the anode, if its electrolyte is composed of 50-90wt% dimethyl ca...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C68/00C07C69/96
CPCB01J31/1633B01J31/1815B01J2531/0238B01J2531/16C07C68/01C07C69/96Y02P20/50
Inventor 陈静黄世俊苏伟平
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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