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Pyridine coordinated copper heterogeneous catalyst and preparation method thereof

A heterogeneous catalyst and catalyst technology, applied in the preparation of carbon monoxide and oxygen, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of difficult separation and recovery, equipment corrosion, and the amount of organic ligands fed Large and other problems, to achieve the effect of overcoming the large amount of feeding and easy separation

Active Publication Date: 2017-09-26
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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  • Pyridine coordinated copper heterogeneous catalyst and preparation method thereof
  • Pyridine coordinated copper heterogeneous catalyst and preparation method thereof
  • Pyridine coordinated copper heterogeneous catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 3.5mL of 3-aminopropyltriethoxysilane and 1.33mL of pyridine in 80mL of dry diethyl ether for later use. Another 2.67g of pyridine-2-formyl chloride hydrochloride was dissolved in 140mL of dry diethyl ether, under a nitrogen atmosphere, under continuous stirring, the diethyl ether solution of aminopropyltriethoxysilane and pyridine was added, and after reacting at room temperature for 21h, the The reaction mixture was filtered to remove solids, and the mother liquor was rotovapped to give a pale yellow oil.

[0024] The product obtained in Step 1 and 3.0 g of dry nano-silica (50 nm in diameter) were heated to 120° C. in 50 mL of dry toluene solvent under the protection of nitrogen, and refluxed for 24 h. After cooling to room temperature, filter and wash the filter cake with toluene several times, and dry the solid in vacuum for 3-5 hours to obtain pyridine-modified silica.

[0025] Dissolve 1.3427g (0.007mol) CuI in 30mL of acetonitrile, add 1.6125g of surfac...

Embodiment 2

[0028] Take 3.000g of dry nano-silica (50nm diameter) and 3.5mL of 3-aminopropyltriethoxysilane into 50mL 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.

[0029]In a nitrogen atmosphere, mix 2.5g of pyridine-2-formyl chloride hydrochloride and 2.34g of surface-aminated silicon dioxide in 50mL of dry toluene, add 15mL of triethylamine under stirring, and reflux overnight at 120°C. Cool to room temperature, filter, and wash the filter cake with water and toluene several times, and dry the solid in vacuum for 3-5 hours to obtain pyridine-modified silica.

[0030] Dissolve 2.228 g of CuI in 50 mL of acetonitrile, add the surface-modified pyridine silica obtained in step 2, and stir and reflux for 24 h under nitrogen pr...

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Abstract

The invention relates to a pyridine coordinated copper heterogeneous catalyst and a preparation method thereof. The carrier of the catalyst is pyridine modified silicon dioxide, and the active component is copper; the molar ratio of the pyridine modified silicon dioxide to the copper is (0.5-1.9):1; in the catalyst, the Cu accounts for 4 to 6 percent of the total weight of the catalyst. In application to preparation of dimethyl carbonate, the selectivity of the dimethyl carbonate reaches 99.9 percent and the yield of the dimethyl carbonate exceeds 54 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a pyridine-coordinated copper heterogeneous catalyst and a preparation method thereof. Background technique [0002] Dimethyl carbonate is a widely used bulk chemical raw material. It has various chemical reactivity and can undergo carbonylation, carbonylmethoxylation and methylation reactions. Moreover, the toxicity of dimethyl carbonate is very low. Europe listed it as a non-toxic chemical as early as 1992. It is an ideal substitute for highly toxic reagents widely used in industries such as phosgene, dimethyl sulfate, and methyl chloroformate. , known as a green chemical product, will become the new cornerstone of chemical synthesis in the future world. After deep processing, dimethyl carbonate can be used as a gasoline additive to replace the environmentally harmful antiknock agent methyl tert-butyl ether, increase the octane number, and effe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C68/00C07C69/96
CPCB01J31/1815B01J2531/0213B01J2531/0241B01J2531/16C07C68/01C07C69/96Y02P20/50
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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