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Complex catalyst for synthesizing carbonate ester by using homogeneous oxidation carbonylation of alcohol (S), its prepn. tech. and use

A homogeneous oxidation and preparation technology, which is applied in the preparation of organic compounds, catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, etc. low problems, to achieve the effect of stable catalyst structure, good selectivity and stability, and simple preparation process

Inactive Publication Date: 2006-06-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] However, the catalysts used in the above methods all contain highly corrosive chloride ions, and there are technical problems such as equipment corrosion, large catalyst usage and poor stability.
[0013] Chinese patent CN1376665A proposes a new type of polymer complex catalyst, which uses a divalent copper system with better stability, and uses a high molecular polymer containing heteroatoms as a ligand. Low corrosiveness, but there are problems such as complex catalyst preparation, high toxicity of reaction medium and high reaction pressure
Alcohol / carbon monoxide homogeneous oxidative carbonylation synthesis of carbonate is currently an advantageous industrial method, but there are technical problems such as equipment corrosion, large catalyst usage and poor stability, and the scale of industrialization is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 11.2gCuBr 2 and 42.2g of tetraethylammonium bromide were dissolved in 100ml and 50ml of absolute ethanol or methyl acetate respectively, then the two were mixed, heated and boiled at 80°C, and maintained for about 70min, cooled to room temperature, filtered, and vacuumed Dry at 60°C to get 51.0g brown powder CuBr 2 - Tetraethylammonium bromide catalyst.

Embodiment 2

[0038] In a 1000ml autoclave, add 100ml methanol, 5gCuBr 2 -Tetraethylammonium bromide catalyst (Cu / N=1 / 2), use CO to replace the air in the reactor, then press CO to about 2.0MPa at room temperature, and when heated to 110°C, feed an appropriate amount of O 2 , maintain the reaction pressure at about 3.5MPa, and react for 2.5h. During the reaction process, the consumed CO and O need to be continuously replenished. 2 . After cooling, it was analyzed by gas chromatography. The selectivity of dimethyl carbonate is 99.5%, and the productivity of the catalyst is 2.5gDMC / g.cat.h.

Embodiment 3

[0040] Use 5gCuBr2-tetrabutylammonium bromide (Cu / N=1 / 2) as catalyzer, all the other conditions are with embodiment 2, dimethyl carbonate selectivity is 98.5%, and catalyst productivity is 3.0gDMC / g.cat.h .

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Abstract

A complex catalyst for preparing carbonate from alcohol by homogeneous oxidizing-carbonylating reaction has a chemical formula MXnLm, where M is metal, X is chosen from halogen, SO4 (or HSO4) radical, CO3 (or HCO3) radical, etc, L is chosen from RN4 ion, RP4 ion, pyridine, etc, and m=1-12. It is prepared through complex reaction between quaternary ammonium (or phosphorus) salt and metal salt. Its application method is also disclosed.

Description

technical field [0001] The invention belongs to the field of catalysts, and relates to a complex catalyst for synthesizing carbonates by homogeneous oxidative carbonylation of alcohols, and also relates to a preparation process and a use method of the complex catalyst. Background technique [0002] Carbonate (Carbonate), the general formula is: R and R' are chain alkyl or aromatic groups, R and R' can be the same or different; they can also be cyclic carbonates: R and R' can be alkyl, alkoxy and the like. [0003] Carbonates are a class of compounds that are widely used in industry. For example, carbonate is a high-boiling and highly polar organic solvent with excellent performance, widely used in the synthesis of pharmaceuticals and fine chemical intermediates; it can also be used as a fuel additive to improve the octane number of gasoline and reduce the exhaust gas generated by combustion; it can also be used as Organic compounds such as polycarbonate, polyurethane, a...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J37/00C07C68/00C07C69/96
Inventor 刘晓勤刘定华杨洋姚虎卿
Owner NANJING UNIV OF TECH
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