Method for catalytically synthesizing diethoxymethane by ionic liquid

A technology of ionic liquids and cations, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of deactivation, low yield of target products, easy carbon deposition on the surface of catalysts, etc., and achieve mild reaction conditions, The effect of low corrosion and simple reaction process

Inactive Publication Date: 2017-06-20
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Solid acid overcomes the shortcomings of liquid acid, such as difficulty in separation and severe corrosion, but the yield of target product is generally low, and the surface of the catalyst is prone to carbon deposition and deactivation

Method used

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  • Method for catalytically synthesizing diethoxymethane by ionic liquid
  • Method for catalytically synthesizing diethoxymethane by ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0038] In a 100mL autoclave, add 4.3g / 0.1mol (70%) formaldehyde solution, 0.73g / 2.3mmol ionic liquid a and 13.6g / 0.3mol ethanol successively, close the reactor, and use 1.0MPa of N 2 Replace the air in the reaction system, fill with N 2 to 1.0MPa. Stir and heat up to 120 within 30 minutes o C, react for 1h under the condition of 2.0 MPa. After the reaction is completed, cool to room temperature and release the pressure. GC analysis, quantification by internal standard method. The conversion of formaldehyde was 81.3% and the selectivity to diethoxymethane was 95.5%.

Embodiment 2

[0040] Same as Example 1, using 0.85g / 2.3mmol catalyst b, the conversion rate of formaldehyde is 82.1%, and the selectivity of diethoxymethane is 95.8%.

Embodiment 3

[0042] Same as Example 1, using 0.72g / 2.3mmol catalyst c, 60% formaldehyde aqueous solution as the reaction raw material, and the feeding amount is 5.0g / 0.1mol. The conversion of formaldehyde was 78.2%, and the selectivity to diethoxymethane was 96.1%.

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Abstract

The invention discloses a method for catalytically synthesizing diethoxymethane by ionic liquid. The method takes the ionic liquid as a catalyst and takes formaldehyde and ethanol as reactants to react for 0.5h to 6h in a nitrogen atmosphere under conditions that the reaction temperature is 80 DEG C to 160 DEG C and the reaction pressure is 0.5Mpa to 5.0MPa; a positive ion part of the ionic liquid is selected from imidazole positive ions, pyridine positive ions, quaternary ammonium positive ions, quaternary phosphonate positive ions and heterocyclic positive ions. According to the method disclosed by the invention, raw materials are obtained from coal chemical industry and biomass and are cheap and easy to obtain; the catalyst has high activity, can be repeatedly used, has low corrosion and has no special requirements on equipment; reaction conditions are moderate, and reaction and separation processes are simple.

Description

technical field [0001] The invention relates to a method for synthesizing diethoxymethane through the acetalization reaction of formaldehyde and ethanol by using ionic liquid as a catalyst. Background technique [0002] Diethoxymethane, also known as diethanol formal (DEM), has a boiling point of 88°C and a solubility in water of 4.4% (20°C). It has a low affinity for water and can form a binary azeotrope with water and ethanol. ;Has good stability, stable under strong alkali and weak acid conditions such as hydroxide, sodium hydride, Grignard reagent, etc., and is not easy to form peroxide; low viscosity, good brushing performance. As a more economical solvent, DEM is increasingly used in organic synthesis, extraction, dilution, recrystallization and other fields, and it is very likely to replace some common solvents such as tetrahydrofuran (THF), ethyl acetate, dichloroethane, toluene , Ethylene oxide, methyl tert-butyl ether, etc., to achieve industrial applications. In...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C43/30
CPCC07C41/56C07C43/30
Inventor 陈静宋河远金福祥康美荣
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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