A kind of method for preparing isosorbide ethyl ether

A technology of isosorbide and ethoxylated isosorbide, which is applied in the field of preparing isosorbide ethyl ether, can solve the problems of many by-products, limiting the development and application of isosorbide etherified products, and low yield of etherified products, achieving corrosive mild effect

Active Publication Date: 2016-12-28
DALIAN 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

In summary, in the preparation process of isosorbide etherified derivatives, there are highly toxic halogenated hydrocarbons as etherification reagents, or strong corrosive acids and alkalis as catalysts, or there are many by-products, or the yield of etherification products is low. and many other problems limit the development and application of isosorbide etherification, so it is of great scientific significance and application prospect to seek efficient and green etherification methods

Method used

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  • A kind of method for preparing isosorbide ethyl ether

Examples

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Comparison scheme
Effect test

Embodiment 1

[0023]In a typical preparation, the etherification reaction of isosorbide and ethanol is carried out in a closed reactor. Put ethanol and isosorbide into a stainless steel reaction kettle according to a molar ratio of 50:1, add phosphotungstic heteropolyacid with 5% isosorbide mass, and use sulfolane as an etherification reaction solvent (5 times the mass of isosorbide ), filled with 3MPa nitrogen in advance, sealed the reactor, and reacted with magnetic stirring at 200°C for 2 hours. After the reactor was cooled to room temperature, the reaction solution was taken and analyzed by gas chromatography. The conversion rate of raw material isosorbide and the yield of etherification products were calculated by the internal standard method of gas chromatography. The obtained isosorbide etherification products include 5-ethoxy isosorbide (5-MEI), 2-ethoxy isosorbide (2-MEI) and isosorbide diethyl ether (DEI). Example 2

Embodiment 2

[0024] In a typical preparation, the etherification reaction of isosorbide and ethanol is carried out in a closed reactor. Put ethanol and isosorbide into a stainless steel reaction kettle according to a molar ratio of 50:1, add phosphotungstic heteropolyacid with 30% isosorbide mass, and use sulfolane as an etherification reaction solvent (5 times the mass of isosorbide ), filled with 3MPa nitrogen in advance, sealed the reactor, and reacted with magnetic stirring at 200°C for 2 hours. The conversion rate of raw material isosorbide and the yield of etherification products were calculated by gas chromatography internal standard method.

Embodiment 3

[0026] In a typical preparation, the etherification reaction of isosorbide and ethanol is carried out in a closed reactor. Put ethanol and isosorbide into the stainless steel reaction kettle according to the molar ratio of 50:1, add phosphotungstic heteropolyacid with 50% isosorbide quality, and use sulfolane as the etherification reaction solvent (5 times the isosorbide quality ), filled with 3MPa nitrogen in advance, sealed the reactor, and reacted with magnetic stirring at 200°C for 2 hours. The conversion rate of raw material isosorbide and the yield of etherification products were calculated by gas chromatography internal standard method.

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Abstract

The invention relates to a method for preparing isosorbide ether by directly etherifying isosorbide and ethanol. Raw materials comprising isosorbide and ethanol are directly etherified under the action of an acidic catalyst to synthesize 2-ethoxy isosorbide (2-MEI), 5-ethoxy isosorbide (5-MEI) and isosorbide diethyl ether (DEI), and the total yield of isosorbide ether can reach above 65%. The environmentally-friendly acidic catalyst is adopted to catalyze the direct etherification of isosorbide and ethanol, so the introduction of highly toxic halogenated hydrocarbons and the generation of a large amount of halide salt byproducts are avoided, the corrosion problem caused by strong acids and strong alkalis is avoided. The isosorbide monoethyl ether and isosorbide diethyl ether synthesis method provided by the invention has the advantages of high efficiency and environmental protection.

Description

technical field [0001] The invention relates to a method for preparing isosorbide ethyl ether, in particular to preparing 2-ethoxyisosorbide (2-MEI) and 5-ethoxyisosorbide through the direct etherification of isosorbide and ethanol catalyzed by an acidic catalyst (5-MEI) and diethyl ether isosorbide (DEI). Background technique [0002] Fossil resources provide the necessary energy and chemical guarantees for the survival and development of human society. With the depletion of fossil resources and the increasingly prominent hazards of greenhouse gases, the research on seeking renewable resources to replace fossil resources to obtain fuels and chemicals has attracted more and more attention. As a renewable organic carbon resource, biomass can be converted into fuels and chemicals, providing a sustainable route for social development. [0003] Isosorbide is an important biomass-based compound, which can be obtained from sorbitol, the hydrogenation product of glucose, through ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 徐杰车鹏华路芳聂鑫黄义争高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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