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Method for preparing diethylene glycol dimethyl ether through ethylene glycol monomethyl ether

A technology of diethylene glycol dimethyl ether and ethylene glycol monomethyl ether, which is applied in the field of chemical raw material preparation, can solve the problems of small profit margin and high cost, and achieves a reaction with less by-products, less by-products and simple products. Effect

Inactive Publication Date: 2017-09-08
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the market price of raw material triethylene glycol monomethyl ether is about 14,000 per ton, and the market price of diethylene glycol dimethyl ether is about 20,000 per ton. The cost of synthesizing diethylene glycol dimethyl ether in this way is too high and the profit less space

Method used

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  • Method for preparing diethylene glycol dimethyl ether through ethylene glycol monomethyl ether
  • Method for preparing diethylene glycol dimethyl ether through ethylene glycol monomethyl ether
  • Method for preparing diethylene glycol dimethyl ether through ethylene glycol monomethyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 15.2 g of ethylene glycol monomethyl ether and 2 g of catalyst in a 180 mL autoclave, the catalyst carrier is silica, and the loads are 20% MgO, K 2 CO 3 、KNO 3 , KF. use N 2 Under the condition of 1.0 MPa, replace the air in the kettle three times, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Under the condition of ensuring airtightness, the reaction was heated and heated. The stirring speed of the reactor was 500 rpm, the reaction pressure was 0.1 MPa, the reaction temperature was 140 °C, and the reaction time was 6 h. The reaction results are shown in Table 1.

[0042] Table 1. Effects of solid base catalysts with different loads on the reactivity of ethylene glycol monomethyl ether and the selectivity of reactants

[0043]

[0044] From the reaction data o...

Embodiment 2

[0046] Add 15.2 g of ethylene glycol monomethyl ether and 2 g of catalyst in a 180 mL autoclave. The catalyst load is 20% KF, and the supports are silica, activated carbon, magnesium oxide, calcium oxide, zirconium dioxide, and titanium dioxide. . use N 2 Under the condition of 1.0 MPa, replace the air in the kettle three times, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Under the condition of ensuring airtightness, the reaction was heated and heated. The stirring speed of the reactor was 500 rpm, the reaction pressure was 0.1 MPa, the reaction temperature was 140 °C, and the reaction time was 6 h. The reaction results are shown in Table 2.

[0047] Table 2. Effect of solid base catalysts with different supports on reaction activity and product selectivity

[0048]

[00...

Embodiment 3

[0051] Add 15.2 g of ethylene glycol monomethyl ether, 2 g of KF / SiO loaded with 20 % KF into a 180 mL autoclave 2 catalyst, at room temperature with N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Under the condition of ensuring no air leakage, the heating was carried out under normal pressure, the stirring speed of the reactor was 500 rpm, the reaction time was 6 hours, the reaction pressure was 0.1 MPa, and the reaction temperatures were 100 °C, 120 °C, 140 °C, 150 °C, 160 ℃, 170 ℃, 180 ℃, 190 ℃, the reaction results under different reaction temperature conditions are shown in Table 3

[0052] Table 3. KF / SiO 2 Effect of Catalysts on Reaction Activity and Product Selectivity at Different Reaction Te...

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Abstract

The invention provides a method for preparing diethylene glycol dimethyl ether through ethylene glycol monomethyl ether and relates to a preparation method of a chemical raw material. The method comprises the following steps: taking the ethylene glycol monomethyl ether as a raw material, reacting for 6 hours by taking solid alkali KF / SiO2 as a catalyst under the conditions that the temperature is 170 DEG C and the pressure is 3.0 MPa, and preparing the diethylene glycol dimethyl ether at a high selectivity (92.05%). The ethylene glycol monomethyl ether as the reaction raw material is prepared by hydrogenating methyl methoxyacetate synthesized by methylal and carbon monoxide at a high selectivity; the methylal and the carbon monoxide as initial raw materials are cheap and easy to obtain; at prevent, a mature technology for preparing the methyl methoxyacetate is provided, therefore, a pathway to the synthesis of the diethylene glycol dimethyl ether has a certain experimental basis and industrial economic benefits. The method is used for synthesizing the diethylene glycol dimethyl ether, is simple in whole process operation, and has no special requirements for reaction equipment; side reactions are few, the target product selectivity is high, the added value of the diethylene glycol dimethyl ether is high, and the method is good in application prospect and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing chemical raw materials, in particular to a method for preparing diethylene glycol dimethyl ether from ethylene glycol monomethyl ether. Background technique [0002] Diethylene glycol dimethyl ether (CH 3 OCH 2 CH 2 OCH 2 CH 2 OCH 3 ), a colorless transparent liquid with a boiling point of 162 °C and a relative density of 0.9467, is a high boiling point aprotic polar solvent. It has a faint ether odor and is miscible with water, alcohols, dimethyl ether and hydrocarbon solvents. It is able to chelate small cationic groups, making it easier for anions to react with them. Therefore, the use of diethylene glycol dimethyl ether in reactions using metal-organic reagents such as Grignard reactions or reduction reactions using metal hydrides can significantly increase the reaction rate. Moreover, diethylene glycol dimethyl ether is stable in a high pH environment, and its high boiling point makes it very...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/09C07C43/11C07C41/26C07C43/13C07C67/37C07C69/708
CPCC07C41/09C07C41/26C07C67/37C07C69/708C07C43/13C07C43/11
Inventor 石磊胡亚威刘洋王玉鑫
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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