Synthesis method of glycol dialkyl ether

A technology of ethylene glycol dialkyl ether and synthesis method, which is applied in the direction of preparation of ether from alkylene oxide, ether preparation, organic chemistry, etc. It can solve the problems of difficult separation of liquid acid catalyst and product, environmental pollution, and many by-products , to achieve the effect of green and environmental protection production method, less corrosion of equipment and convenient treatment

Inactive Publication Date: 2012-05-02
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of the direct method is that the preparation method is simple, economical and cheap; the disadvantage is that there are many by-products, the reaction system is homogeneous, it is difficult to separate the liquid acid catalyst from the product, the equipment is severely corroded, and it needs to be neutralized to remove it, which pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] Initially charge 1.8 g H in a nitrogen-purged 0.5 L steel autoclave 3 PO 4 / AC and 138.0 g (3.0 mol) dimethyl ether. At 50 °C and 1.0 MPa, add 44.0 g (1 mol) of ethylene oxide. Stir at 50°C for 2 h to complete the reaction, discharge excess dimethyl ether, and suction filter the still liquid to obtain 13.5 g of the reaction product. According to gas chromatography analysis, the product composition is shown in Table 1:

[0032] Element DMEG Diox MMG DMDG MMDG DMTG DMTeG unknown content / % 31.2 10.8 3.4 27.3 2.5 10.2 3.1 11.5

[0033] Table 1

example 2

[0035] Initially charge 1.8 g HBF in a nitrogen-purged 0.5 L steel autoclave 4 / AC and 138.0 g (3.0 mol) dimethyl ether. At 50 °C and 1.0 MPa, add 44.0 g (1 mol) of ethylene oxide. Stir at 50°C for 2 h to complete the reaction, discharge excess dimethyl ether, and suction filter the still liquid to obtain 66.8 g of reaction product. According to gas chromatography analysis, the product composition is shown in Table 2:

[0036] Element DMEG Diox MMG DMDG MMDG DMTG DMTeG unknown content / % 44.3 6.9 5.2 22.3 1.6 9.8 4.3 5.6

[0037] Table 2

example 3

[0039] Initially charge 1.8 g of BF in a nitrogen-purged 0.5 L steel autoclave 3 / AC and 138.0 g (3.0 mol) dimethyl ether. At 50 °C and 1.0 MPa, add 44.0 g (1 mol) of ethylene oxide. Stir at 50°C for 2 h to complete the reaction, discharge excess dimethyl ether, and suction filter the still liquid to obtain 64.6 g of the reaction product. According to gas chromatography analysis, the product composition is shown in Table 3:

[0040] Element DMEG Diox MMG DMDG MMDG DMTG DMTeG unknown content / % 47.9 7.8 4.0 20.5 1.3 8.5 3.6 6.4

[0041] table 3

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PUM

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Abstract

The invention relates to a synthesis method of glycol dialkyl ether. The synthesis method is characterized by comprising the following step: reacting ethylene oxide with dialkyl ether which are utilized as raw materials in the presence of active carbon supported acid as a catalyst so as to obtain the glycol dialkyl ether, wherein the reaction temperature is 30-100 DEG C, the reaction pressure is less than 5.0MPa, the reaction time is 0.5-5 hours, the mol ratio of dialkyl ether to ethylene oxide is (1:1)-(10:1), the use amount of the active carbon supported acid catalyst is 0.2-5% of the total mass of reactants, the supported acid amount of the active carbon supported acid catalyst is 5-60mt%, and the active carbon supported acid catalyst is single-component supported acid catalyst or composite supported acid catalyst. The synthesis method has the advantages that the yield and the selectivity of glycol dialkyl ether are high; the catalyst can be easily separated from products; and the corrosivity on equipment is small, and the production process is clean.

Description

technical field [0001] The invention relates to a method for synthesizing ethylene glycol dialkyl ethers, in particular to a method for preparing ethylene glycol dialkyl ethers by reacting ethylene oxide and dialkyl ethers with activated carbon immobilized by acid. It belongs to the field of organic chemical technology. Background technique [0002] Ethylene glycol dialkyl ether (ROCH 2 CH 2 OR, R=C 1 ~C 4 Alkyl) is an aprotic polar solvent with excellent performance, which has stable chemical properties and solubility, and is mainly used in advanced solvents and chemical industries such as polymer chemistry, electrochemistry, boron chemistry, and fine organic synthesis. In recent years, the continuous development and progress of my country's ethylene glycol dialkyl ether production technology has promoted the continuous expansion of the application of ethylene glycol dialkyl ether, especially in medicine, pesticides, dye intermediates, electronic chemicals, paints and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/02C07C43/11C07C43/10C07C43/13C07D319/12
Inventor 朱新宝顾建财于清跃王琪
Owner NANJING FORESTRY UNIV
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