Method of preparing glycol dimethyl ether through continuous etherification in fixed bed

A technology of ethylene glycol dimethyl ether and fixed bed, which is applied in the fields of ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, organic chemistry, etc., which can solve the problems of difficult post-processing, low diether selectivity, pollution, etc., and achieve reaction The process is green, the reaction process is simple, and the effect of reducing dependence on petroleum resources

Inactive Publication Date: 2016-05-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

[0003] At present, among the synthetic methods of glycol ether compounds, the Williamson synthetic method is the most commonly used, which is also the method adopted in industrial scale production, but this method is organic synthesis, which easily produces a large amount of sodium chloride or sodium sulfate. Pollution to a certain extent, difficult post-processing, and certain limitations to industrial production
Catalytic synthesis of ethylene glycol diether compounds is an important method, but most products are mainly ethylene glycol monoether, such as the ring-opening etherification of ethylene oxide, using niobium oxide as a catalyst, The conversion rate of diol is greater than 99%, and the selectivity of ethylene glycol monoether is greater than 82% (CN101190876B); the ethylene glycol monoether is prepared by using titanium silicon molecular sieves to catalyze the one-step reaction of ethylene, hydrogen peroxide and low-carbon alcohols, Selectivity greater than 75% (CN102452908A), low diether selectivity

Method used

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  • Method of preparing glycol dimethyl ether through continuous etherification in fixed bed
  • Method of preparing glycol dimethyl ether through continuous etherification in fixed bed
  • Method of preparing glycol dimethyl ether through continuous etherification in fixed bed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The test of embodiment 1 ethylene glycol and methanol etherification reaction performance

[0020] The catalyst is loaded into the fixed bed reactor, and the reactor is installed in the fixed bed. Prepare ethylene glycol and methanol raw materials with a molar ratio of 0.2, and then pump them into a preheating premixer with a preheating temperature of 250°C. Introduce 40ml / min of nitrogen, control the reaction pressure to maintain around 0.5MPa, then pump the raw materials into the reactor, control the reaction temperature to 230°C, and the liquid space velocity to 1.5h -1 , After 2 hours of reaction, samples were taken for analysis. The catalyst evaluation results are shown in Table 1.

[0021] Table 1 ethylene glycol and methanolylation reaction results

[0022]

[0023]

Embodiment 2

[0024] Embodiment 2 catalyst stability test

[0025] This example mainly investigates the catalyst stability in the etherification reaction of ethylene glycol and methanol. Choose L to be catalyst, experimental process is with embodiment 1, and the results are shown in Table 2.

[0026] Table 2 Catalyst stability test

[0027]

Embodiment 3

[0028] The influence of embodiment 3 reaction temperature on ethylene glycol etherification reaction

[0029] In this example, the influence of the reaction temperature on the result of the etherification reaction between ethylene glycol and methanol is studied, which is embodied in the conversion rate of ethylene glycol and the selectivity of ethylene glycol dimethyl ether. L catalyst was loaded into the fixed bed reactor. Prepare ethylene glycol and methanol raw materials with a molar ratio of 0.2, and then pump them into a preheating premixer with a preheating temperature of 250°C. Introduce 40ml / min of nitrogen, control the reaction pressure and maintain it at about 0.3MPa, then pump the raw materials into the reactor, and the liquid space velocity is 1.5h -1 , After 2 hours of reaction, samples were taken for analysis. The results are shown in Table 3.

[0030] The relation of table 3 reaction temperature and ethylene glycol etherification reaction result

[0031] ...

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Abstract

The invention discloses a method of preparing glycol dimethyl ether through continuous etherification in a fixed bed. In the method, with industrial ethylene glycol and industrial methanol as raw materials and with a solid acid catalyst, the glycol dimethyl ether is continuously prepared through the fixed bed, wherein the molar ratio of the ethylene glycol to the methanol is 0.02-10, the reaction temperature is 100-400 DEG C, the reaction pressure is 0.1-10 MPa and liquid space velocity is 0.3-2/h. The method reaches more than 90% in conversion of the ethylene glycol and more than 74% in selectivity on the glycol dimethyl ether. The method is simple in processes, is high in product selectivity and is suitable for further large-scale production.

Description

technical field [0001] The invention relates to a method for preparing ethylene glycol dimethyl ether, in particular to a method for preparing ethylene glycol dimethyl ether through fixed-bed continuous etherification. Background technique [0002] Ethylene glycol diether products are oxygen-containing compounds with high cetane number and energy density, miscibility with diesel oil, stable performance and good ignition performance, so they are potential oxygen-containing ether liquid fuels. As an important compound in ethylene glycol diether products, ethylene glycol dimethyl ether has excellent performance. Compared with ethanol, its boiling point is similar to that of ethanol, but its energy density is nearly twice that of ethanol (35MJ / L), equivalent to gasoline; meanwhile, ethylene glycol dimethyl ether has a higher cetane number, and its energy density is equivalent to that of diesel. Therefore, ethylene glycol dimethyl ether has broad application prospects as a dies...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/10C07C41/09
Inventor 路芳徐杰于维强陈帅陈佳志高进苗虹车鹏华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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