Method for preparing diethoxymethane by supported heteropolyacid catalyst

A technology of diethoxymethane and dimethoxymethane, which is applied in the field of preparation of diethoxymethane with supported heteropolyacid catalysts, can solve the problems of excessive consumption, unfavorable large-scale production, and low output, and achieve cheap raw materials Easy to get, good application prospect, high selectivity effect

Inactive Publication Date: 2016-06-01
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The amount of dimethyl sulfoxide is large, the catalyst is unstable to acid and the yield is not high, which is not conducive to large-scale production
This method chloramphenicol by-product method is not conducive to large-scale production because of limited output

Method used

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  • Method for preparing diethoxymethane by supported heteropolyacid catalyst
  • Method for preparing diethoxymethane by supported heteropolyacid catalyst
  • Method for preparing diethoxymethane by supported heteropolyacid catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0042] In a 200mL autoclave, add 30g dimethoxymethane, 40g ethanol and 3g catalyst, the catalyst is 33%H 3 PW 12 o 40 / SiO 2 , 33%H 4 SiW 12 o 40 / Activated carbon, 33%H 3 PMo 12 o 40 / SBA-15, 33%H 4 SiMo 12 o 40 / MCM-41, 33%H 3 PW 12 o 40 / TiO 2 and 33%H 3 PW 12 o 40 / Al 2 o 3 . The preparation method of load type heteropolyacid uses 33%H 3 PW 12 o 40 / SiO 2 As an example, the preparation process is as follows: use an aqueous solution of phosphotungstic acid with a concentration of 33 mass percent, and use SiO 2 As a carrier, the volume of the impregnating liquid is similar to the pore volume. Mix the two evenly and let it stand at room temperature for 10 hours to obtain a catalyst sample. Dry the sample at 120°C and roast at 350°C for 4 hours to obtain a mass fraction of 33%H 3 PW 12 o 40 / SiO 2 catalyst. Other catalyst preparation procedures are the same as the above process, the difference lies in one or more of the carrier, solvent (ethanol ca...

Embodiment 2

[0047] In a 200mL autoclave, the ratio of the amount of raw material dimethoxymethane and ethanol is 2:1, 1:1, 1:2, 1:3, 1:4 and 3g mass fraction is 33%H 3 PW 12 o 40 / SiO 2 Supported heteropolyacid catalyst, at room temperature with N 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. Under the condition of ensuring no air leakage, the temperature was raised under normal pressure, the stirring speed of the reactor was 500 rpm, the reaction temperature was 120°C, the reaction pressure was 3.0 MPa, and the reaction time was 6 hours. The results of controlling the ratio of raw materials are shown in Table 2.

[0048] Table 2. The effect of different raw material ratios on the reaction activity and product sel...

Embodiment 3

[0052] In 200mL autoclave, add 30g dimethoxymethane, 40g ethanol, 3g mass fraction is 33%H 3 PW 12 o 40 / SiO 2 Supported heteropolyacid catalyst, at room temperature with N 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. Under the condition of ensuring no air leakage, heat up under normal pressure, the stirring speed of the reactor is 500 rpm, the reaction time is 6 hours, the reaction pressure is 3.0MPa, and the reaction temperatures are 25°C, 40°C, 60°C, and 80°C respectively , 100°C, 120°C, 130°C, 140°C, 150°C, 160°C, the reaction results under different reaction temperature conditions are shown in Table 3.

[0053] Table 3.33%H 3 PW 12 o 40 / SiO 2 Effects of catalysts on the reactivity and produ...

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Abstract

The invention relates to a method for preparing diethoxymethane, in particular to a method for for preparing diethoxymethane by a supported heteropolyacid catalyst. According to the method, dimethoxymethane and ethanol are taken as raw materials, liquid acid and supported liquid acid are taken as catalysts, the preparation method of the supported heteropolyacid catalyst, for example 33% of H3PW12O40/SiO2, comprises the following steps that a phosphotungstic acid aqueous solution with the concentration of 33% by mass is used, SiO2 is taken as a carrier, the impregnation liquid volume is the approximate to the pore volume, a catalyst sample is obtained after the phosphotungstic acid aqueous solution and the SiO2 are mixed uniformly and stood at the normal temperature by 10h, the sample is dried at the temperature of 120 DEG C, and calcination is performed at the temperature of 350 DEG C to obtain the 33% of H3PW12O40/SiO2 catalyst by the mass is prepared. According to the method, the product is relatively simple, the selectivity is high, and the method has an excellent application prospect. The raw materials required by the method are easy to obtain, the whole process operation is simple, at the same time, the method doesn't produce any chemical substances polluting the environment, and the method belongs to the environment-friendly technology route.

Description

technical field [0001] The invention relates to a method for preparing diethoxymethane, in particular to a method for preparing diethoxymethane with a supported heteropolyacid catalyst. Background technique [0002] Diethoxymethane is an important chemical raw material, English name: dietoxymethan, abbreviated as DEM, structural formula: CH 3 CH 2 OCH 2 OCH 2 CH 3 . Diethoxymethane is a colorless, clear and volatile liquid with an odor similar to ether, with a melting point of -66.5°C and a boiling point of 89°C. It is soluble in benzene, ether, and ethanol, and slightly soluble in water. Diethoxymethane has the properties of low toxicity, high oxygen content, both hydrophilic and lipophilic properties, strong solubility, small surface tension and low heat of vaporization. Its application is mainly divided into two categories: one is used as a solvent, and the other is used as a reaction reagent. As a solvent, diethoxymethane is an aprotic solvent and can be used in s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/30C07C41/48B01J31/18B01J31/16B01J31/26B01J31/38
CPCB01J23/30B01J27/188B01J29/035B01J29/78B01J2229/20C07C41/48C07C43/30
Inventor 石磊赵佳姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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