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Method for synthesizing diethoxymethane from dimethoxymethane and ethanol

A technology of dimethoxymethane and diethoxymethane, which is applied in the field of methane preparation, can solve the problems of high consumption, low output, unfavorable large-scale production, etc., and achieves cheap and easy-to-obtain raw materials, simple process operation, and good application foreground effect

Active Publication Date: 2016-06-15
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 synthesizing diethoxymethane from dimethoxymethane and ethanol
  • Method for synthesizing diethoxymethane from dimethoxymethane and ethanol
  • Method for synthesizing diethoxymethane from dimethoxymethane and ethanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 30g of dimethoxymethane, 40g of ethanol and 3g of catalyst into a 200mL autoclave. The catalysts are KAD302 (Beijing Kairui Environmental Protection), KC107 (Tianjin Yunkai), NKC-9 (Tianjin Bohong), DA-330 (Jiangsu Tehua), D009B (Dandong Pearl), Amberlyst-15 (Jiangsu Sekesaisi), D072H (Tianjin Yunkai). use 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 airtightness, heating and heating reaction were carried out, the stirring speed of the reactor was 500 rpm, the reaction temperature was 120°C, the reaction pressure was 3.0MPa, and the reaction time was 6 hours. The results of controlling the catalyst type are shown in Table 1.

[0040] Table 1. Effects of diffe...

Embodiment 2

[0044] 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 3gAmberlyst-15 catalyst, at room temperature use 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.

[0045] Table 2. The effect of different raw material ratios on the reaction activity and product selectivity.

[0046]

[0047] As can be seen from Table 2...

Embodiment 3

[0049] In 200mL autoclave, add 30g dimethoxymethane, 40g ethanol, 3gAmberlyst-15 catalyst, under room temperature condition, use 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.

[0050] Table 3. Effect of Amberlyst-15 catalyst on the reactivity and product selectivity of dimethoxymethane and ethanol at different rea...

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Abstract

The invention provides a method for synthesizing diethoxymethane from dimethoxymethane and ethanol, relating to a method for preparing methane. The method comprises the following step: by using dimethoxymethane and ethanol as raw materials, reacting at 0-160 DEG C under the reaction pressure of 0.1-10.0 MPa by using a liquid acid and a supported liquid acid as catalysts to generate diethoxymethane at high selectivity. The resin catalyst is one or more of KAD302, KC107, NKC-9, DA-330, D009B, Amberlyst-15 and D072H containing sulfonic acid functional group. The reaction temperature is 0-160 DEG C, and the reaction pressure is 0.1-10.0 MPa. The filling gas is inert gas which is argon, helium, carbon dioxide or N2 mixture or a gas mixture thereof. The method has the advantages of single product and high selectivity, and has favorable application prospects. The required raw materials are cheap and accessible, and the whole process is simple to operate and can not generate any environment-polluting chemical substance. Thus, the method belongs to an environment-friendly technical route.

Description

technical field [0001] The invention relates to a method for preparing methane, in particular to a method for synthesizing diethoxymethane with dimethoxymethane and ethanol. 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 some water-se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/50C07C43/30
CPCC07C41/50C07C43/30
Inventor 石磊赵佳姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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