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A method for synthesizing diethoxymethane with 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 achieve simple process operation, cheap and easy-to-obtain raw materials, and good application foreground effect

Active Publication Date: 2018-06-19
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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  • A method for synthesizing diethoxymethane with dimethoxymethane and ethanol
  • A method for synthesizing diethoxymethane with dimethoxymethane and ethanol
  • A method for synthesizing diethoxymethane with dimethoxymethane and ethanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 30 g of dimethoxymethane, 40 g of ethanol and 3 g of catalysts into a 200 mL 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 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 no air leakage, the reaction was heated and heated. 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 catalyst types are shown in Table 1.

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

Embodiment 2

[0044] In the 200 mL autoclave, the ratio of the amount of substances that add raw material dimethoxymethane and ethanol is 2:1, 1:1, 1:2, 1:3, 1:4 and 3 g Amberlyst-15 catalyst, in N at room temperature 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 no air leakage, heating was carried out 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 ...

Embodiment 3

[0049] Add 30 g of dimethoxymethane, 40 g of ethanol, and 3 g of Amberlyst-15 catalyst in a 200 mL autoclave, and 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 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 3.0 MPa, and the reaction temperatures are 25 ℃, 40 ℃, 60 ℃, 80 ℃ respectively , 100 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 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 reaction temper...

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Abstract

A method for synthesizing diethoxymethane with dimethoxymethane and ethanol relates to a method for preparing methane, using dimethoxymethane and ethanol as raw materials, using liquid acid and loaded liquid acid as catalysts, and using dimethoxymethane and ethanol as catalysts. React under the conditions of reaction temperature 0-160°C and reaction pressure 0.1-10.0 MPa to form diethoxymethane with high selectivity; resin catalysts are KAD302, KC107, NKC‑9, DA‑330, D009B, Amberlyst containing sulfonic acid functional groups ‑15, D072H one or more resin catalysts; the reaction temperature is 0-160°C, the reaction pressure is 0.1-10.0 MPa; the filling gas is an inert gas, which is one of argon, helium, carbon dioxide, or N2 mixed gas species or mixture. The product of the invention is relatively single, has high selectivity, and has good application prospects. Moreover, the raw materials required by the method are cheap and easy to obtain, and the whole process is easy to operate. At the same time, the method does not produce any chemical substances that pollute the environment, and belongs to an environmentally friendly process path.

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 Patents(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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