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A kind of preparation method of ethoxymethoxymethane

A technology of ethoxymethoxymethane and dimethoxymethane, which is applied in the field of preparation of ethoxymethoxymethane, can solve the problems of low EMM yield, achieve high selectivity, simple products, and no pollution Effect

Inactive Publication Date: 2018-06-19
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Rakhmankulov, I. L. et al. reported (Nekotor. Vopr. Issled. Razl. Khim. SistemFiz.-Khim. Metodami, Ashkhabad Pages55-7 Journal 1980) using methylal and diethoxymethane as reaction raw materials and methyl acetate as solvent , to synthesize ethoxymethoxymethane, but the EMM yield of this method is low, only 10%

Method used

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  • A kind of preparation method of ethoxymethoxymethane
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  • A kind of preparation method of ethoxymethoxymethane

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Experimental program
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Effect test

Embodiment 1

[0024] Add 38 g of dimethoxymethane, 23 g of ethanol and 3 g of catalysts into a 180 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 airtightness, the reaction was heated and heated. The stirring speed of the reactor was 500 rpm, the reaction pressure was 0.1 MPa, the reaction temperature was 70°C, and the reaction time was 4 hours. The reaction results are shown in Table 1.

[0025]

[0026] From the reaction data in Table 1, it ca...

Embodiment 2

[0028] Under the condition of normal pressure and 70 ℃, add the raw materials dimethoxymethane and Ethanol and 3 g of NKC-9 catalyst (the quality of ethanol is 23 g), at room temperature with 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, heating was carried out under normal pressure, the stirring speed of the reactor was 500 rpm, and the reaction time was 4 hours. The influence of different raw material ratios on the reaction activity and product selectivity is shown in Table 2.

[0029]

[0030] It can be seen from Table 2 that at normal pressure and 70°C, after 4 hours of reaction, different molar ratios of the reaction raw materials dimethoxymethan...

Embodiment 3

[0032] Add 38 g of dimethoxymethane, 23 g of ethanol, and 3 g of NKC-9 catalyst in a 180 mL autoclave, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, 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 the temperature, the stirring speed of the reactor is 500 rpm, the reaction time is 4 hours, the reaction pressure is 0.1 MPa, and the reaction temperatures are 25 ℃, 40 ℃, 60 ℃, 80 ℃, 100 ℃ respectively , 120 °C, 130 °C, 140 °C, 150 °C, 160 °C, the reaction results under different reaction temperature conditions are shown in Table 3.

[0033]

[0034] It can be seen from Table 3 that when NKC-9 is used as a catalyst, the reaction is carried out under normal pressure for 4 hours, and when t...

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Abstract

A method for preparing ethoxymethoxymethane, relates to a method for preparing methane, the method uses dimethoxymethane and ethanol as raw materials, and uses resin as a catalyst under temperature and pressure to prepare ethoxymethane Resin catalyst is one or more resin catalysts of KAD302, KC107, NKC-9, DA-330, D009B, Amberlyst-15, D072H; Resin catalyst is based on the resin catalyst containing sulfonic acid group; 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 nitrogen or a mixture thereof; the reactor is a fixed bed or tank type Reactor; the molar ratio of raw materials dimethoxymethane and ethanol is 1:2 to 5:1. The synthesis process of the invention has simple products, fewer side reactions, and high selectivity of the required product ethoxymethoxymethane; meanwhile, the method of the invention basically does not pollute the environment.

Description

technical field [0001] The invention relates to a method for preparing methane, in particular to a method for preparing ethoxymethoxymethane. Background technique [0002] Ethoxymethoxymethane (EMM), with a molecular weight of 90.12 and a boiling point of 65.90 °C, is an important methanol derivative that contains both methoxy and ethoxy groups, and can be used as a co-solvent for methanol gasoline. [0003] We consulted SciFinder, using ethoxymethoxymethane as the product, and found that there are few reports on the synthesis method of ethoxymethoxymethane in the literature and patents. [0004] (1) Methanol, ethanol and formaldehyde aqueous solution method: [0005] A kind of method for preparing ethoxymethoxymethane by acetal reaction is reported in the patent CN102070416, and this method is raw material with ethanol, methyl alcohol and 30% methylal aqueous solution, and strongly acidic cation exchange resin Amberlyst 35 is catalyst, in intermittent Under the formula re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C41/48
CPCC07C41/48C07C43/30
Inventor 石磊姚杰赵佳
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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