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Method for preparing butoxy methoxy methane

A technology of butoxymethoxymethane and dimethoxymethane, which is applied in the field of preparation of butoxymethoxymethane, achieves the effects of high product yield, simple process operation and mild reaction conditions

Inactive Publication Date: 2016-07-13
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Only the synthesis of methoxybutoxymethane, the raw material of the first step reaction, has not been reported on the specific synthesis method and route on SciFinder.

Method used

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  • Method for preparing butoxy methoxy methane
  • Method for preparing butoxy methoxy methane
  • Method for preparing butoxy methoxy methane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 38g of dimethoxymethane, 37g of n-butanol and 3g of catalyst to a 180mL high pressure reactor. 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 Seco Saisi), D072H (Tianjin Yunkai). Use N 2 Replace the air in the kettle three times under the condition of 1.0MPa to make the remaining air content in the kettle less than 0.1%, and then pass in 2.0MPaN again 2 , Let it stand for 30 minutes for leak detection in the reactor to ensure that the device does not leak, and then empty the gas in the reactor. Under the condition of ensuring no air leakage, the heating and raising reaction was carried out, 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.

[0035] Table 1. The influence of different resi...

Embodiment 2

[0039] Under normal pressure and 70℃, add the raw materials dimethoxymethane and n-butyl with molar ratios of 1:3, 1:2, 2:1, 3:1, 4:1, 5:1 into a 180mL autoclave Alcohol and 3g NKC-9 catalyst (wherein the mass of n-butanol is 37g), use N at room temperature 2 Replace the air in the kettle three times under the condition of 1.0MPa to make the remaining air content in the kettle less than 0.1%, and then pass in 2.0MPaN again 2 , Let it stand for 30 minutes for leak detection in the reactor to ensure that the device does not leak, and then empty the gas in the reactor. Under the condition of ensuring no air leakage, heating is performed under normal pressure, the stirring speed of the reactor is 500 rpm, and the reaction time is 4 hours. The effects of different raw material ratios on the reaction activity and product selectivity are shown in Table 2.

[0040] Table 2. The influence of different raw material ratios on reaction activity and product selectivity

[0041]

[0042] It can ...

Embodiment 3

[0044] Add 38g of dimethoxymethane, 37g of n-butanol, 3g of NKC-9 catalyst into a 180mL autoclave, and use N at room temperature 2 Replace the air in the kettle three times under the condition of 1.0MPa to make the remaining air content in the kettle less than 0.1%, and then pass in 2.0MPaN again 2 , Let it stand for 30 minutes for leak detection in the reactor to ensure that the device does not leak, and then empty the gas in the reactor. Under the condition of ensuring no air leakage, heat up, 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 temperature is 25, 40, 60, 80, 100, 120, 130, Table 3 shows the reaction results under different reaction temperature conditions at 140, 150 and 160°C.

[0045] Table 3. The effect of NKC-9 catalyst on the reaction activity and product selectivity under different reaction temperature conditions

[0046]

[0047] It can be seen from Table 3 that when NKC-9 is used as...

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Abstract

The invention provides a method for preparing butoxy methoxy methane and relates to a method for preparing methane. The method includes a synthesis path of ethylene glycol monobutyl ether, the path includes three steps that 1, methylal and butyl alcohol synthesize the butoxy methoxy methane; 2, directional carbonylation of the butoxy methoxy methane is conducted, and butoxy methyl acetate is generated; 3, hydrogenation is conducted on the butoxy methyl acetate to generate the ethylene glycol monobutyl ether and methane; dimethoxymethane and n-butyl alcohol serve as raw materials, under the temperature and pressure, resin serves as a catalyst, the butoxy methoxy methane is prepared. The brand new synthesis path of the ethylene glycol monobutyl ether and the preparation method of the butoxy methoxy methane are developed; the required raw materials are cheap and easy to obtain, the whole procedure is simple in operation, a product is singular and high in selectivity, good application prospect is achieved, and the butoxy methoxy methane is suitable for industrial production.

Description

Technical field [0001] The invention relates to a method for preparing methane, in particular to a method for preparing butoxymethoxymethane. Background technique [0002] Ethylene glycol butyl ether (HOCH 2 CH 2 OCH 2 CH 2 CH 2 CH 3 ), a colorless and flammable liquid with a moderately ethereal taste and a boiling point of 171°C. Because its molecules contain both ether bonds and hydroxyl groups, this unique property allows it to dissolve organic molecules, synthetic or natural macromolecule compounds, and to be miscible with water or water-soluble compounds to varying degrees, so it is widely used Used as paint, ink, cleaning agent, drug extraction agent, etc. According to statistics, in 2010, my country's paint and ink industries consumed about 200,000 tons of glycol ethers, accounting for about 80% of the total consumption of glycol ethers. The cleaning agent industry consumes about 20,000 tons of glycol ether, accounting for about 8% of the total consumption of glycol ethe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/50C07C43/30
CPCC07C41/26C07C41/50C07C67/37C07C43/30C07C69/708C07C43/13
Inventor 石磊姚杰赵佳李朕权
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY