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Method for preparing methanol by directly oxidizing methane in ionic liquid under action of microwaves

A technology of ionic liquid and methanol, applied in the direction of oxidation reaction preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve problems such as high temperature and long reaction time, and achieve shortened production process, The effect of low process energy consumption and operating costs

Inactive Publication Date: 2014-04-16
DALIAN TIANBAO CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid-phase catalytic oxidation of methane to directly synthesize methanol is a direction that has just started in the past 20 to 30 years. Most of the reactions use noble metals as catalysts. 3 Aqueous solution of COOH and H 2 SO 4 The reaction is carried out in the solution, the reaction time is longer and the temperature is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In the three-neck flask, add the ionic liquid [C 4 mim] Cl, K 2 S 2 o 8 , TFA, TFAA, Au / SiO 2 (mass ratio is 10: 77: 22.3: 13.3: 0.1), be placed in microwave reactor, microwave reactor power 300W, methane gas is passed in the liquid with the speed of 10ml / min, at 80 ℃, react 30min . After stopping the reaction, 20ml of deionized water was added to the reaction solution, and hydrolyzed at 25°C for 30min. The hydrolyzate was distilled to obtain the distillate at 90°C as the product methanol. The methane conversion rate was 5.1%, and the methanol yield was 4.8%.

Embodiment 2

[0019] In the three-neck flask, add the ionic liquid [C 1 mim] Cl, K 2 S 2 o 8 , TFA, TFAA, Au / SiO 2 (mass ratio is 10: 77: 22.3: 13.3: 0.1), be placed in microwave reactor, microwave reactor power 100W, methane gas is passed in the liquid with the speed of 20ml / min, at 80 ℃, react 30min . After stopping the reaction, 20ml of deionized water was added to the reaction solution, and hydrolyzed at 25°C for 30min. The hydrolyzate was distilled to obtain the distillate at 90°C as the product methanol. The methane conversion rate was 4.7%, and the methanol yield was 4.6%.

Embodiment 3

[0021] In the three-neck flask, add the ionic liquid [C 1 mim] Cl, K 2 S 2 o 8 , TFA, TFAA, Au / SiO 2 (mass ratio is 10: 77: 22.3: 13.3: 0.1), be placed in microwave reactor, microwave reactor power 300W, methane gas is passed in the liquid with the speed of 20ml / min, at 80 ℃, react 30min . After stopping the reaction, 20ml of deionized water was added to the reaction solution, and hydrolyzed at 25°C for 30min. The hydrolyzate was distilled to obtain the distillate at 90°C as the product methanol. The methane conversion rate was 4.8%, and the methanol yield was 4.6%.

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Abstract

The invention discloses a method for preparing methanol by directly oxidizing methane in ionic liquid under the action of microwaves, which comprises the following steps: placing a three-neck flask filled with ionic liquid, trifluoroacetic acid, trifluoroaceticanhydride, potassium persulfate and catalyst in a microwave reactor, introducing methane into the liquid at a certain speed with stirring by a magnetic force, heating at 80 to 110 DEG C for 30 to 120 minutes by microwaves to obtain methyl trifluoroacetate, and hydrolyzing the methyl trifluoroacetate to obtain methanol. In the invention, the ionic liquid is used as a solvent and microwave heating is combined, so the reaction time is reduced and the reaction yield and conversion rate are improved. The ionic liquid used as the solvent can be reclaimed, the operation is convenient and the cost is low.

Description

technical field [0001] The present invention relates to the direct oxidation of methane and belongs to the field of organic chemistry. In particular, it relates to the methanol preparation process of the direct oxidation of methane in an ionic liquid solvent system under the action of microwaves. Background technique [0002] Methane is an important chemical raw material, and as the main component of natural gas, it is an abundant natural resource. However, methane is often difficult to utilize because it is expensive to transport methane gas or liquefied natural gas. Direct conversion of methane into transportable liquid fuels and useful chemicals is highly desirable. [0003] The conversion of methane is mainly divided into two categories: indirect conversion and direct conversion. At present, most of the processes for converting methane into methanol are indirect conversion methods, that is, steam cracking is used to produce synthesis gas with a certain carbon-to-hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/04C07C29/48B01J23/52
CPCY02P20/52Y02P20/54
Inventor 宋云保马英冲付泉于长顺王少君
Owner DALIAN TIANBAO CHEM IND