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Method for performing liquid-phase partial oxidation on methane

A methane, liquid-phase technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of industrialization difficulties, environmental pollution, expensive platinum complex catalyst Pt, etc., to avoid toxicity problems, reduce cost effect

Inactive Publication Date: 2013-04-24
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, mercury salt catalysts are highly toxic and cause serious environmental pollution. Platinum complex catalysts Pt(bpym)Cl 2 The price is very expensive, and these defects make the industrialization of such methods very difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In 20ml of trifluoroacetic acid, add 3.47mg of phosphomolybdovanadate H 5 PMo 10 V 2 o 40 (0.1mM), 6.53mg potassium chloropalladate K 2 PdCl 4 (1 mM), 58.44 mg sodium chloride (50 mM). The above mixture was added into a stainless steel reaction kettle (50ml) with a polytetrafluoroethylene liner, and 1MPa methane was introduced, exhausted, and this operation was repeated 3 times. Start magnetic stirring, and introduce 1.5MPa of methane and 1.5MPa of oxygen. After reacting at a constant temperature of 80°C for 8 hours, cool the reactor with ice water, collect the liquid phase reaction liquid, and analyze it by gas chromatography. The concentration of acetic acid is 112.86mM, the concentration of methyl trifluoroacetate is 2.38mM, and the conversion rate of methane is 23.04%. .

Embodiment 2

[0014] In 20ml of trifluoroacetic acid, add 3.47mg of phosphomolybdovanadate H 5 PMo 10 V 2 o 40 (0.1mM), 3.26mg potassium chloropalladate K 2 PdCl 4 (0.5mM), 2.92mg sodium chloride (2.5mM). The above mixture was added into a stainless steel reaction kettle lined with polytetrafluoroethylene, and 1 MPa methane was passed into it, exhausted, and this operation was repeated 3 times. Start magnetic stirring, and introduce 1.5MPa of methane and 1.5MPa of oxygen. After reacting at a constant temperature of 80°C for 8 hours, cool the reactor with ice water, collect the liquid phase reaction solution, and analyze it by gas chromatography. The concentration of acetic acid is 107.40mM, the concentration of methyl trifluoroacetate is 0.77mM, and the conversion rate of methane is 21.77%. .

Embodiment 3

[0016] 20ml potassium chloropalladate K 2 PdCl 4 Concentration is 0.05mM, phosphomolybdovanadate H 5 PMo 10 V 2 o 40 The reaction solution with a concentration of 0.05mM and a sodium chloride concentration of 2.5mM was put into a stainless steel reaction kettle with a polytetrafluoroethylene liner, and 1MPa methane was introduced into it, and the gas was exhausted. This operation was repeated 3 times. Start magnetic stirring, and introduce 3.0MPa of methane and 0.5MPa of oxygen. After reacting at a constant temperature of 80°C for 8 hours, cool the reactor with ice water, collect the liquid phase reaction liquid, and analyze it by gas chromatography. The concentration of acetic acid is 76.18mM, the concentration of methyl trifluoroacetate is 3.38mM, and the methane conversion rate is 7.87%. .

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PUM

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Abstract

The invention provides a method for performing liquid-phase partial oxidation on methane, and belongs to the field of methane conversion. The method is characterized in that: potassium tetrachloropalladate and molybdovanadophosphoric heteropolyacid are used as catalysts and oxygen is used as an oxidant in a trifluoroacetic acid solvent; and the methane is oxidized to form acetic acid and methyl trifluoroacetate. In the method, the molar ratio of the potassium tetrachloropalladate to the molybdovanadophosphoric heteropolyacid serving as the catalysts is 500:1-0.01:1; the concentration of the potassium tetrachloropalladate and the molybdovanadophosphoric heteropolyacid is respectively 0.01 to 5mm and 0.01 to 1mm; the total pressure of the methane and oxygen is 2.5 to 5.0MPa; the partial pressure ratio of the methane to the oxygen is (0.5-10):1; and reaction is performed for 1 to 15 hours at the temperature of between 40 and 120 DGE C to form the acetic acid and methyl trifluoroacetate. The conversion rate of the methane can reach 23.04 percent; and the method is favorable for solving the problems of high price and toxicity of the catalyst and the like in the liquid-phase oxidation reaction of the methane.

Description

technical field [0001] The invention relates to a method for liquid-phase partial oxidation of methane, which belongs to the technical field of methane conversion. Background technique [0002] Methane is the main component of natural gas with abundant reserves, and it is a low-value-added carbon-based raw material. Converting natural gas into liquid products such as acids, aldehydes, and alcohols can not only accelerate the development and utilization of natural gas resources, but also serve as an important supplement to basic chemical products. Methane resource utilization usually converts gaseous methane into synthesis gas (CO+H 2 ), and then through Fischer-Tropsch (Fischer-Tropsch) synthesis to produce other advanced products such as acid, aldehyde, alcohol and other liquid products. However, the process of converting methane into synthesis gas needs to be carried out at high temperature (about 850°C), which consumes a lot of energy. [0003] The liquid-phase catalyt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/08C07C51/215C07C69/63C07C67/00B01J27/199B01J27/13
Inventor 元炯亮刘路
Owner BEIJING UNIV OF CHEM TECH