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Preparation method of double effect catalyst for high selective oxidation of methane to prepare dimethoxymethane

A dimethoxymethane, high-selectivity technology, applied in the preparation of organic compounds, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of catalyst reactivity and selectivity reduction, acid center easy loss of catalytic activity , selectivity reduction and other issues, to achieve the effect of stable activity, not easy to lose, and good dispersibility

Inactive Publication Date: 2016-05-04
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current method of introducing acid centers is to modify by post-treatment of liquid acid aqueous solution or salt solution containing acid radicals, but after modification, V 2 o 5 The dispersibility and redox properties of the catalyst change, which reduces the reactivity and selectivity of the catalyst, that is, the selectivity of dimethoxymethane decreases, and the acid center is easy to lose, thereby reducing the catalytic activity.

Method used

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  • Preparation method of double effect catalyst for high selective oxidation of methane to prepare dimethoxymethane
  • Preparation method of double effect catalyst for high selective oxidation of methane to prepare dimethoxymethane
  • Preparation method of double effect catalyst for high selective oxidation of methane to prepare dimethoxymethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 1g oxalic acid H 2 C 2 o 4 2H 2 O solid and 1 g potassium sulfate K 2 SO 4 , dissolved in 20g ethanol-distilled water solution, the mass concentration of ethanol in distilled water is 5%, after stirring to dissolve the solid, add 0.5g ammonium metavanadate NH 4 VO 3 , stirring to make NH 4 VO 3 Completely dissolved, the resulting solution was mixed with 10g of calcined TiO 2 The powders were mixed, stirred evenly at room temperature, and then allowed to stand for 1 hour, then transferred to a reactor with a polytetrafluoroethylene substrate and treated at 80°C for 12 hours. After the treatment, take out the reaction kettle, cool it in the air naturally, filter the precipitate in the reaction kettle, wash it with ethanol for 3 times, then wash it with water for 3 times, and then dry it in vacuum at 40°C for 18 hours to obtain a powder; put the dried powder at 400°C Under roasting for 8h, SO 4 2- Modified TiO 2 load V 2 o 5 solid catalyst.

Embodiment 2

[0028] Weigh 1g oxalic acid H 2 C 2 o 4 2H 2 O solid and 2.5 g sodium sulfate Na 2 SO 4 , dissolved in 10g ethanol-distilled water solution, the mass concentration of ethanol in distilled water is 25%, after stirring to dissolve the solid, add 1g ammonium metavanadate NH 4 VO 3 , stirring to make NH 4 VO 3 Completely dissolved, the resulting solution was mixed with 4g of calcined TiO 2 The powders were mixed, stirred evenly at room temperature, and then allowed to stand for 12 hours, then transferred to a reactor with a PTFE substrate and treated at 140°C for 4 hours. After the treatment, take out the reaction kettle, cool it naturally in the air, filter the precipitate in the reaction kettle, wash with ethanol for 3 times, then wash with water for 3 times, then vacuum dry at 80°C for 4 hours to obtain a powder; dry the obtained powder at 600°C Roasted for 3h to get SO 4 2- Modified TiO 2 load V 2 o 5 solid catalyst.

Embodiment 3

[0030] Weigh 0.3g oxalic acid H 2 C 2 o 4 2H 2 O solid and 2.5 g magnesium sulfate MgSO 4 , dissolved in 5g ethanol-distilled water solution, the mass concentration of ethanol in distilled water is 45%, after stirring to dissolve the solid, add 0.25g ammonium metavanadate NH 4 VO 3 , stirring to make NH 4 VO 3 Completely dissolved, the resulting solution was mixed with 5g of calcined TiO 2 The powders were mixed, stirred evenly at room temperature, and then allowed to stand for 6 hours, then transferred to a reactor with a polytetrafluoroethylene substrate and treated at 100°C for 7 hours. After the treatment, take out the reaction kettle, cool it naturally in the air, filter the precipitate in the reaction kettle, wash it with ethanol for 3 times, then wash it with water for 3 times, and then dry it in vacuum at 60°C for 10 hours to obtain a powder; put the dried powder at 500°C Roasted for 4.5h to obtain SO 4 2- Modified TiO 2 load V 2 o 5 solid catalyst.

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Abstract

The invention belongs to the field of solid catalyst for oxidation reactions for preparing dimethoxymethane, and especially relates to a preparation method of a double effect catalyst for high selective oxidation of methane to prepare dimethoxymethane. The preparation method comprises the following steps: (1) weighing oxalic acid and sulfate, adding distilled water containing ethanol, and stirring to dissolve the solid to obtain a solution A; (2) adding ammonium metavanadate into the solution A obtained in the step (1), and stirring to dissolve the solid ammonium metavanadate to obtain a solution B; (3) mixing burned TiO2 with the solution B obtained in the step (2), evenly stirring the solution at a room temperature, and allowing the system to stand still; (4) transferring the product obtained in the step (3) to a reactor, and heating the product; (5) after heating, taking out the product obtained in the step (4) from the reactor, cooling, filtering the white precipitate in the reactor, filtering, drying in vacuum, and burning the powder obtained in the drying step to obtain the target product. The catalyst has the advantages that the V2O5 is well dispersed, and the catalyst has an oxidation activity and acid center.

Description

technical field [0001] The invention belongs to the field of solid catalysts for the oxidation of dimethoxymethane, in particular to a method for preparing a double-effect catalyst for the highly selective oxidation of methanol to dimethoxymethane. Background technique [0002] Dimethoxymethane is a colorless, non-toxic, environmentally friendly chemical raw material. Due to its high oxygen content and cetane number, it has attracted much attention as a diesel additive with excellent performance in recent years. Traditionally, dimethoxymethane is synthesized by a two-step method. Methanol is first oxidized to formaldehyde, and then formaldehyde and methanol are condensed to form methylal. The first step of the process uses silver at 873-923K or iron-molybdenum catalyst at 573-703K, and the reaction temperature is relatively high; the second step uses acid catalysts such as acidic cation exchange resin, AlCl3, sulfuric acid, etc. This traditional process has problems such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C41/50C07C43/30
CPCB01J27/053C07C41/50C07C43/30
Inventor 钱建华董清华李君华刘琳邢锦娟
Owner BOHAI UNIV
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