Method for preparing V-Ti-Si-O composite catalyst used in methanol oxidation for synthesizing methylal

A composite catalyst, v-ti-si-o technology, applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve problems such as complex processes, and achieve The effect of simple preparation process, good performance, improved thermal stability and molding ability

Inactive Publication Date: 2010-06-09
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process of the catalyst, the vanadium species and sulfate radicals are loaded on the surface of titanium dioxide by impregnation method, and the process is relatively complicated.

Method used

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  • Method for preparing V-Ti-Si-O composite catalyst used in methanol oxidation for synthesizing methylal
  • Method for preparing V-Ti-Si-O composite catalyst used in methanol oxidation for synthesizing methylal
  • Method for preparing V-Ti-Si-O composite catalyst used in methanol oxidation for synthesizing methylal

Examples

Experimental program
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Effect test

Embodiment 1

[0013] 13.52g of titanium sulfate and 0.90g of vanadyl sulfate were ultrasonically dissolved in 450mL of water to obtain a blue solution A, and 35mL of ammonia water (25%) was added to 700mL of water to form an ammonia solution, and the vanadium-titanium solution A was dissolved in 3 mLmin -1 Add it dropwise into the ammonia solution at a high speed. After the addition is complete, continue to stir for 1 hour, age at room temperature for 8 hours, filter, and roast the obtained filter cake in air at 350°C for 3 hours to obtain a solid sample. The vanadium content was determined to be 9.8% (by mass percentage of vanadium pentoxide), the titanium content was 86.4% (by mass percentage of titanium dioxide), and the sulfur was 3.8% (by mass percentage of sulfate). The prepared V 2 o 5 The composite catalyst is crushed and sieved, and the 20-40 mesh sample is taken in a U-shaped tube reactor with an external diameter of 8mm, and the ratio of the amount of the substance is methanol 5...

Embodiment 2

[0022] 9.62g of titanium sulfate and 1.40g of vanadyl sulfate were ultrasonically dissolved in 350mL of water to obtain a blue solution A. Take 30mL of ammonia water (25%) and add 180mL of water to form an ammonia solution. -1 Add it dropwise into the ammonia solution at a high speed. After the dropwise addition is complete, continue to stir for 3 hours, age at room temperature for 10 hours, filter, and roast the obtained filter cake in air at 400°C for 6 hours to obtain a solid sample. The vanadium content was determined to be 18.9% (by mass percentage of vanadium pentoxide), the titanium content was 79.5% (by mass percentage of titanium dioxide), and the sulfur was 1.6% (by mass percentage of sulfate radical). The prepared V 2 o 5 The composite catalyst is crushed and sieved, and the 20-40 mesh sample is taken in a U-shaped tube reactor with an external diameter of 8mm, and the ratio of the amount of the substance is methanol 5%, O 2 15%, N 2 80% of the mixed gas was pr...

Embodiment 3

[0024] 7.21g of titanium sulfate and 2.87g of vanadyl sulfate were ultrasonically dissolved in 370mL of water to obtain a blue solution A. Take 30mL of ammonia water (25%) and add 180mL of water to make an ammonia solution. The vanadium-titanium solution A was dissolved in 4 mL min -1 Add it dropwise into the ammonia solution at a high speed. After the dropwise addition is complete, continue to stir for 5 hours, age at room temperature for 10 hours, filter, and roast the obtained filter cake in air at 400°C for 6 hours to obtain a solid sample. The vanadium content was determined to be 38.9% (by mass percentage of vanadium pentoxide), the titanium content was 59.8% (by mass percentage of titanium dioxide), and the sulfur was 1.3% (by mass percentage of sulfate). The prepared V 2 o 5 The composite catalyst is crushed and sieved, and the 20-40 mesh sample is taken in a U-shaped tube reactor with an external diameter of 8mm, and the ratio of the amount of the substance is methan...

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Abstract

The invention provides a method for preparing a V-Ti-Si-O composite catalyst used in methanol oxidation for synthesizing methylal. The method comprises: taking vanadyl sulfate (VOSO4), titanium sulfate (Ti(SO4)2) and tetraethoxysilane (Si(OC2H5)4) as precursors; adding water for dissolution to form mixed solution; and taking aqueous solution of ammonia as precipitant and using a coprecipitation method to directly prepare the V-Ti-Si-O composite catalyst containing sulfate radicals. The introduction of SiO2 improves the thermal stability and molding capability of the catalyst, and as the catalyst contains the sulfate radicals which do not need to be introduced through second impregnation, the method is simple in preparation process. The catalyst is used in the selective oxidation of methanol for synthesizing methylal and has good performance.

Description

1. Technical field [0001] The invention relates to a preparation method of a V-Ti-Si-O composite catalyst, which is used for synthesizing methylal by reacting methanol with oxygen. 2. Background technology [0002] Vanadium-titanium-based catalysts, that is, titania-supported vanadium oxide catalysts, are an important class of catalysts. In many oxidation-reduction reactions, such as the oxidation of methanol to formaldehyde or methyl formate, the oxidation of o-xylene to o-xylene anhydride, and the catalytic NO x Revert to N 2 (SCR reaction), selective oxidation of hydrocarbons, ammonia oxidation, and oxidative dehydrogenation of alkanes, etc., vanadium-titanium-based catalysts show good catalytic performance. Therefore, vanadium-titanium-based catalysts have been attracting the attention of academia and industry. with silicon dioxide (SiO 2 ) or aluminum oxide (A1 2 o 3 ) and other supports, titanium dioxide (TiO 2 ) carrier has good dispersibility to vanadium oxide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/22B01J21/06C07C43/30C07C41/50
Inventor 沈俭一刘经伟傅玉川孙清
Owner NANJING UNIV
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