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Preparation method of pure M1-phase MoVTeNbOx catalyst with high specific surface area

A technology of high specific surface area and catalyst, applied in the field of catalysis, can solve the problems of restricting catalytic activity, small specific surface area of ​​catalyst, and a certain distance in the production capacity of catalyst with space-time yield, and achieve low price, excellent catalytic activity and high space-time yield Effect

Active Publication Date: 2018-11-23
安徽环轩材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among molybdenum vanadium tellurium niobium multi-element composite metal oxides, the pure M1 phase catalyst is a catalyst system with great application prospects at present, and it can achieve high ethane conversion rate and ethylene selectivity at a relatively low temperature, but the current patent Compared with the MoVTeNbOx pure M1 phase catalyst reported in the literature, there is still a certain distance between the space-time yield and the production capacity of the catalyst and the requirements of industrialization.
In addition, currently pure M1 phase catalysts are generally prepared by hydrothermal method or precipitation method with a suitable purification process. The specific surface area of ​​the prepared catalyst is usually small, which restricts its catalytic activity.

Method used

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  • Preparation method of pure M1-phase MoVTeNbOx catalyst with high specific surface area
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  • Preparation method of pure M1-phase MoVTeNbOx catalyst with high specific surface area

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preparation example Construction

[0036] The invention provides a method for preparing a pure M1 phase MoVTeNbOx catalyst with a high specific surface area, comprising the following steps:

[0037] S1) Mix and dissolve the molybdenum-containing compound, the vanadium-containing compound, the tellurium-containing compound, the niobium-containing compound and the protective agent to obtain a precursor-protective agent mixed solution;

[0038] The protective agent is a surfactant or a small molecule organic acid and a salt thereof;

[0039] S2) performing a hydrothermal reaction on the precursor-protecting agent mixed solution, and separating to obtain a solid;

[0040] S3) Calcining the solid in an air atmosphere, then calcining in an inert gas, and then purifying hydrogen oxide to obtain a pure M1 phase MoVTeNbOx catalyst.

[0041] The invention uses molybdenum-containing compounds, vanadium-containing compounds, tellurium-containing compounds and niobium-containing compounds as raw materials to prepare pure M...

Embodiment 1

[0087] According to the molar ratio of Mo, V, Te, Nb and protective agent (sodium citrate) is 1:0.25:0.23:0.12:0.14, under the heating condition of 80 ℃, weigh a certain amount of ammonium niobium oxalate in proportion and dissolve in In deionized water, solution 1 was obtained, and a certain quality of ammonium molybdate, vanadyl sulfate, and telluric acid was also weighed, and dissolved in deionized water to obtain solution 2. The volume ratio of solution 1 and solution 2 was 1:2.5, and solution 1 After cooling with solution 2, mix and stir evenly to obtain the precursor solution, then add 0.05mol / L sodium citrate solution, the volume ratio of the protective agent solution to the precursor solution is 1:6.5, continue to mix and stir evenly; The solution was transferred to a hydrothermal kettle, and heated at 175°C for 48 hours to obtain a purple suspension; the suspension obtained by hydrothermal synthesis was centrifuged and washed, dried overnight at 80°C in a blast drying ...

Embodiment 2

[0094] According to the molar ratio of Mo, V, Te, Nb and protective agent (ammonium citrate) is 1:0.25:0.23:0.12:0.14, under the heating condition of 80 ℃, weigh a certain amount of ammonium niobium oxalate in proportion and dissolve in In deionized water, solution 1 was obtained, and a certain quality of ammonium molybdate, vanadyl sulfate, and telluric acid was also weighed, and dissolved in deionized water to obtain solution 2. The volume ratio of solution 1 and solution 2 was 1:2.5, and solution 1 After cooling with solution 2, mix and stir evenly to obtain a precursor solution. Add 0.05mol / L ammonium citrate protective agent solution to the precursor solution, the volume ratio of the protective agent solution to the precursor solution is 1:8.5, mix and stir evenly, transfer to a hydrothermal kettle, and heat at 175°C for 48h After that, a lavender suspension was obtained; after the suspension was centrifugally washed, it was dried overnight at 80°C in a blast drying oven,...

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Abstract

The invention provides a preparation method of a pure M1-phase MoVTeNbOx catalyst with high specific surface area. The preparation method comprises the following steps: S1), mixing and dissolving a molybdenum-containing compound, a vanadium-containing compound, a tellurium-containing compound, a niobium-containing compound and a protective agent to obtain a precursor-protective agent mixed solution, wherein the protective agent is a surfactant or low-molecular organic salt and salt thereof; S2), performing hydrothermal reaction on the precursor-protective agent mixed solution and performing separation to obtain a solid; S3), roasting the solid in an air atmosphere, then roasting the solid in inert gas, and then performing hydrogen oxide purification treatment to obtain the pure M1-phase MoVTeNbOx catalyst. The pure M1-phase MoVTeNbOx catalyst synthesized by adopting the method has the rich porous volume and the high specific surface area, and shows the excellent conversion ratio, selectivity, space time yield and stability in oxidative dehydrogenation reaction of ethane to ethylene.

Description

technical field [0001] The invention relates to the field of catalysis, in particular to a method for preparing a pure M1 phase MoVTeNbOx catalyst with a high specific surface area. Background technique [0002] Ethylene (C 2 h 4 ) is one of the largest chemical products in the world, and is an important basic chemical raw material, mainly used in synthetic fibers, rubber, plastics, acrylic fibers, adhesives and other chemicals. At present, ethylene products account for more than 40% of organic chemicals, and about 75% of petrochemical products are produced from ethylene, which occupies an important position in the national economy. The world has taken ethylene production scale, technology and output as one of the important symbols to measure the development level of a country's petrochemical industry. [0003] Currently, ethylene is produced mainly through steam cracking and catalytic cracking of naphtha and ethane. This type of cracking process is a strong endothermic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/887B01J35/10
CPCB01J23/002B01J23/8877B01J2523/00B01J35/61B01J2523/55B01J2523/56B01J2523/64B01J2523/68
Inventor 黄伟新章轩语卫泽跃尤瑞
Owner 安徽环轩材料科技有限公司