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Oxo-vanadium phosphate catalyst, and preparation method and application thereof

A technology of vanadyl phosphate catalyst and solvent, which is used in the oxidation preparation of carbonyl compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc. Safety hazard, stable effect

Inactive Publication Date: 2014-02-05
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] It can be seen from the above that at present, almost all vanadyl phosphate materials are prepared by using water or alcohol as solvent, and the specific surface area of ​​catalysts synthesized by these methods is low (2 / g), the preparation process requires high equipment (closed, high pressure), etc.

Method used

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  • Oxo-vanadium phosphate catalyst, and preparation method and application thereof
  • Oxo-vanadium phosphate catalyst, and preparation method and application thereof
  • Oxo-vanadium phosphate catalyst, and preparation method and application thereof

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preparation example Construction

[0023] The preparation method of vanadyl phosphate catalyst, its step is:

[0024](1) Preparation of ionic liquids and eutectic mixtures, such as the synthesis of 1-alkyl-3-methylimidazolium bromides as [Emim]Br and [Bmim]Br from N-methylimidazole and the corresponding brominated The alkanes are reacted at 30°C-70°C for 3-10 hours, then washed several times with ethyl acetate, and dried in vacuum; the eutectic mixture is obtained by mixing and melting choline chloride and urea or other similar substances; chlorination The mixing molar ratio of choline and urea is 1:1~1:5;

[0025] (2) To prepare the vanadyl phosphate precursor, put the phosphorus source and the vanadium source into the ionic liquid and the eutectic mixture at a certain ratio, and the molar ratio of the ionic liquid solvent to the vanadium is 20-40; during the synthesis process, it is necessary to add A small amount of mineralizer, the synthesis temperature is 120-180°C, normal pressure, and the reaction time ...

Embodiment 1

[0030] Example 1: Add 40.51 g of choline chloride and 34.83 g of urea into a reaction vessel, melt at 80°C, continue to add 5.0 g of 85% phosphoric acid, 5.08 g of ammonium metavanadate, and 1.13 g of ammonium fluoride, and heat up to 120°C for reaction 12 h, washed with water and ethanol, and filtered to obtain a brown-black solid.

[0031] Post-treatment: drying at 110°C, and air calcination at 400°C for 4 h to obtain a vanadyl phosphate catalyst, which is denoted as VPO-Eut-1, such as figure 1 As shown, the material prepared by this method exhibits a rod-like morphology, most of which have a diameter of 20-50 nm. The specific surface area is shown in Table 1.

Embodiment 2

[0032] Example 2: 25.08 g of 85% phosphoric acid, 2.54 g of ammonium metavanadate, and 0.56 g of ammonium fluoride were added to the reaction vessel, and the temperature was raised to 180° C. for 144 h. Others were the same as in Example 1.

[0033] Post-treatment: drying at 110°C, followed by air calcination at 450°C for 6 h to obtain a vanadyl phosphate catalyst, which is designated as VPO-Eut-2. The specific surface area is shown in Table 1.

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Abstract

The invention relates to an oxo-vanadium phosphate catalyst, and a preparation method and application thereof. The catalyst is prepared through the following steps: preparing a precursor by performing ionothermal synthesis on vanadium pentoxide or metavanadate and phosphate or biphosphate used as raw materials in ionic liquid or eutectic mixture solvent at 120-180 DEG C under normal pressure; and then roasting. The synthesis method is operated under normal pressure, is safe and convenient, and has low requirements for equipment. The catalyst prepared through the method has a special spherical or claviform shape, has high specific surface area and can be used for cyclohexanol oxidation reaction.

Description

technical field [0001] The invention relates to a preparation method of a vanadyl phosphate catalyst and the application of the catalyst in redox reactions. Background technique [0002] Since the 1960s, people began to study vanadium-based phosphate catalysts extensively, because of their rich and complex structural chemical characteristics, and as a composite oxide material, they have been widely used in the selective oxidation of alkanes for many years, especially in It has important applications in selective oxidation of C2-C4 alkanes, dehydration, and low-temperature liquid phase reactions. The catalytic oxidation of butane to maleic anhydride (MA) by vanadyl phosphate catalyst is a classic example, and the industry has not yet found a better catalyst to replace it. [0003] So far, the preparation method of vanadium-based phosphate materials is to synthesize the precursor hydrogen phosphate hemihydrate (VOHPO 4 1 / 2H 2 O), and then calcined in the air containing abou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198C07C45/29C07C49/403
CPCY02P20/54
Inventor 赵鹬李贵贤张琪
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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