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The preparation method of nano wox/zro2 superacid

A super-acid and nanotechnology, which is applied in the direction of tungsten oxide/tungsten hydroxide, zirconia, etc., can solve the problems of large particle size, complicated process, and low tungsten loading of products

Active Publication Date: 2011-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is the complex process existing in the existing synthesis technology, the low tungsten loading of the product, and the large particle size of the product. It provides a new nano-scale WO x / ZrO 2 The preparation method of superacid

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  • The preparation method of nano wox/zro2 superacid
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  • The preparation method of nano wox/zro2 superacid

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Embodiment 1

[0018] Nano-WO with high tungsten loading x / ZrO 2 Preparation method of superacid. First, tungsten isopropoxide and zirconium isopropoxide are dispersed in toluene to obtain mixed liquid I, (the boiling point of toluene is higher than that of water, which helps water preferentially diffuse to the surface of the organic solution in the form of vapor, and the nanocrystals after hydrolysis are collected in the organic solvent , effectively avoiding nano-agglomeration caused by capillary condensation). The molar ratio of W:Zr in the mixed solution I is 0.1:1; the ratio of the total moles of tungsten and zirconium to the organic solvent is 0.1:1. Under the condition of 150°C, water vapor is brought into contact with the mixed liquid I, so that the tungsten isopropoxide and zirconium isopropoxide in the mixed liquid I are hydrolyzed at the same time, and the nano-WO x / ZrO 2 Precursors of superacids II. After drying in the air, the precursor II was calcined at 600°C for 12 hou...

Embodiment 2～8

[0020] According to the method of Example 1, just change the reaction temperature, the type of organic tungsten, zirconium and different molar ratios of tungsten and zirconium. x / ZrO 2 Nano-WO with different sizes and different tungsten loads can be obtained by further adjusting the particle size and W:Zr ratio of superacid x / ZrO 2 super acid. The specific results are shown in Table 1.

[0021] Table 1

[0022] Example

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Abstract

The invention relates to a preparation method of nanometer WOx / ZrO2 super acid, which mainly solves the problem of low tungsten loading capacity of WOx / ZrO2 super acid in the existing preparation method, resulting in low catalytic efficiency. The invention solves the problem of low loading by adopting the technical scheme of hydrolyzing organic tungsten and zirconium solutions with water vapor at a certain temperature, and can be used in the industrial production of nano WOx / ZrO2 super acid with high tungsten loading.

Description

technical field [0001] The present invention relates to a kind of nano WO x / ZrO 2 Preparation method of superacid. Background technique [0002] In 1988, Hino et al first reported WO x / ZrO 2 Compared with liquid acid catalysts, it has the advantages of no pollution, no corrosion, and easy separation from products; moreover, it has good thermal stability and will not lose components under high temperature and redox atmosphere. WO x / ZrO 2 As an acidic catalyst, it exhibits high catalytic activity and good selectivity in reactions such as alkane isomerization, hydrocarbon alkylation, esterification, and dehydration. [0003] Existing WO x / ZrO 2 There are usually three methods for preparing superacids: impregnation method, co-precipitation method, and sol-gel method. (1) The synthesis process of the impregnation method is to first use zirconium salt to adjust the pH value by adding ammonia water dropwise, and then precipitate to prepare Zr(OH) 4 Precursor, impregna...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02C01G25/02
Inventor 唐康健杨为民高焕新贾银娟
Owner CHINA PETROLEUM & CHEM CORP