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Preparation method of WO3/ZrO2 solid super acidic catalyst

A solid super acid and catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., to achieve enhanced catalytic activity, low reaction temperature, and small specific surface area. Effect

Inactive Publication Date: 2013-04-17
NORTHEAST GASOLINEEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, WO 3 / ZrO 2 The application of solid superacid catalysts in various acid-catalyzed reactions such as alkane isomerization, alkylation, esterification, acylation, and alcohol dehydration has been reported. Among them, alkane isomerization is used as a method to increase the octane number of gasoline in petroleum refining processes. The main way has received more and more attention. At present, C 5 / C 6 Isomerization of light isoparaffins is a mature process, but there are few reports on the isomerization of C7 and higher carbon number alkanes

Method used

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  • Preparation method of WO3/ZrO2 solid super acidic catalyst
  • Preparation method of WO3/ZrO2 solid super acidic catalyst
  • Preparation method of WO3/ZrO2 solid super acidic catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Example 1. Under the condition of stirring, add 0.6 m 3 min -1 25% volume fraction of concentrated ammonia water was added dropwise at a high speed to form a hydrogel, and the pH value was adjusted to 9~10. Stirring was continued for 1-2 hours, and after aging at room temperature for 1-12 hours, the prepared hydrogel was transferred to a round-bottomed flask connected with a condenser tube, and heated at 90-110°C for 1-12 hours. Suction filter and wash the precipitate with deionized water until there is no chloride ion. Then filter the cake in a constant temperature drying oven with a concentration of 99% C 2 h 5 Soak in OH for 1~12 hours. Take out after cooling to room temperature, filter to remove residual C 2 h 5 OH, dry at 90~120°C for 1~12 hours, grind it finely to get white powder zirconium hydroxide carrier. Then impregnate Zr(OH) with ammonium metatungstate solution (W mass fraction is 15%) 4 , calcined at 800°C for 2 to 5 hours under a static air atmos...

Embodiment 2

[0024] The catalyst was prepared according to the method of Example 1, except that the mass fraction of W in the mixture was 10%. The conversion rate of n-heptane catalyzed by the obtained catalyst and the selectivity of isoheptane were shown in Table 3.

[0025] n-heptane conversion Isoheptane selectivity Product yield 38.56 95.83% 36.95%

[0026] table 3

[0027] Note: In the evaluation of reaction performance, samples were taken for analysis after 20 minutes of stable reaction, and the test time was all over 48 hours.

Embodiment 3

[0029] The catalyst was prepared according to the method of Example 1, except that the mass fraction of W in the mixture was 18%. The conversion rate of n-heptane catalyzed by the obtained catalyst and the selectivity of isoheptane were shown in Table 4.

[0030] n-heptane conversion Isoheptane selectivity Product yield 32.81% 90.68% 29.75%

[0031] Table 4

[0032] Note: In the evaluation of reaction performance, samples were taken for analysis after 20 minutes of stable reaction, and the test time was all over 48 hours.

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Abstract

The invention relates to a preparation method of a WO3 / ZrO2 solid super acidic catalyst. The method comprises the following steps that a zirconium hydroxide emulsion is heated in a round-bottom flask with a condenser pipe for 1-24h; a zirconium hydroxide solution is repeatedly leached and washed till a pH value of a filtrate is 6-8 and no chlorion exists; a zirconium hydroxide filter cake is soaked in C2H5OH with the concentration of 99% in a constant-temperature drying oven; drying is conducted after C2H5OH is removed; powdery zirconium hydroxide is obtained, and ground till a particle size is less than 80 meshes; and then ammonium metatungstate serves as a raw material, and is impregnated by an equal-volume method, dried and roasted to form the WO3 / ZrO2 solid super acidic catalyst. The method has the advantages of easiness and simplicity in operation, low reaction temperature, good stability and the like; in addition, in the WO3 / ZrO2 solid super acidic catalyst prepared by the method, the proportion of a tetragonal phase of zirconium dioxide is increased; a specific surface area is increased; the activity of catalytic reaction is improved obviously; and the cost is lowered effectively.

Description

technical field [0001] The invention relates to a WO with tungsten trioxide as the active component and zirconium dioxide as the carrier 3 / ZrO 2 Preparation method of solid superacid catalyst. Background technique [0002] In 1979, Japanese scientists Hino and others first synthesized SO 4 2- / ZrO 2 The solid superacid was used to catalyze the isomerization of n-butane for the first time, and it was found that it had good isomerization activity. However, due to the SO in the process of reaction and regeneration 4 2- easy in H 2 and air atmosphere into H 2 S and SO 2 , causing environmental pollution and the loss of active components to significantly reduce the acid strength, limiting its industrial application. For this reason, in 1988, Hino and Arata et al. treated zirconia with molybdic acid and ammonium tungstate instead of sulfuric acid, and obtained a supported oxide solid superacid WO 3 / ZrO 2 and M O o 3 / ZrO 2 . This kind of solid superacid catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/30C07C9/16C07C5/27
Inventor 汪颖军李言所艳华常伟
Owner NORTHEAST GASOLINEEUM UNIV
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