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Method for preparing catalyst carrier used for preparing vinyl acetate by fluidized bed process

A technology of catalyst carrier and vinyl acetate, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc., and can solve the problem of low catalyst selectivity

Active Publication Date: 2010-11-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the catalyst produced by the carrier produced by the prior art has the problem of low selectivity, and a new preparation method for the catalyst carrier used in the production of vinyl acetate by the fluidized bed process is provided

Method used

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  • Method for preparing catalyst carrier used for preparing vinyl acetate by fluidized bed process
  • Method for preparing catalyst carrier used for preparing vinyl acetate by fluidized bed process
  • Method for preparing catalyst carrier used for preparing vinyl acetate by fluidized bed process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) carrier preparation

[0022] The specific steps of carrier preparation are:

[0023] a) will contain 5% coarse porous microsphere silica gel (specific surface is 328 meters 2 / gram, pore volume 1.19 milliliters / gram, average pore diameter 14.5 nanometers), 22.5% (calculated as silicon dioxide) silica sol (colloid particle diameter 78 nanometers) and the mixture of 72.5% water wet grinding 12 hours with stirring mill.

[0024] b) The obtained slurry is then subjected to spray granulation with a centrifugal spray dryer under the conditions of an inlet temperature of 310° C., an outlet temperature of 150° C., and an atomization disc rotation speed of 32 Hz.

[0025] c) Calcining the obtained spray-dried product in a muffle furnace at 600° C. for 6 hours. The specific surface of this product is 295 meters 2 / g, the pore volume is 0.76 ml / g, and the average pore diameter is 11.2 nanometers.

[0026] d) 400 grams of roasted product and 3000 grams of aqueous electroly...

Embodiment 2

[0046] (1) carrier preparation

[0047] The operation is carried out according to [Example 1] part (1), and the specific process parameters and results are shown in Table 1 to Table 3.

[0048] (2) Catalyst preparation

[0049] Take 100 g of the carrier, add 72 ml of Na containing 0.86 g of Pd and 0.42 g of Au under stirring 2 PdCl 4 , HAuCl 4Aqueous solution, stirred evenly, left standing for 1 hour, dried at 80° C. for 12 hours, then slowly added to 384 g of 5% hydrazine hydrate aqueous solution under stirring. After adding hydrazine hydrate, let it stand for 12 hours and stir thoroughly every 3 hours. Then filter, the filter cake was washed with deionized water for 12 hours, then dried at 80°C for 12 hours, then added 72 grams of KOAc aqueous solution containing 6.6 grams of KOAc under stirring, stirred evenly, stood for 1 hour, and dried at 60°C for 12 hours. Hours to get the finished catalyst. The weight composition of the catalyst is: Pd 0.791%, Au 0.383%, KAc 6.08...

Embodiment 3

[0057] (1) carrier preparation

[0058] The operation is carried out according to [Example 1] part (1), and the specific process parameters and results are shown in Table 1 to Table 3.

[0059] (2) Catalyst preparation

[0060] Take 100 g of the carrier, add 60 ml of Na containing 1.37 g of Pd and 0.74 g of Au under stirring 2 PdCl 4 , HAuCl 4 Aqueous solution, stirred evenly, left standing for 1 hour, dried at 80° C. for 12 hours, then slowly added to 630 g of 5% hydrazine hydrate aqueous solution under stirring. After adding hydrazine hydrate, let it stand for 12 hours and stir thoroughly every 3 hours. Then filter, wash the filter cake with deionized water for 12 hours, then dry at 80°C for 12 hours, then add 72 grams of KOAc aqueous solution containing 8.8 grams of KOAc under stirring, stir well, let stand for 1 hour, and dry at 60°C for 12 hours Hours to get the finished catalyst. The weight composition of the catalyst is: Pd 1.22%, Au 0.655%, KAc 7.81%.

[0061] F...

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Abstract

The invention relates to a method for preparing a catalyst carrier used for preparing vinyl acetate by a fluidized bed process, which mainly solves the problem that a catalyst prepared by using a carrier prepared in the prior art has low selectivity. The method comprises the following steps of: a) preparing serum from a mixture of porous silicon dioxide and silica sol; b) spray granulating; c) roasting spray granulated products; d) performing thermal treatment on the obtained product in electrolyte aqueous solution to obtain a precursor; and e) drying the precursor I to obtain the carrier finished product. The technical scheme better solves the problem and can be used for the industrial preparation of the catalyst carrier for synthesizing the vinyl acetate by an ethylene process and the fluidized bed process.

Description

technical field [0001] The invention relates to a preparation method of a catalyst carrier used for producing vinyl acetate by a fluidized bed process. Background technique [0002] With ethylene, acetic acid and oxygen or oxygen-containing gas as raw materials, the catalyst used in the reaction of fluidized bed gas phase reaction to prepare vinyl acetate is to use silicon dioxide as the main body of the porous material as the carrier to support Pd, Au and KAc (acetic acid Potassium), this technique is well known to those of ordinary skill in the art. [0003] USP 5591688 has reported a kind of preparation method that is used for the preparation method of the catalyst support of vinyl acetate in ethylene method fluidized bed process, and this method is to adopt nano-scale fumed silica and silica sol to mix and make slurry, spray dry this slurry, high temperature The catalyst carrier for synthesizing vinyl acetate by ethylene method fluidized bed process is obtained by lower...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/08B01J21/06B01J37/08B01J35/02C07C69/15C07C67/055B01J35/00
Inventor 张士福杨运信张丽斌宋朝红查晓钟秦群英
Owner CHINA PETROLEUM & CHEM CORP