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Preparation method and application of silicon dioxide coating type integral catalyst

A monolithic catalyst and silicon dioxide technology, which is applied in the direction of physical/chemical process catalysts, ketene preparation, chemical instruments and methods, etc., can solve the problems of fast catalyst deactivation rate, poor reaction selectivity, long process, etc., and achieve good results Adsorption effect, small bed pressure drop, high dispersion effect

Active Publication Date: 2019-07-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is the problems of poor reaction selectivity, long flow process and fast catalyst deactivation rate in the previous literature technology, and a method for preparing a novel silica-coated monolithic catalyst is provided. At the same time, the present invention Also provided is a catalyst and its application in the process of cracking organic carboxylic acids to produce enones, which has the advantages of high target product selectivity and good catalyst stability, and has good industrial application value

Method used

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  • Preparation method and application of silicon dioxide coating type integral catalyst
  • Preparation method and application of silicon dioxide coating type integral catalyst
  • Preparation method and application of silicon dioxide coating type integral catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] The silica-coated monolithic catalyst is prepared by impregnation method, and the specific steps are as follows:

[0063] (1) Weigh 100g of cordierite powder, 15g of hydroxymethyl cellulose, 10g of kaolin, 20g of pore-forming agent graphite, and 50g of water, mix them in a mixer, and mechanically stir for more than 1h to obtain a preliminary mixed coarse mud, kneading into After stripping, move it into a vacuum mud refining machine, practice the mud 3 to 5 times, wrap it into a ball, and freeze and rot for 4 hours to obtain fine mud.

[0064] (2) Pass the fine sludge obtained in step (1) through a piston-type ceramic extruder to obtain extruded ceramic blanks, use a cutting machine to segment the blanks according to the size of the reactor, move them into an oven for drying, and put them into Roasted in a muffle furnace to obtain several cylindrical monolithic honeycomb ceramic carriers with a size of Φ10mm*50mm, 33 small holes and a porosity of 60%.

[0065] (3) Accur...

Embodiment 2~5

[0070] The silicon dioxide-coated monolithic catalyst prepared in Example 1 is loaded into a fixed-bed reactor, and isobutyric acid is used as a raw material, and isobutyric acid and nitrogen are mixed in a volume ratio of 1 / 9 and passed through the cracking process equipped with a catalyst. In the reactor, the pressure is normal pressure, the contact time is 0.30s, and at different cracking temperatures, the reaction results of one-way cracking of isobutyric acid into dimethylketene are shown in Table 1:

[0071] Table 1 The results of the catalytic cracking reaction of isobutyric acid under the contact time of 0.30s

[0072] serial number temperature, ℃ Conversion rate,% DMK selectivity, % DMK yield, % 2 520 55.61 28.14 18.30 3 540 60.70 30.27 18.36 4 560 71.42 32.00 22.85 5 580 76.22 34.75 26.52

Embodiment 6~9

[0074] The silicon dioxide-coated monolithic catalyst prepared in Example 1 is loaded into a fixed-bed reactor, and isobutyric acid is used as a raw material, and isobutyric acid and nitrogen are mixed in a volume ratio of 1 / 9 and passed through the cracking process equipped with a catalyst. In the reactor, the pressure is normal pressure, the contact time is 0.20s, and at different cracking temperatures, the reaction results of one-way cracking of isobutyric acid into dimethylketene are shown in Table 2 below:

[0075] Table 2. The results of the catalytic cracking reaction of isobutyric acid under the contact time of 0.20s

[0076] serial number temperature, ℃ Conversion rate,% DMK selectivity, % DMK yield, % 6 520 46.56 28.22 13.14 7 540 56.34 31.19 17.57 8 560 70.59 44.37 31.32 9 580 74.77 44.67 33.44

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Abstract

The invention discloses a silicon dioxide coating type integral catalyst, a preparation method thereof and application thereof in the process of producing a ketenes compound through organic carboxylicacid cracking. The catalyst comprises a honeycomb integral catalyst carrier and an active silicon dioxide coating loaded on the integral catalyst, wherein an active ingredient is free silicon hydroxyl on the surface of silicon dioxide. On the basis of the honeycomb integral catalyst carrier, an impregnating method is adopted to prepare the silicon dioxide coating type integral catalyst. The preparation method includes: mixing raw material isobutyrtic acid and inert gas, and being in catalytic cracking reaction with the silicon dioxide coating type integral catalyst in a fixed bed reactor to obtain the ketenes compound, and recycling other products serving as liquid-phase raw materials to be returned into the fixed bed reactor. The catalyst has great industrial application value.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a method for preparing a silica-coated monolithic catalyst and the application of the catalyst in the process of cracking organic carboxylic acids to produce enone compounds. Background technique [0002] Ketones are important intermediates in organic synthesis, such as ketene, diketene, and dimethylketene. Since the molecular structure of ketene compounds contains two double bonds, it is highly unsaturated, and its chemical properties are very active. It can undergo reactions such as addition, decomposition and polymerization. It is a raw material for the production of various fine chemicals and is widely used. In the fields of dyes, medicines, pesticides, feed additives, etc. The molecular formulas of several typical enone compounds are: [0003] [0004] Ethylene ketene is the simplest ketene compound, generally exists as dimer diketene, and is currently mainly produced by pyroly...

Claims

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Application Information

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IPC IPC(8): B01J21/16B01J35/10C07C45/89C07C49/88
CPCB01J21/16C07C45/89B01J35/61C07C49/88
Inventor 毛伟刘严成有为时强王丽军李希
Owner ZHEJIANG UNIV