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Composite catalyst of silica-coated multi-metal nanoparticles and activated carbon powder and preparation method and application thereof

A technology of activated carbon powder and nanoparticles, which is applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, catalyst carrier, etc. It can solve the problems of poor carrier hardness and sensitive placement, and achieve high mechanical strength , prolong the storage time, and increase the effect of type selection

Inactive Publication Date: 2010-05-05
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the poor hardness of the carrier of the Wacker type catalyst, and to place more sensitive defects in the air, to provide a composite catalyst with silica gel wrapped multi-metal nanoparticles and activated carbon powder, which is used for one-step methanol gas-phase oxidative carbonylation Synthesis of dimethyl carbonate with high activity and good stability

Method used

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  • Composite catalyst of silica-coated multi-metal nanoparticles and activated carbon powder and preparation method and application thereof
  • Composite catalyst of silica-coated multi-metal nanoparticles and activated carbon powder and preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0025] Silica gel-coated multi-metal nanoparticles and activated carbon powder particle catalysts were prepared by Sol-Gel method (Sol-Gel). Add 0.7 grams of metal active components and additives (molar ratio Pd: Cu: K=1: 18.6: 14.7) in the three-necked flask, then add 10 milliliters of tetraethyl orthosilicate, 7 milliliters of diethylene glycol, 6 The deionized water of milliliter and the mass percentage concentration of 2 milliliters are that the concentrated hydrochloric acid of 36.5% is stirred in 70 ℃ of water baths, adds the activated carbon powder of 2 grams (coal-based activated carbon, 80~100 orders, BET specific surface area 809m 2 / g, pore volume 0.4ml / g), stirred for 2 hours to obtain a sol, aged at room temperature for 6 hours to become a gel, and then put it into a vacuum drying oven (vacuum degree of 0.01MPa) at 120°C for 3 hours to obtain Silica gel wrapped catalyst 5.5 grams. (The mass fraction of each component in the catalyst is polymetallic nanoparticles:...

Embodiment 2

[0029] The specific preparation steps of the catalyst are as in Example 1, except that the co-solvent is ethanol instead of diethylene glycol.

[0030] Carry out activity evaluation on continuous tubular fixed-bed reactor, evaluation condition is as embodiment 1, and reaction product is divided into gas-liquid two-phase through condensation, records through gas chromatography online analysis in 6 hours: the space-time yield of dimethyl carbonate is 570g·L-cat -1 h -1 , the conversion of methanol was 21%, and the selectivity of carbon monoxide was 51%.

Embodiment 3

[0032] The specific preparation steps of the catalyst are as in Example 1.

[0033] Weigh 1ml of the above-prepared catalyst with a particle size of 20-40 mesh and mix it with 1ml of quartz sand with the same particle size as the catalyst, and place it in a tubular fixed-bed reactor with an inner diameter of 8mm for activity evaluation, carbon monoxide 40.0ml / min , Oxygen 16.5ml / min mixed with methanol 0.11ml / min, heated to 120°C by a preheater, and then entered the catalyst reaction bed, the space velocity of the raw material gas was 7100h -1 , the reaction temperature is 160°C, the reaction pressure is 0.3MPa, the reaction product is condensed into gas-liquid two-phase, and the gas chromatography is analyzed online for 6 hours: the space-time yield of dimethyl carbonate is 590g·L-cat -1 h -1 , the conversion of methanol was 15%, and the selectivity of carbon monoxide was 38%. Continue to catalyze the reaction, and when running for 12 hours, the space-time yield of dimethyl...

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Abstract

The invention relates to a composite catalyst of silica-coated multi-metal nanoparticles and activated carbon powder. The catalyst comprises a multi-metal nanoparticle component, the activated carbon powder and a carrier, wherein the metal nanoparticles comprise palladium, copper and potassium, and the molar ratio of Pd: Cu: K is equal to 1: 18.6: 14.7; and the carrier is silica. The weight percents of the components are as follows: 10%-20% of multi-metal nanoparticles, 10%-50% of activated carbon powder and 40%-85% of carrier. The catalyst can effectively prolong the storage time of an original Wacker type catalyst in the air and reduce the air sensitivity. Furthermore, as the carrier becomes activated carbon and the silica, the hardness is higher than that of the pure activated carbon, and the hardness of the catalyst is 2-20 times of that of the catalyst which takes the pure activated carbon as the carrier, thereby leading the mechanical strength of the carrier to be higher than that of the pure activated carbon carrier and expanding the selection range of the types of catalyst reactors.

Description

Technical field: [0001] The invention belongs to the synthesis of dimethyl carbonate, in particular to a composite catalyst comprising silica gel-wrapped polymetallic nanoparticles and activated carbon powder, and a preparation method and application thereof. technical background: [0002] Dimethyl Carbonate (Dimethyl Carbonate, referred to as DMC) is a typical green chemical product that has attracted widespread attention at home and abroad in recent years. Because the molecular structure contains -CH 3 , -C=O, -O-CH 3 、-COOCH 3 Such functional groups can carry out reactions such as methylation, carbonylation, methoxylation and carboxymethylation, and can replace highly toxic dimethyl sulfate (DMS), phosgene (COCl 2 ), methyl chloride (CH 3 Cl) and methyl chloroformate (ClCOOCH 3 ) react with a variety of alcohols, phenols, hydrazine and ester compounds to synthesize many high value-added downstream products, so it has a wide range of applications in the fields of plast...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J32/00B01J37/00C07C69/96C07C68/00
Inventor 王延吉丁晓墅岳川赵新强王淑芳
Owner HEBEI UNIV OF TECH
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