Method for preparing Cu/SiO2 catalyst

A catalyst and surfactant technology, applied in the field of preparation of supported catalysts, can solve the problems of uneven agglomeration of active components, low loading of active components, and growth of copper grains on the surface, achieving high copper loading, It is convenient for industrialization promotion and the effect of easy control of process conditions

Inactive Publication Date: 2010-09-15
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The current study shows that Cu / SiO 2 Catalysts have a wide range of uses as selective hydrogenation catalysts, and there are many preparation methods, but they all have certain limitations. For example, the carrier impregnation method is prone to uneven agglomeration of the active components at the edge of the fine particles of the carrier; although the ion exchange method It can disperse active components well, but the loading of active components is very low; Cu / SiO prepared by precipitation deposition method 2 The content of Cu in the catalyst is low, increasing the content of copper will lead to the growth of copper grains on the surface, which is easy to sinter

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Add 200ml of deionized water to the reactor equipped with a thermometer, a pH meter and a stirrer, and start the stirrer at a speed of 3000r / min, so that the temperature of the reactor is 80°C.

[0024] 2) Prepare an ethyl silicate solution with a concentration of 1.0 mol / L, and then add sodium dodecylbenzenesulfonate to the solution so that the concentration of sodium dodecylbenzenesulfonate is 0.01mol / L. Prepare a nitric acid solution with a concentration of 0.5mol / L.

[0025] 3) Add ethyl silicate solution in the reaction kettle at a flow rate of 3ml / min, and simultaneously add nitric acid solution dropwise, so that the pH value of the solution in the reaction kettle is 8.5, keep constant stirring speed and constant temperature in the reaction, and dropwise add Afterwards, aging at constant temperature for 1 to 2 hours under stirring.

[0026] 4) Dissolve 11ml of the solution obtained in step 3) into 18.5ml of absolute ethanol, and stir evenly. 1ml of HNO 3 , 8...

Embodiment 2

[0031] The preparation process is the same as in Example 1. The temperature of the reaction kettle is 80°C, the concentration of the ethyl silicate solution is 1.0mol / L, the concentration of sodium dodecylbenzenesulfonate is 0.01mol / L, the flow rate of the ethyl silicate solution into the reaction kettle is 3ml / min, and the reaction The pH value of the solution in the kettle is 8.5, Cu(NO 3 ) 2 The calculated amount of Cu in the solution is 2%, the pH value is adjusted by ammonia water to 7.2, the temperature of the constant temperature water bath is 65°C, and the specific surface area of ​​the catalyst is 715.5m 2 / g, the pore volume is 0.689cc / g, the obtained catalyst is used in the reaction of preparing ethylene glycol by hydrogenation of diethyl oxalate, the conversion rate of diethyl oxalate is 93.8% and the yield of ethylene glycol is 79.8%.

Embodiment 3

[0033] The preparation process is the same as in Example 1. The temperature of the reaction kettle is 85°C, the concentration of the ethyl silicate solution is 0.5mol / L, the concentration of sodium dodecylbenzenesulfonate is 0.01mol / L, the flow rate of the ethyl silicate solution into the reaction kettle is 3ml / min, and the reaction The pH value of the solution in the kettle is 9.0, Cu(NO 3 ) 2 The calculated amount of Cu in the solution is 2%, the pH value is adjusted by ammonia water to 7.5, the temperature of the constant temperature water bath is 65°C, and the specific surface area of ​​the catalyst is 714.9m 2 / g, the pore volume is 0.690cc / g, the obtained catalyst is used in the reaction of preparing ethylene glycol by hydrogenation of diethyl oxalate, the conversion rate of diethyl oxalate is 93.5% and the yield of ethylene glycol is 80%.

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Abstract

The invention relates to a catalyst, in particular to a method for preparing a Cu / SiO2 catalyst. The prepared Cu / SiO2 catalyst has the advantages of higher specific area, Cu loading capacity, dispersibility, stability and the like. The preparation method comprises the following steps of: preparing an ethyl silicate solution containing a surface active agent; preparing an inorganic acid solution; adding the prepared ethyl silicate solution containing a surface active agent to a reaction kettle, simultaneously adding the prepared inorganic acid solution to the reaction kettle, stirring, and aging at constant temperature to obtain a mixed solution; dissolving the obtained mixed solution in absolute ethyl alcohol, stirring, adding catalyst and ethanol, and stirring again to obtain a mixed liquid; adding a copper salt solution containing Cu of 2-5% in calculated amount to the obtained mixed liquid, adding ammonia water to adjust the pH value, stirring, aging at room temperature, carrying out water bath at constant temperature, drying, calcining, grinding, and sieving to obtain the Cu / SiO2 catalyst.

Description

technical field [0001] The present invention relates to a catalyst, in particular to a catalyst composition suitable for the polymerization of olefins, with SiO 2 The invention discloses a preparation method of a supported catalyst in which Cu is a carrier and Cu is an active component. Background technique [0002] The chemical composition of silica gel is SiO 2 At room temperature, there is a layer of physically adsorbed water on the surface of silica gel, and the silanol [-SiOH] structure exists on the surface at the same time. At 423-473K, most of the adsorbed water is desorbed, and [-SiOH] is mainly left on the surface. At higher temperatures, the adjacent [-OH] dehydrates to form a [Si-O-Si] structure. Silica gel has special pore structure, large specific surface area and excellent thermal stability, and is widely used as adsorbent, desiccant, thickener, chromatographic column support and catalyst support, etc. [0003] As the carrier of the catalyst required for ol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07C31/20C07C29/149
Inventor 罗学涛张蓉李锦堂
Owner XIAMEN UNIV
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