Method for preparing zirconia-alumina composite oxide xerogel

A composite oxide, aluminum hydroxide sol technology, used in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problem of rapid precipitation of zirconia, wide particle size distribution, and different particle sizes. problem, to achieve the effect of large pore volume, low preparation cost and simple production process

Inactive Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, zirconia is added when the carrier is gelled. The pH value of alumina is in the alkaline range, while the zirconium-containing solution is acidic. When the two are mixed, it is easy to cause rapid precipitation of zirconia, with different particle sizes. Re-peptization of alumina precipitation, and then adding alkaline reagents, the particle size distribution of alumina is wide, which is easy to cause dispersion of pore size distribution

Method used

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  • Method for preparing zirconia-alumina composite oxide xerogel

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Mix 1000ml 2mol / L aluminum nitrate with 20ml silica gel (containing SiO 2 25 wt%), mixed with ammonia water to adjust the pH value to 7, and reacted at 80°C to obtain Sol A. 1mol / l ZrCl 4 The solution and dilute ammonia water were added dropwise in a beaker filled with ethanol and deionized water, the ethanol accounted for 15v% of the water, the pH value was controlled to 6.5, and the reaction temperature was 45°C to obtain Sol B. Mix sol B and sol A, stir for 2 hours, heat up to 50°C, age for 2 hours, add 200ml of ethanol, filter with suction, wash with deionized water for 3 times, dry at 120°C for 3 hours, and pulverize to obtain the composite oxide dry glue. Calcined at 600°C for 3 hours to obtain a composite oxide, in which the content of zirconia is 60wt%, and the content of silicon oxide is 1.5wt%. The main properties are listed in Table 1.

[0029] Take 123g of composite oxide dry glue, 13.9g of SB powder, add 3g of scallop powder, 5ml of dilute nitric acid, k...

Embodiment 2

[0031] Mix 100ml 2mol / L aluminum nitrate with 20ml silica gel (containing SiO 225 wt%), mixed with ammonia water to adjust the pH value to 7.0, and reacted at 60°C to obtain Sol A. Under the condition of stirring, oxalic acid (0.1mol / l) was slowly dropped into 0.1mol / l zirconium nitrate to make the pH value = 5.5, and after continuing to stir for 10 minutes, put it into a three-necked flask and heat it to 95°C, and reflux at a constant temperature for 2 Sol B was obtained in 1 hour. Dilute sol B twice with distilled water and mix it with sol A, stir for 2 hours, heat up to 50°C, age for 2 hours, add 200ml of ethanol, filter with suction, wash 3 times with deionized water, dry at 120°C for 3 hours and pulverize to obtain The composite oxide dry glue was calcined at 600°C for 3 hours to obtain a composite oxide, in which the content of zirconia was 30wt%, and the content of silicon oxide was 2wt%. The main properties are listed in Table 1.

[0032] Take 114g of composite oxide...

Embodiment 3

[0034] Mix 1 mol / L aluminum sulfate and 1 mol / L sodium aluminate in parallel, adjust the pH value to 7.0, and react at 50°C to obtain Sol A. All the other are identical with embodiment 1. Wherein the content of zirconia in the composite oxide is 10wt%, and its main properties are listed in Table 1.

[0035] Take 132g of composite oxide dry glue, 13.9g of SB powder, add 3g of scallop powder, 5ml of dilute nitric acid, knead, extrude, dry at 120°C for 3 hours, and roast at 600°C for 3 hours to obtain a composite oxide carrier.

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Abstract

The invention discloses a method for preparing a zirconia-alumina composite oxide xerogel. An aluminum hydroxide sol and a zirconium-containing sol are prepared firstly, and then are mixed, aged, washed, filtrated and dried to obtain the composite oxide xerogel. In the method, most of zirconia is distributed on the surface of alumina, the impact on a pore structure of the alumina is weakened, the co-catalysis of the zirconia is improved, the advantages of the alumina and the zirconia are fully utilized, and the obtained composite oxide xerogel has the characteristics of large pore volume, high specific surface area, concentrated pore size distribution and controllable acidity, and is suitable for being used as a hydrogenation catalyst carrier.

Description

technical field [0001] The invention relates to a preparation method of a zirconia-alumina composite oxide dry glue, in particular to a preparation method of a zirconia-alumina composite oxide dry glue used for preparing a hydrogenation refining catalyst carrier. Background technique [0002] The preparation process of the alumina support is simple, the specific surface area is high, the mechanical strength is good, and the pore size is suitable. It is one of the most widely used catalyst supports at present. Inactive species, such as nickel-aluminum spinel, are less likely to form highly reactive type II active phases. Therefore, the preparation and modification of alumina carriers and the preparation of aluminum-containing composite oxides have always been the research direction of scientists. At present, zirconia materials show unique catalytic activity and selectivity as supports or catalysts in the field of catalysis due to their simultaneous acidic and basic surface c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J32/00B01J21/06
Inventor 徐黎明高玉兰李崇慧陈光
Owner CHINA PETROLEUM & CHEM CORP
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