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Method for preparing zirconia-alumina composite oxide carrier

A composite oxide and alumina technology, applied in catalyst carriers, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of rapid precipitation of zirconia, wide particle size distribution, and different particle sizes, and achieve easy vulcanization. , the effect of narrow pore size distribution and simple production process

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

AI Technical Summary

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 carrier
  • Method for preparing zirconia-alumina composite oxide carrier

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Mix 1000ml 2mol / L aluminum nitrate with 20ml silica gel (containing SiO 2 25wt%) and mixed, adding ammonia water to adjust the pH to 7, and reacting at 80° C. to obtain sol A. 1mol / l ZrCl 4 The solution and dilute ammonia water were added dropwise to a beaker containing ethanol and deionized water. The ethanol accounted for 15v% of the water. The pH value was controlled to be 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 200 ml of ethanol, filter with suction, wash 3 times with deionized water, dry at 120°C for 3 hours and pulverize to obtain a composite oxide dry glue. After calcination at 600° C. for 3 hours, a composite oxide was obtained, in which the content of zirconia was 60 wt % and the content of silicon oxide was 1.5 wt %. The main properties are listed in Table 1.

[0033] Take 123g of composite oxide dry glue, 13.9g of SB powder, add 3g of succulent powder, 5ml of di...

Embodiment 2

[0035] Mix 100ml 2mol / L aluminum nitrate with 20ml silica gel (containing SiO 2 25wt%) and mixed, adding ammonia water to adjust the pH to 7.0, and reacting at 60° C. to obtain sol A. Under stirring conditions, oxalic acid (0.1 mol / l) was slowly dropped into 0.1 mol / l zirconium nitrate to make pH=5.5, and after stirring for 10 minutes, it was put into a three-necked flask and heated to 95°C, and refluxed at a constant temperature for 2 Sol B was obtained within hours. Dilute sol B twice with distilled water, mix with sol A, stir for 2 hours, heat up to 50°C, age for 2 hours, add 200 ml of ethanol, filter with suction, wash with deionized water 3 times, dry at 120°C for 3 hours and pulverize. The composite oxide dry glue was calcined at 600° C. for 3 hours to obtain a composite oxide, wherein the content of zirconium oxide was 30 wt %, and the content of silicon oxide was 2 wt %. The main properties are listed in Table 1.

[0036] Take 114g of composite oxide dry glue, 27.8g ...

Embodiment 3

[0038] 1 mol / L aluminum sulfate and 1 mol / L sodium aluminate were mixed in co-current flow, the pH value was adjusted to 7.0, and sol A was obtained by reacting at 50°C. The rest are the same as in Example 1. The content of zirconia in the composite oxide is 10wt%, and its main properties are listed in Table 1.

[0039] Take 132g of composite oxide dry glue and 13.9g of SB powder, add 3g of succulent powder, 5ml of dilute nitric acid, knead, extrude, dry at 120 °C for 3 hours, and bake at 600 °C for 3 hours to obtain a composite oxide carrier. The properties are listed in Table 2.

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Abstract

The invention discloses a method for preparing a zirconia-alumina composite oxide carrier. An aluminum hydroxide sol and a zirconium-containing sol are prepared firstly, and then are mixed, aged, washed, filtrated and dried to obtain a composite oxide xerogel, accordingly, 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 carrier 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 carrier, in particular to a preparation method of a zirconia-alumina composite oxide carrier used for preparing a hydrofinishing catalyst. Background technique [0002] The preparation process of alumina carrier 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 carriers at present. Inactive species, such as nickel-aluminum spinel, are less likely to form a highly reactive type II active phase. Therefore, the preparation and modification of alumina carriers and the preparation of aluminum-containing composite oxides have always been the research directions of scientists. At present, zirconia materials show unique catalytic activity and selectivity in the field of catalysis as supports or catalysts due to their simultaneous acidic and basic surface centers, oxidative an...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J21/06B01J21/12B01J35/10B01J27/19C10G45/08
Inventor 徐黎明高玉兰李崇慧陈光
Owner CHINA PETROLEUM & CHEM CORP
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