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Preparation method of composite oxide carrier

A technology of composite oxides and oxides, applied in the direction of catalyst supports, chemical instruments and methods, chemical/physical processes, etc., can solve the problem of rapid precipitation of zirconia or titania, affecting the physical and surface properties of the carrier, and different particle sizes problems, achieve large pore volume, improve utilization rate, 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

However, the zirconium or titanium in the above method is added after the alumina is gelled, and the pH value of the alumina is in the alkaline range, while the zirconium-containing solution or the titanium-containing solution is acidic. When the two are mixed, it is easy to cause zirconia or titanium oxide Rapid precipitation, different particle sizes, re-peptization of the original alumina precipitation, wide particle size distribution of alumina, which in turn affects the physical and surface properties of the carrier

Method used

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  • Preparation method of composite oxide carrier
  • Preparation method of composite oxide carrier

Examples

Experimental program
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Embodiment 1

[0032] Mix 1000ml 2mol / L aluminum nitrate with 22ml silica gel (containing SiO 2 25wt%) were mixed, ammonia water was added, the pH value was adjusted to 8.5, and Sol A was obtained by reacting at 60°C. 10g / 100ml of Zr(NO 3 ) 4 The solution is mixed with the theoretical complexing amount of ammonium tartrate to obtain the complex solution B. Sol A and complex solution B are mixed, and vigorously stirred, and 30wt% hydrogen peroxide is added at room temperature to make Zr 4+ :H 2 o 2 =1:3 (molar ratio), after reacting for 3 hours, heat up to 60°C and age for 1 hour, 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. 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 10 wt%, and the content of silicon oxide was 5 wt%. The main properties are listed in Table 1.

[0033] Take 123g of composite oxide dry glue, 13.9g ...

Embodiment 2

[0035] Mix 1 mol / L aluminum sulfate and 1 mol / L sodium metaaluminate in parallel, adjust the pH value to 7.0, and react at 50°C to obtain Sol A. The rest are the same as in Example 1 to obtain the composite oxide dry glue. 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 50 wt%, and its main properties are listed in Table 1.

[0036] Take 114g of composite oxide dry glue, 27.8g of SB powder, add 3g of scallop powder, 3ml of dilute nitric acid and 2ml of acetic acid, knead, extrude, dry at 120°C for 3 hours, and roast at 600°C for 3 hours to obtain a composite oxide carrier , and its main properties are listed in Table 2.

Embodiment 3

[0038] Mix 1000ml 2mol / L aluminum nitrate with 22ml silica gel (containing SiO 2 25wt%) mixed, add ammonia, adjust the pH value to 7.5, react at 60°C to get sol A, and mix 20g / 100ml of TiCl 4 The solution is mixed with EDTA of theoretical complexing amount to obtain complex solution B. Mix sol A and complex solution B, and stir vigorously, add 100ml of 30wt% hydrogen peroxide at room temperature, heat up to 60°C for 1 hour after reacting for 3 hours, filter with suction, wash 3 times with deionized water, C and dried for 3 hours and pulverized to obtain dry composite oxide glue. The composite oxide dry glue was calcined at 600°C for 3 hours to obtain a composite oxide, wherein the content of titanium oxide was 10wt%, and the content of silicon oxide was 5wt%. Its main properties are listed in Table 1

[0039] 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 6...

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Abstract

The invention discloses a preparation method of a composite oxide carrier. A composite oxide gel adopted in the method of the invention is obtained by the steps of: first preparing an aluminum hydroxide sol and a water solution containing a group IVB metal complex, then mixing the sol and the water solution, adding dropping a hydrolysis promoter so as to obtain a mixed precipitate, which is then subjected to aging, washing, filtering and drying. The composite oxide gel obtained by the method can make most of group IVB metal oxides distributed on an alumina surface so as to weaken influence onan alumina pore structure, enhance the catalysis assisting effect of group IVB metal oxides, and improve the pore structure and surface performance of the composite oxide carrier. Therefore, the vulcanizing property of a catalyst with the carrier of the invention can be improved, and loaded active metals are easy for reduction.

Description

technical field [0001] The invention relates to a preparation method of a composite oxide carrier, in particular to a preparation method of a composite oxide carrier used for preparing a hydrogenation refining catalyst. 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, Group IVB metal oxides (zirconia, titania) have shown unique catalytic activity as supports or catalysts in the field of catalysis due to their simultaneous acidic and basic surface centers, oxidizing and reducing...

Claims

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Application Information

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