Method for preparing aluminum oxide dry glue powder containing silicon and zirconium

A technology of zirconium alumina and dry rubber powder, which is applied in the field of preparation of dry rubber powder as a carrier material for hydroprocessing catalysts, and can solve the problems of reduced utilization rate, unfavorable catalyst performance, and impact on the physical and chemical properties of the final carrier.

Active Publication Date: 2012-05-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above-mentioned prior art often uses the coprecipitation method or adds auxiliary agent zirconium when molding, and the former will cause ZrO 2 It enters the bulk phase during the co-precipitation process, and multiple substances are precipitated at the same time. The same precipitation conditions cannot be the best precipitation conditions for multiple substances at the same time, thus affecting the physical and chemical properties of the final carrier; while the latter is added to the kneading process. precursor, which is not conducive to the uniform dispersion of zirconium, both of which will cause ZrO 2 The utilization rate is reduced, and it is not conducive to the improvement of the performance of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 1L deionized water into the container, raise the temperature to 62°C, and add 3L containing Al 2 o 3 4g / 100mL aluminum chloride solution and containing NH 3 It is 10g / 100mL ammonia solution, the pH value is controlled at 8.0, and the feeding time is 80min.

[0034] After stopping the feed, the system was aged for 50min under the above temperature and pH conditions, and SiO was added 2 100mL of sodium metasilicate solution with a content of 10g, continue aging for 10min, then add 120mL of zirconium oxychloride solution with a Zr content of 8g, finish adding in 10min, control the pH value of the material to 6.5, continue aging for 60min, and then wash 4 times until Cl - / Al 2 o 3 <0.5% up to.

[0035]After the filter cake was dried at 100° C. for 15 hours, it was crushed until the particle size was less than 180 mesh and accounted for more than 95%, to obtain dry rubber powder A.

Embodiment 2

[0037] Add 1L deionized water into the container, raise the temperature to 65°C, and add 3L containing Al 2 o 3 5g / 100mL aluminum nitrate solution and containing NH 3 It is 10g / 100mL ammonia solution, the pH value is controlled at 8.2, and the feeding time is 45min.

[0038] After stopping the feeding, the system was aged for 20min under the above temperature and pH value conditions, and SiO was added 2 100ml of sodium metasilicate solution with a content of 6g was aged for 40min, and then filtered.

[0039] After stirring the filter cake in the container, add OH - Add 100 mL of sodium hydroxide solution with a content of 5 g in 10 minutes, then add 100 mL of a zirconyl nitrate solution with a zirconium content of 15 g, the addition time is 20 minutes, control the pH value of the material to 7.5, continue to stir for 30 minutes, and then filter.

[0040] Wash 3 times to NO 3 - / Al 2 o 3 <0.8%.

[0041] After the filter cake was dried at 120° C. for 10 h, it was crushe...

Embodiment 3

[0043] Add 1L deionized water into the container, raise the temperature to 65°C, and add 3L containing Al 2 o 3 2g / 100mL aluminum sulfate solution and containing Al 2 o 3 It is 18g / 100mL sodium aluminate solution, the pH value is controlled to 7.5, and the feeding time is 55min.

[0044] After the feeding was stopped, the system was aged for 40min under the conditions of the above temperature and pH value, and SiO was added 2 100ml of sodium metasilicate solution with a content of 9g was aged for 10min and then filtered.

[0045] Wash to SO 4 2- / Al 2 o 3 <3.5%, after stirring the filter cake in the container, add 500mL of sodium carbonate solution with a concentration of 1mol / L, and then add 400mL of zirconyl nitrate solution with a zirconium content of 22g. The addition time is 10min, and the pH value of the control material is 8.5, continue to stir for 20 minutes and then filter.

[0046] Wash 3 times to SO 4 2- / Al 2 o 3 <1.5% until.

[0047] After the filter...

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Abstract

The invention discloses a method for preparing aluminum oxide dry glue powder containing silicon and zirconium. The method comprises the following steps: after an solution containing an aluminum compound and precipitating agent are subjected to gel forming reaction, adding a compound solution containing zirconium into the mixture under the condition of controlling proper pH value and the like, adding a compound containing silicon into the mixture before, after or at the same time of adding the compound containing zirconium, and then washing, filtering and drying the mixture to obtain the dry glue containing the silicon and the zirconium. Through optimizing process and condition of adding the silicon and the zirconium as assistant into the aluminum oxide dry glue, the silicon and the zirconium are evenly dispersed on the surface of aluminum oxide, and can give full play of the assistant.

Description

technical field [0001] The invention relates to a preparation method of alumina dry rubber powder containing silicon and zirconium, in particular to a preparation method of silicon and zirconium containing dry rubber powder of hydrogenation treatment catalyst carrier material. Background technique [0002] Most supported catalysts are prepared by impregnation method, such as various hydrogenation catalysts. Alumina is often used as a carrier material for this type of catalyst. but pure Al 2 o 3 The interaction force between the active metal on the surface and the carrier is relatively large, and it is easy to form inactive species (such as the formation of nickel-aluminum spinel), and it is difficult to completely vulcanize to form a type II active phase with high hydrogenation activity. How to weaken the strong interaction between the metal and the support becomes the key to the preparation of highly active hydrogenation catalysts. [0003] In order to improve the activ...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): B01J32/00B01J21/06
Inventor彭绍忠杨占林刘雪玲姜虹
OwnerCHINA PETROLEUM & CHEM CORP