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Preparation of mesoporous zircite

A technology of mesoporous zirconia and zirconium salts, applied in zirconia and other directions, to achieve the effect of novel ideas

Inactive Publication Date: 2008-12-24
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But in summary, the preparation of ZrO 2 The method of mesoporous materials is generally a combination of sol-gel and template-assisted hydrothermal method, but the templates used are generally organic amines with single cationic groups (CTAB, etc.) or neutral surface active Agents (such as P123), so far there is no report on the use of Gemini cationic surfactant molecules (Gemini) containing two or more cationic groups as templates for the preparation of mesoporous ZrO 2 report

Method used

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  • Preparation of mesoporous zircite
  • Preparation of mesoporous zircite
  • Preparation of mesoporous zircite

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Use the following ratio (molar ratio) to configure the raw materials, zirconium oxychloride octahydrate: G1: NaOH: H 2 O=1:0.1:2:150. Dissolve G1 and NaOH in 140ml of water in a water bath at 80°C, stir at 300r / min for 1h, add the Zr salt solution dropwise at a rate of 1ml / min, continue stirring for 3h and age for 24h, then dissolve the suspension Transfer to a stainless steel reaction kettle, treat it in an oven at 110°C for 48h, and then take it out. The precipitate was washed alternately with water and hot ethanol at 80°C for several times, the filter cake was dried in an oven at 100°C, and the product was heated to 540°C at a rate of 3°C / min in a tube furnace and kept for 3.5 hours to obtain mesoporous ZrO 2 The nitrogen adsorption-desorption curve and corresponding pore size distribution curve of powder and product are shown in the attached figure 1 , the specific surface area of ​​the product is 113m 2 / g.

Embodiment 2

[0033] Use the following ratio (molar ratio) to configure the raw materials, zirconyl sulfate: CTAB: G2: NaOH: H2 O=1:0.055:0.055:2.5:150. Dissolve CTAB, G2 and NaOH in 140ml of water in a water bath at 80°C, stir at 300r / min for 1h, drop Zr salt solution at a rate of 2ml / min, continue stirring for 3h and age for 24h. The turbid liquid was transferred to a stainless steel reaction kettle, treated in an oven at 110° C. for 48 hours, and then taken out. After the precipitate was washed alternately with water and hot ethanol at 80 °C for several times, the filter cake was freeze-dried to directly obtain mesoporous ZrO 2 The nitrogen adsorption-desorption curve and corresponding pore size distribution curve of powder and product are shown in the attached figure 2 , the specific surface area of ​​the product is 151m 2 / g.

Embodiment 3

[0035] Use the following ratios (molar ratios) to configure the raw materials: zirconium oxychloride octahydrate: CTAB: G3: NaOH: H 2 O=1:0.7:0.5:2:150. Dissolve CTAB, G3 and NaOH in 140ml of water in a water bath at 80°C, stir for 1h under the condition of 300r / min, drop Zr salt solution at a speed of 1ml / min, continue stirring for 3h and age for 24h. The turbid liquid was transferred to a stainless steel reaction kettle, treated in an oven at 110° C. for 36 hours, and then taken out. After the sediment was washed alternately with water and hot ethanol at 80°C for several times, the filter cake was dried in an oven at 100°C, and the product was heated to 540°C at a rate of 3°C / min in a tube furnace and kept for 3 hours to obtain mesoporous ZrO 2 The nitrogen adsorption-desorption curve and corresponding pore size distribution curve of powder and product are shown in the attached image 3 , the specific surface area of ​​the product is 160m 2 / g.

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Abstract

The invention discloses a preparation method of mesoporous ZrO2 which is characterized by dissolving a template and zirconium salt with water and stirring the mixture; dropping a NaOH solution into the mixture and continuously stirring and aging the mixture to obtain a suspension solution; transferring the obtained suspension solution into a reactor and taking out the mixture after heat treatment at 100-140 DEG C; washing, drying and calcining the precipitate in the reactor with water and hot alcohol to obtain a ZrO2 mesoporous material; the template is binary star type Gemini surfactants or cetyl trimethyl ammonium bromide or the mixture of one of Gemino surfactants and cetyl trimethyl ammonium bromide. The obtained mesoporous ZrO2 solid solution is an important material in the catalytic field with a specific surface area more than 160m<2> / g.

Description

technical field [0001] The invention belongs to the technical field of catalytic material synthesis, and relates to a mesoporous zirconia (ZrO 2 ) preparation method. Background technique [0002] At present, catalyst materials in the field of petroleum catalysis generally require excellent catalytic ability and stable physical and chemical properties, especially high chemical stability. For the application fields such as petroleum catalytic cracking, the general catalyst use environment is around 300-500°C. Zirconia (ZrO 2 ) has extremely high chemical stability and thermal stability, and is insoluble in any acid or alkali at room temperature, and two distinct acidic centers and basic centers can be shown at different positions on its surface. These unique physical and chemical properties make ZrO 2 become a very ideal catalyst, while ZrO 2 It is also a very good carrier for the catalytic active center, which makes the preparation of ZrO 2 And the catalyst based on it...

Claims

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Application Information

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IPC IPC(8): C01G25/02
Inventor 杨华明欧阳静唐爱东阚开静
Owner CENT SOUTH UNIV
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