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Ordered mesoporous carbon-zirconium dioxide composite and preparation method thereof

A zirconium dioxide and composite material technology, applied in the field of materials, can solve the problems of low ZrO2 content, uneven particle size, uneven particle distribution, etc., and achieve the effects of good characteristics, uniform pore size distribution and low price

Inactive Publication Date: 2013-04-10
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two methods have some disadvantages, such as: ZrO in the composite material obtained by the one-step method 2 The content is low, ZrO 2 The particles are unevenly distributed in the material, and the particle size is not uniform; and the composite material obtained after post-processing is easy to block the pores, etc.

Method used

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  • Ordered mesoporous carbon-zirconium dioxide composite and preparation method thereof
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  • Ordered mesoporous carbon-zirconium dioxide composite and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 2

[0030] Example 1 Preparation of ordered mesoporous carbon-zirconia composite material with zirconia content of 30wt%.

[0031] Step 1: Pre-hydrolysis of zirconium tetrachloride: First, at 0°C, stir and mix 7.50ml of ethanol and 0.50ml of distilled water, cool to 0°C, add 0.643g of zirconium tetrachloride (2.75mmol) into the mixed solution, stir 2h. Zirconium tetrachloride was prehydrolyzed to form Stober's solution.

[0032] Step 2: At the same time as Step 1, dissolve 1.60 g of F127 in a mixed solution of 1.00 ml of distilled water and 8.00 g of ethanol at 40° C., and stir for 2 hours.

[0033] Step 3: Slowly transfer the Stober's solution dropwise to the solution in Step 2, and keep stirring at 40° C. for 0.5 h.

[0034] Step 4: Weigh 5.0 g of an ethanol solution of 20 wt % resole phenolic resin (molecular weight 1000) treated with anhydrous magnesium sulfate, add to the above solution, and continue stirring for 0.5 h.

[0035] Step 5: Apply the above solution evenly on t...

Embodiment 2 2

[0041] Example 2 Preparation of an ordered mesoporous carbon-zirconia composite material with a zirconia content of 50 wt%.

[0042] Step 1: Pre-hydrolysis of zirconium tetrachloride: First, at 0°C, 7.50ml of ethanol and 0.50ml of distilled water were stirred and mixed evenly, cooled to 0°C, 0.643g of zirconium tetrachloride was added to the mixed solution, and stirred for 2h. Zirconium tetrachloride was prehydrolyzed to form Stober's solution.

[0043] Step 2: At the same time as step 1, dissolve 1.00 g of F127 in a mixed solution of 1.00 ml of distilled water and 8.00 g of ethanol at 40° C., and stir for 2 hours.

[0044] Step 3: Slowly transfer the Stober's solution dropwise to the solution in Step 2, and keep stirring at 40° C. for 0.5 h.

[0045] Step 4: Weigh 3.0 g of an ethanol solution of 20 wt % resole phenolic resin (molecular weight 500) treated with anhydrous magnesium sulfate, add to the above solution, and continue stirring for 0.5 h.

[0046] Step 5: Apply the...

Embodiment 3 2

[0050] Example 3 Preparation of ordered mesoporous carbon-zirconia composite material with zirconia content of 70wt%.

[0051] Step 1: Prehydrolysis of zirconium tetrachloride: First, at 0°C, 7.50ml of ethanol and 0.50ml of distilled water were stirred and mixed evenly, cooled to 0°C, 0.643g of zirconium tetrachloride was added to the mixed solution, and stirred for 2h. Zirconium tetrachloride was prehydrolyzed to form Stober's solution.

[0052] Step 2: At the same time as step 1, dissolve 0.60 g of F127 in a mixed solution of 1.00 ml of distilled water and 8.00 g of ethanol at 40° C., and stir for 2 hours.

[0053] Step 3: Slowly transfer the Stober's solution dropwise to the solution in Step 2, and keep stirring at 40° C. for 0.5 h.

[0054] Step 4: Weigh 1.6g of an ethanol solution of 20wt% resole phenolic resin (molecular weight: 2000) treated with anhydrous magnesium sulfate, add to the above solution, and continue to stir for 0.5h.

[0055] Step 5: Apply the above sol...

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Abstract

The invention belongs to the technical field of mesoporous material preparation, and particularly relates to a solid carbon-zirconium dioxide nano composite in an ordered mesoporous structure, and a synthetic method of the composite. The composite is large in specific surface area (300-594m<2> / g) and pore volume (0.20-0.48cm<3> / g), and uniform in aperture (2.5-3.2nm). The synthetic method of the composite comprises the steps of taking zirconium tetrachloride as an inorganic precursor, A-stage phenolic resin as a polymeric source and F127 as a surfactant, and synthesizing the ordered mesoporous carbon-zirconium dioxide nano composite by integrating a ternary co-assembly method and an in-situ crystallization technology. The synthetic method is simple to operate and low in cost, and the prepared composite has immeasurable potential application prospects in many aspects.

Description

technical field [0001] The invention relates to the field of materials, and relates to an ordered mesoporous carbon-zirconia composite material and a preparation method thereof. Background technique [0002] In recent years, due to the wide application of zirconia in gas sensors, fuel cells, automobile catalysts, acid-base bifunctional catalysts, etc., it has received widespread attention. However, due to the low The specific surface and porosity limit its application. Many people try to use ionic or non-ionic surfactants as structure-directing agents to synthesize porous zirconia materials with high specific surface area and uniform pores. For example, Shi et al. used cetyltrimethylammonium bromide as a structure-directing agent and zirconium sulfate as an inorganic precursor to synthesize phosphorylated mesoporous zirconia materials by a hydrothermal method. However, the mesoporous materials obtained by the above method usually have poor thermal stability, the mesoporous...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01G25/02B82Y30/00C01B32/05
Inventor 万颖李燕
Owner SHANGHAI NORMAL UNIVERSITY
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