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Nano-crystal large poresize mesopore oxide material and its preparation method

A nano-crystallization and oxide technology, applied in chemical instruments and methods, titanium oxide/hydroxide, niobium compounds, etc., can solve the problems of insufficient mesopore order and thermal stability of materials, and achieve controllable synthesis conditions , high specific surface area, highly ordered effect

Inactive Publication Date: 2007-04-18
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on this aspect at home and abroad is still in its infancy, and the mesoporous order and thermal stability of the obtained materials are not high enough.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021]Example 1, Synthesis of highly ordered, thermally stable, two-dimensional hexagonal mesoporous titanium dioxide: 1 g of P123 template was dissolved in 10-30 g of ethanol, and stirred for 2-3 hours. Add 0.01 mole of ethyl titanate or isopropyl titanate or butyl titanate, and 0.02-8 g of one of the above acids, and continue stirring for 3-5 hours. The reaction mother liquor was transferred to a Petri dish, and evaporated to dryness at 10-30°C at 10-20% relative humidity. After 2-5 days, transfer it to an oven at 60-100°C for drying, then place it in a tube furnace or muffle furnace, and bake it at 350°C for 6 hours to obtain the desired material. Pore ​​diameter: 7.6nm, BET specific surface area: 270m 2 / g. Or calcined at 350°C for 6 hours, followed by calcining at 450°C for 2 hours, the pore size of the obtained material is: 6.0nm, and the specific surface area is: 170m 2 / g. Thermal stability up to 450°C. The pore wall crystal phase is anatase phase.

Embodiment 2

[0022] Example 2, highly ordered, highly thermally stable, two-dimensional hexagonal mesoporous titanium dioxide and silicon dioxide [xTiO 2 -ySiO 2 , x / y=(100-90) / (0-10)] Synthesis of composite material: 1 gram of P123 template was dissolved in 10-30 gram of ethanol, and stirred for 1-2 hours. Add 0.010-0.0085 mole of ethyl titanate or isopropyl titanate or butyl titanate, 0-0.0015 mole of ethyl orthosilicate and 0.02-8 g of one of the above acids, and continue stirring for 1-3 hours. The reaction mother liquor was transferred to a petri dish, and evaporated to dryness at 70-100% relative humidity and 60-80°C. After 2-5 days, transfer it to an oven at 70-100°C for drying, then place it in a tube furnace or muffle furnace, and bake it at 350°C for 6 hours, and then bake it at 400°C--800°C The required materials can be obtained within 2-4 hours. Pore ​​diameter: 7.7-6.0nm, BET specific surface area: 291-150m 2 / g. The highest thermal stability can reach above 750℃. The po...

Embodiment 3

[0023] Example 3, highly ordered, ultra-high thermal stability, two-dimensional hexagonal mesoporous titanium dioxide and silicon dioxide [xTiO 2 -ySiO 2 , x / y=(85-5) / (15-95)] Synthesis of composite material: 1 gram of P123 template agent was dissolved in 10-30 gram of ethanol, and stirred for 7-10 hours. Add 0.0085-0.0005 moles of ethyl titanate or isopropyl titanate, 0.0015-0.0095 moles of ethyl orthosilicate and 0.02-8 grams of one of the above acids, and continue stirring for 5-10 hours. The reaction mother liquor was transferred to a petri dish, and evaporated to dryness at 30-50% relative humidity and 10-30°C. After 2-5 days, transfer it to an oven at 60-100°C for drying, then place it in a tube furnace or muffle furnace, and bake it at 400°C for 6 hours, then at 600°C for 4 hours, and then at 650°C --Roast at 900°C for 2-4 hours to get the desired material. Pore ​​diameter: 4.0-7.7nm, BET specific surface area: 580--60m 2 / g. Thermal stability up to 900°C. The por...

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Abstract

The present invention belongs to the field of inorganic advanced material technology, in the concrete, it relates to a kind of nano crystal large-diameter mesopore oxide material and its preparation method. Said mesopore oxide material is synthesized by using inorganic precursor and organic template agent molecules through a self-assembly process including organic solvent evaporation and induction treatment in the acidic environment, its space group structure is two-dimensional hexagonal structure, three-dimensional hexagonal structure and three-dimensional cubic structure, its pore diameter range is 1-18nm, BET specific surface area is 50-800 sq.m/g and its thermal stability is higher than 400 deg.C.

Description

technical field [0001] The invention belongs to the technical field of inorganic advanced materials, and specifically relates to a mesoporous oxide material with different compositions and pore structures, highly ordered, high thermal stability, nano crystallization, and large aperture and a preparation method thereof. Background technique [0002] Silica-based mesoporous materials with uniform pore size distribution are formed using cations, anions, neutral molecular surfactants, and nonionic amphiphilic macromolecules as templates. These materials have adjustable pore size (2nm ~ 30nm), variable channel structure (two-dimensional channel, three-dimensional channel and layered structure), high specific surface area (up to 1500m 2 / g or more) and other structural features, can be used as adsorbents, catalysts, catalyst supports, etc., and thus have a very wide range of application values ​​in many fields. The above-mentioned template synthesis method has been extended to sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G1/02C01G23/047C04B35/46C01G33/00C01G35/00
Inventor 董维阳李哲伟孙尧俊赵东元华伟明吕新春
Owner FUDAN UNIV
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