Method for synthesizing high specific surface area ordered mesoporous metal oxide by using hard template agent

A high specific surface area, hard template technology, applied in the direction of rare earth metal compounds, chromium oxide/hydrate, chemical instruments and methods, etc., can solve the problems of poor pore structure regularity, easy channel collapse, and poor universality of the method. Achieve the effects of narrow pore size distribution, low preparation cost and high specific surface area

Inactive Publication Date: 2008-07-09
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the disadvantages of poor sample pore structure regularity, easy collapse of the channel, and poor universality of the method obtained by other organic template methods in the past.

Method used

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  • Method for synthesizing high specific surface area ordered mesoporous metal oxide by using hard template agent
  • Method for synthesizing high specific surface area ordered mesoporous metal oxide by using hard template agent
  • Method for synthesizing high specific surface area ordered mesoporous metal oxide by using hard template agent

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: At room temperature, in 100mL 0.5mol / L hydrochloric acid solution, add 2.7g triblock copolymer (EO) 20 (PO) 70 (EO) 20 (Pluronic P123), stir until dissolved, slowly (2°C / min) heat up to 35°C, add 2.8g n-butanol while stirring, and keep stirring at 35°C for 1 hour, then add 5.8g orthosilicon to the above solution Ethyl acetate (the molar ratio of each substance is: ethyl orthosilicate: triblock copolymer (EO) 20 (PO) 70 (EO) 20 : hydrochloric acid: deionized water: n-butanol=1: 0.017: 1.83: 195: 1.31), keep stirring at 35°C for 24 hours, transfer to an autoclave and heat at 100°C for 24 hours, filter, deionized water and ethanol After washing, it was dried at 60°C, and then the temperature was programmed in a muffle furnace (1°C / min) to 550°C and burned at 550°C for 4 hours to obtain a cubic phase mesoporous silica (KIT-6) white powder. The specific surface area of ​​the resulting KIT-6 is 780m 2 / g, the average pore diameter is 3nm.

[0021] Add 1.0...

Embodiment 2

[0022] Example 2: The synthesis of hard template KIT-6 is the same as that in Example 1. Add 0.5g of ammonium dichromate to 10mL of 50wt% ethanol solution, stir to dissolve, add 0.5g of KIT-6 white powder to the above solution, ultrasonically disperse for 100 minutes, and then place the mixture at 40°C under magnetic stirring Evaporated until the obtained solid was heated to 400°C at a rate of 1°C / min in a nitrogen atmosphere (nitrogen flow rate of 30mL / min) and kept at 400°C for 4 hours, and finally washed with 10wt% HF solution to remove the silicon template. After drying at 60°C for 24 hours, the mesoporous polycrystalline chromium oxide powder was obtained with a specific surface area of ​​167m 2 / g, the average pore diameter is 7nm.

Embodiment 3

[0023]Example 3: The synthesis of hard template KIT-6 is the same as that in Example 1. Add 1.2g of chromium oxalate to 10mL of absolute ethanol, stir to dissolve, add 0.5g of KIT-6 white powder to the above solution, ultrasonically disperse for 100 minutes, then evaporate the mixture to dryness at 40°C under magnetic stirring, The obtained solid was heated up to 400° C. at a rate of 1° C. / min in a nitrogen atmosphere (nitrogen flow rate of 30 mL / min) and kept at 400° C. for 4 hours. Finally, the silicon template was removed by washing with 10 wt % HF solution, and then at 60 After drying at ℃ for 24 hours, the mesoporous polycrystalline chromium oxide powder is obtained, and its specific surface area is 125m 2 / g, the average pore diameter is 15nm.

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Abstract

A synthesis method of order mesoporous metal oxide with high specific surface area by hard template agent belongs to the filed of the preparation of solid mesoporous materials. The prior art is difficult to control the problems of the hydrolysis rate of metal salt, easy collapse and the poor universality of channels when templates are removed by calcination, etc. In the invention, firstly, hard template agent cubic-phase mesoporous silicon oxide powder is synthetized; the silicon oxide powder is added into 50 to 95wt percent of ethyl alcohol solution of metal salt with the concentration of 0.12 to 0.40 mol/L to form mixed solution; after 90 to 120 min of ultrasonic dispersion, the product is mixed again, vaporized under the temperature of 40 DEG C to 50 DEG C and dried; and then the product is heated to 400 DEG C to 850 DEG C in atmosphere at 1 DEG C/min, and kept for 4 hours under the temperature to obtain the mesoporous oxide precursor powder; the mol ratio of the cubic-phase mesoporous silicon oxide powder and the metal salt is 7-14; 10wt percent of HF solution is used to wash, so as to remove the cubic-phase mesoporous silicon oxide template agent, and the product is dried under 60 DEG C to 70 DEG C for 20 to 24 hours. The mesoporous metal oxide of the invention is suitable to be adsorbent, catalyst, carrier, etc., and is applicable to dyes, magnetic, photoelectric materials, etc.

Description

technical field [0001] The invention relates to a preparation technology of solid mesoporous materials, in particular to a method for synthesizing ordered mesoporous metal oxides with high specific surface area by using cubic phase mesoporous silicon oxide (KIT-6) powder as a hard template. Background technique [0002] In recent years, the preparation technology of nanoparticles and ordered porous materials has been developed rapidly, making it possible to controlly synthesize such materials. Due to the high specific surface area and pore volume of mesoporous oxide materials, it has become an important research object in surface structure and heterogeneous catalysis, and is widely used in gas separation, heterogeneous catalysis, energy storage, printing and dyeing, Electromagnetic, optoelectronic and many other fields. Therefore, it is of great practical value to develop a method for preparing mesoporous metal oxides with high specific surface area. [0003] The usual pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01G37/02C01F17/00
Inventor 戴洪兴夏云生何洪訾学红
Owner BEIJING UNIV OF TECH
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