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Mesoporous hexaaluminate prepared by carbon template method and having large specific surface area and preparation method of hexaaluminate

A technology of high specific surface area and hexaaluminate, which is applied in the field of mesoporous high specific surface area hexaaluminate and its preparation, can solve the problem that it is difficult to form organic-inorganic mesoporous phase and the uniformity of hexaaluminate particles is not good enough , Inorganic network excessive growth and polymerization and other problems, to achieve the effect of good application prospects, cheap synthetic raw materials, and easy large-scale production

Active Publication Date: 2014-06-04
河北中芯凤华科技发展有限公司
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Problems solved by technology

[0003] The synthesis methods of hexaaluminate currently reported mainly include coprecipitation method, sol-gel method and inverse microemulsion method. The hexaaluminate prepared by different methods has great differences when used as a catalyst. Patents CN1698951A and CN101612572A discloses co-precipitation method to prepare hexaaluminate catalysts, which are used for light hydrocarbon combustion and N 2 O decomposition, this method is relatively simple, but the specific surface area of ​​the prepared hexaaluminate is small, and the catalyst performance is not high
CN101012066A adopts a urea combustion method, the calcination temperature is very high, and the uniformity of the obtained hexaaluminate particles is not good enough
[0005] At present, the preparation of inorganic nanomaterials by the template method is a relatively mature method, but when using the template method to prepare hexaaluminate with mesoporous high specific surface area, the synthesis of crystalline hexaaluminate-based mesoporous materials is much more complicated. The main difficulties in its synthesis are: first, the high hydrolysis polymerization rate of the metal salt precursor leads to excessive growth and polymerization of the inorganic network, making it difficult to form an organic-inorganic mesoporous phase; second, the valence change, Factors such as excessive crystallization of inorganic pore walls and removal of surfactants / templates (high-temperature roasting and solvent extraction) will destroy the target mesoporous structure; the third is the high crystallization temperature of hexaaluminate (about 1200 ° C), which is suitable for large For most hexaaluminate-based materials, the samples obtained at low calcination temperature often contain impurities. Although increasing the calcination temperature can reduce the amount of impurities, it will lead to excessive crystallization of the mesoporous pore walls, resulting in the collapse of the channels and the decrease of the specific surface area of ​​the sample. decrease

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  • Mesoporous hexaaluminate prepared by carbon template method and having large specific surface area and preparation method of hexaaluminate
  • Mesoporous hexaaluminate prepared by carbon template method and having large specific surface area and preparation method of hexaaluminate
  • Mesoporous hexaaluminate prepared by carbon template method and having large specific surface area and preparation method of hexaaluminate

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Embodiment 1

[0041] Preparation of mesoporous barium hexaaluminate: the mesoporous carbon prepared by 1.0g (the mesoporous carbon is prepared by the method in the document J.Am.Chem.Soc.2006,128,11652., the thickness of the pore wall of the obtained mesoporous carbon 6.0 nm, mesopore size 6.2 nm) immersed in 15 mL of nitric acid with a concentration of 5.0 mol / L, wherein the mass ratio of carbon material to solvent was 1:15, treated at 40 ° C for 3 h, filtered, washed and dried to obtain functionalized media porous carbon, and then highly dispersed it in 10mL of ethanol to obtain suspension A; weigh 4.5g of aluminum nitrate, 0.26g of barium nitrate and dissolve them in a mixture of 20mL of water and ethanol (the water / ethanol volume ratio is 1:3 ), the mass ratio of the salt precursor to the solvent is 1: 4.2, and the salt precursor solution B is obtained; then the solution B is added to A, and the resulting mixture is stirred at 20°C and evaporated to dryness to obtain the salt / charcoal C...

Embodiment 2

[0048] Preparation of mesoporous barium hexaaluminate: immerse 1.0 g of prepared mesoporous carbon (pore wall thickness 9.4 nm, mesopore size 7.0 nm) in 10 mL of hypochlorous acid solution with a concentration of 2.0 mol / L, wherein the carbon material and The mass ratio of the solvent is 1:10, treated at 40°C for 8 hours, filtered, washed and dried to obtain functionalized mesoporous carbon, and then highly dispersed in 10mL of ethanol to obtain suspension A; weigh 4.5g of aluminum nitrate , 0.25g barium acetate is dissolved in the mixed solution of 38mL water and acetone (water / acetone volume ratio is 3: 1), the mass ratio of salt precursor and solvent is 1: 8, makes salt precursor solution B; Then Add solution B to A, stir the resulting mixture at 40°C, and evaporate to dryness to obtain a salt / charcoal compound; put the salt / charcoal compound into a sand core funnel, place it in a 20mL container with a concentration of 6.0mol / In a hydrothermal kettle with L ammonium carbon...

Embodiment 3

[0053] Preparation of mesoporous barium hexaaluminate: Immerse 1.0 g of prepared mesoporous carbon (pore wall thickness 8.0 nm, mesopore size 6.5 nm) in 5 mL of 8.0 mol / L sulfuric acid, wherein the mass ratio of carbon material to solvent is 1:5, treated at 90°C for 5 hours, filtered, washed and dried to obtain functionalized mesoporous carbon, and then highly dispersed in 10mL ethanol to obtain suspension A; weigh 13.5g aluminum nitrate, 0.75g barium acetate Dissolve in the mixed solution of 28.5mL water and propanol (water / propanol volume ratio is 1: 1), the mass ratio of salt precursor and solvent is 1: 2, makes salt precursor solution B; Then solution B was added to A, and the resulting mixture was stirred at 50°C and evaporated to dryness to obtain a salt / charcoal composite; the salt / carbon composite was put into a funnel with a sand core, placed in a 20mL urea with a concentration of 2.0mol / L In the hydrothermal kettle of the aqueous solution, after standing at 110°C for...

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Abstract

The invention relates to the field of preparation of hexaaluminate materials, in particular to mesoporous hexaaluminate prepared by a carbon template method and having a large specific surface area and a preparation method of the hexaaluminate. The preparation method comprises the following steps of: 1) pretreating carbon materials, and dispersing the carbon materials into a solvent to obtain mesoporous carbon suspension; 2) dissolving an aluminum salt precursor and one or more of an alkaline-earth metal precursor, a rare-earth metal precursor and a transition metal precursor into the solvent to obtain a metal salt precursor solution; 3) adding the metal salt precursor solution into the mesoporous carbon suspension, stirring and drying by distillation to obtain a salt-carbon composite; 4) placing the salt-carbon composite in a labile nitrogen compound-containing aqueous solution, reacting, and washing, baking and roasting the obtained sample to obtain a hexaaluminate precursor-carbon composite; and 5) adding the hexaaluminate precursor-carbon composite into the metal salt precursor solution for impregnation, and finally performing thermal treatment and roasting to obtain the mesporous hexaaluminate having the large specific surface area.

Description

technical field [0001] The invention relates to the field of preparation of hexaaluminate materials. Specifically, the invention relates to a hexaaluminate with mesoporous high specific surface area prepared by a carbon template method and a preparation method thereof. Background technique [0002] Hexaaluminate is often used to catalyze the high-temperature combustion of methane, methane carbon dioxide reforming and N 2 O decomposition and other fields. Hexaaluminate available AAl 12 o 19 Indicates (A is alkali metal, alkaline earth metal or rare earth metal), which is a layered structure material in which the spinel formed by alumina is separated by the "mirror surface" composed of oxides of alkali metal or alkaline earth metal, and has a β-Al 2 o 3 Type or magnetoplumbite type structure, this special anisotropic layered structure endows hexaaluminate with outstanding high temperature thermal stability and thermal shock resistance, and can still maintain a high specifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/02B82Y40/00
Inventor 苏发兵古芳娜高加俭平原翟世辉
Owner 河北中芯凤华科技发展有限公司
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