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Soft and hard double template method for preparing three-dimensional ordered macroporous iron oxide with mesoporous pore wall

A three-dimensional ordered, iron oxide technology, used in iron oxide, iron oxide/iron hydroxide, etc.

Inactive Publication Date: 2010-06-09
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, domestic and foreign literature and patents have not reported the preparation method of this kind of iron oxide with dual-mode pore structure.

Method used

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  • Soft and hard double template method for preparing three-dimensional ordered macroporous iron oxide with mesoporous pore wall
  • Soft and hard double template method for preparing three-dimensional ordered macroporous iron oxide with mesoporous pore wall
  • Soft and hard double template method for preparing three-dimensional ordered macroporous iron oxide with mesoporous pore wall

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: At normal temperature (25°C), normal pressure (1atm) and ultrasonic conditions (90HZ), 10mmolFe(NO 3 ) 3 9H 2 O was dissolved in 10 mL of absolute ethanol, and after being mixed evenly, it was added dropwise to a Buchner funnel equipped with 2 g of PMMA microspheres arranged in a close-packed arrangement. After the PMMA microspheres were completely infiltrated, suction filtration was performed to remove excess liquid, and then Dry at room temperature with a relative humidity lower than 50% for 12 hours, and finally put the obtained powder into a muffle furnace, raise the temperature from room temperature to 300°C at a rate of 1°C / min and keep the temperature constant for 3 hours, then rise to 650°C and keep the temperature constant After 3 hours, a disordered porous iron oxide with a rhombohedral crystal structure is obtained, with a pore diameter of 30-120 nm.

Embodiment 2

[0014] Example 2: At normal temperature (25°C), normal pressure (1atm) and ultrasonic conditions (90HZ), 25mmolFe(NO 3 ) 3 9H 2 O was dissolved in 10mL of anhydrous methanol and 15mL of anhydrous ethylene glycol (the volume ratio of methanol and ethylene glycol was 2:3), and after being mixed evenly, it was added dropwise to a Brookfield container equipped with 2 g of close-packed PMMA microspheres. In the funnel, after the PMMA microspheres are completely infiltrated, perform suction filtration to remove excess liquid, then dry at room temperature with a relative humidity below 50% for 12 hours, and finally put the obtained powder into a muffle furnace at 1°C / min The heating rate is raised from room temperature to 300°C and kept at a constant temperature for 3 hours, and then raised to 650°C and kept at a constant temperature for 3 hours to obtain macroporous iron oxide with a rhombohedral crystal structure and a certain degree of order, with a macropore diameter of 180-230n...

Embodiment 3

[0015] Example 3: At normal temperature (25°C), normal pressure (1atm) and ultrasonic conditions (90HZ), 1g P123 and 10mmol Fe(NO 3 ) 3 9H 2 O was dissolved in 10 mL of absolute ethanol, and after being mixed evenly, it was added dropwise to a Buchner funnel equipped with 2 g of PMMA microspheres arranged in a close-packed arrangement. After the PMMA microspheres were completely infiltrated, suction filtration was performed to remove excess liquid, and then Dry at room temperature with a relative humidity lower than 50% for 24 hours, and finally put the obtained powder into a muffle furnace, raise the temperature from room temperature to 300°C at a rate of 1°C / min and keep the temperature constant for 3 hours, then rise to 500°C and keep the temperature constant After 3 hours, three-dimensional ordered macroporous iron oxide with a rhombohedral crystal structure is obtained, the diameter of the macropores is 250-280 nm, and the diameter of the pore walls is 20-50 nm.

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Abstract

The invention relates to a soft and hard double template method for preparing three-dimensional ordered macroporous iron oxide with a mesoporous pore wall, belonging to the field of multi-phase catalysis. The method comprises the steps of: under the conditions of normal temperature, normal pressure and ultrasound, dissolving ferric nitrate nonahydrate and a soft template P123 into the mixed solution of absolute ethyl alcohol or absolute methanol and anhydrous ethylene glycol; soaking hard template PMMA microballoons which are arranged in a close packing way into the mixed solution; and finally, carrying out suction filtration by using the mixed solution containing the PMMA, drying and programming heating and calcining, and obtaining the hree-dimensional ordered macroporous iron oxide which has rhombohedral structure and the mesoporous pore wall. The iron oxide with macroporous and mesoporous double-mold pore channel structure has good application prospect in the fields such as multi-phase catalysis, absorption, pigment, etc.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis, and relates to a three-dimensional ordered macroporous Fe 2 o 3 The preparation method of , specifically involves the use of soft and hard dual templates to prepare three-dimensional ordered macroporous Fe with mesoporous pore walls 2 o 3 Methods. Background technique [0002] Iron oxide exhibits good redox performance due to its multiple variable valence states, and porous iron oxide is an effective adsorbent due to its high specific surface area. Therefore, porous iron oxide can be used as a catalyst or support for many reactions and as an adsorbent for certain gases. Studies have shown that the catalytic activity and adsorption performance of iron oxide in heterogeneous catalytic reactions are directly related to its synthesis route, microscopic morphology and other factors. [0003] The methods for synthesizing porous iron oxide mainly include sol-gel method, sonochemical method, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06
Inventor 戴洪兴张汝珍赵振璇孟雪何洪
Owner BEIJING UNIV OF TECH
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