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Method for preparing iron-carrying ordered mesoporous carbon materials

A mesoporous carbon and iron-loaded technology, which is applied in the field of preparation of iron-loaded ordered mesoporous carbon materials, can solve the problems of complex preparation process and achieve the effects of simplified synthesis process, simple operation and low cost

Inactive Publication Date: 2009-11-18
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some progress has been made in the synthesis of ordered mesoporous carbon-supported metals (oxides) by soft template route, the existing methods all need to add a certain proportion of inorganic acid in the preparation process to catalyze the carbon source precursor. The polycondensation reaction of the body, the preparation process is still relatively complicated
In addition, due to the excellent magnetic properties and chemical activity of nano-metallic iron, it has important application value in the fields of catalysis, separation, and environmental pollution remediation. However, the synthesis of iron-loaded ordered mesoporous carbon has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The first step: at room temperature, select 0.303g of Fe(NO 3 ) 3 9H 2 O is dissolved in the water / ethanol mixed solution as the iron salt precursor, and the clear solution A obtained by magnetic stirring is stand-by, and then the resorcinol of the nonionic surfactant F127 of 2.5g and 1.65g is selected and dissolved in water / ethanol (volume Ratio 1 / 1) in the mixed solution, magnetic stirring obtains the solution B that is bright brown; The second step: the prepared dissolved 0.303gFe(NO 3 ) 3 9H 2 The water / ethanol mixed solution A of O is slowly added to the mixed solution B of F127 and resorcinol, stirred and mixed for 1 hour, and the solution obtained after the reaction is dark purple; the third step: add 2.5g of 37% formaldehyde solution to the above second In the mixed solution of the first step, continue to stir and mix for 3 hours to fully polymerize the phenolic resin, then stop stirring, and the mixed solution is gradually divided into upper and lower layer...

Embodiment 2

[0024] The reaction steps are exactly the same as in Example 1, except that the Fe(NO3) 9H2O of 0.606g is selected as the iron salt precursor; the stirring and mixing time of the mixed solution containing solution A and solution B in the second step is 3 After adding the formaldehyde solution, the stirring and mixing time was continued for 2 hours; the final two-phase mixture was left at room temperature for 72 hours, stirred for another 24 hours, and finally transferred to a 100°C oven for curing for 12 hours, and the product was placed in a nitrogen atmosphere at 800°C The hexagonal iron-loaded ordered mesoporous carbon material can be obtained by roasting for 2 hours, and the heating rate is 20-400° C. (1° C. / min) and 400-800° C. (5° C. / min). The obtained iron-loaded ordered mesoporous carbon material has a pore diameter of 3.9 nm, a pore volume of 0.41 cm3·g-1, and a specific surface area of ​​586 m2·g-1.

Embodiment 3

[0026]The reaction steps are exactly the same as in Example 1, except that 0.365g of FeCl is selected as the iron salt precursor; the second step: the prepared water / methanol mixed solution A with 0.365g of FeCl is slowly added to F127 and Resorcinol In the mixed solution B of phenol, the stirring and mixing time of the mixed solution containing solution A and solution B in the second step is 5 hours; the continuous stirring and mixing time after adding the formaldehyde solution is 2 hours; the final two-phase mixed solution is allowed to stand at room temperature 96 hours, then stirred for 10 hours, and finally transferred to 105°C oven for curing for 24 hours, then the product was calcined at 800°C for 3 hours under an argon atmosphere to obtain a hexagonal iron-loaded ordered mesoporous carbon material with a heating rate of 20- 500°C (1°C / min), 500-900°C (5°C / min). The obtained iron-loaded ordered mesoporous carbon material has a pore diameter of 3.9nm, a pore volume of 0....

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Abstract

The invention discloses a method for preparing novel iron-carrying ordered mesoporous carbon materials. Through a soft template route, under the condition of adding no acid additionally, acid produced by iron-salt precursor hydrolysis of a synthesis system is utilized to catalyze phenolic polycondensation, and iron-salt precursors and phenolic polycondensation products are self-assembled around surfactant and are carbonized in inert atmosphere so as to prepare the iron-carrying ordered mesoporous carbon materials. The obtained iron-carrying ordered mesoporous carbon materials are ordered in height, high in specific surface area (410-586m2 . g-1) and uniform in pore size distribution (3.9 nm). The method realizes the one-step synthesis of the iron-carrying ordered mesoporous carbon materials. Compared with mesoporous carbon synthesis through a hard template route and an impregnating-loading process, the method has the advantages of easy operation, low cost, low requirements for equipment, and the like. The iron-carrying ordered mesoporous carbon materials prepared by the method have wide application prospects in the fields of catalysis, separation, electrode materials, repair to environmental pollutants, and the like.

Description

technical field [0001] The invention relates to a method for preparing an ordered mesoporous material, in particular to a method for preparing an iron-loaded ordered mesoporous carbon material. Background technique [0002] Due to its regular channels, large specific surface area, uniform pore size and high stability, ordered mesoporous carbon materials have important application value in many high-tech fields, such as fuel cells, catalyst supports, sensors, and membrane separation. In order to further expand the application range of ordered mesoporous carbon, the study of loading metal (oxide) nanocrystals in mesoporous carbon matrix to form mesoporous carbon matrix composites has attracted great attention of researchers. Mesoporous carbon-based composites show many remarkable properties due to the regular channels of mesoporous carbon and the unique properties of supported metal (oxide) nanocrystals. For example, after loading Pt in the ordered mesoporous carbon matrix, it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 李健生王连军顾娟李慧君申战辉孙秀云韩卫清刘晓东
Owner NANJING UNIV OF SCI & TECH
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