Method for preparing iron modified SBA-15 mesoporous molecular sieve

A mesoporous molecular sieve and modification technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of long preparation cycle, high cost, and short preparation cycle, and achieve the goal of improving mass transfer rate, increasing surface area, and improving degradation performance Effect

Inactive Publication Date: 2010-09-22
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the preparation method of iron-modified SBA-15 mesoporous molecular sieve in the prior art, there are defects that the preparation period is too long and the cost is high. SBA-15 Mesoporous Molecular Sieve Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 3.6g triblock copolymer P123 and 0.1834g ferric nitrate nonahydrate in 10mL hydrochloric acid (2mol / L) and 100mL deionized water to prepare a solution (pH≈1), wherein P123: Fe(NO 3 ) 3 ·9H 2 O:HCl:H 2 The molar ratio of O is 0.0155:0.011:2.2:156, and the solution is magnetically stirred at room temperature until the solution is clear and transparent; 9 mL of ethyl orthosilicate is added (the molar ratio of ethyl orthosilicate and triblock copolymer is 1.0:0.0155) , continue stirring for 15min, then the mixed solution is placed in the ultrasonic tank of the KQ-300B model ultrasonic instrument, and the working frequency is an ultrasonic wave of 40KHz for one hour; the volume ratio of concentrated ammonia water and deionized water is 1: 3 ammonia solution, The pH of the reaction solution was adjusted to ≈ 3, and the ultrasonic wave was continued for 1 hour, then transferred to the reaction kettle and hydrothermally heated at 100 °C for 24 hours. The components i...

Embodiment 2

[0020] 3.6g triblock copolymer P123 and 0.1664g ferric nitrate nonahydrate were dissolved in 10mL hydrochloric acid (2mol / L) and 100mL deionized water to prepare a solution (pH≈1), wherein P123: Fe(NO 3 ) 3 ·9H 2 O:HCl:H 2 The molar ratio of O is 0.0155:0.010:2.2:156, and magnetic stirring at room temperature until the solution is clear and transparent; add 9 mL of ethyl orthosilicate (the molar ratio of ethyl orthosilicate and triblock copolymer is 1.0:0.0155 ), stirring continuously for 15min, then the mixed solution is placed in the ultrasonic tank of the KQ-300B model ultrasonic instrument, and the working frequency is the ultrasonic wave of 40KHz to act for one hour; with concentrated ammonia water and deionized water volume ratio is 1: 3 aqueous ammonia solution , adjust the pH of the reaction solution ≈ 3, continue the ultrasonic action for one hour, and then transfer to the reaction kettle, hydrothermally under the condition of 100 ° C for 24 hours, the components in...

Embodiment 3

[0022] 3.6g triblock copolymer P123 and 0.2065g ferric nitrate nonahydrate were dissolved in 10mL hydrochloric acid (2mol / L) and 100mL deionized water to prepare a solution (pH≈1), wherein P123: Fe(NO 3 ) 3 ·9H 2 O:HCl:H 2 The molar ratio of O is 0.0155: 0.013: 2.2: 156, and magnetic stirring at room temperature until the solution is clear and transparent; add 9 mL of ethyl orthosilicate (the molar ratio of ethyl orthosilicate and triblock copolymer is 1.0: 0.0155 ), stirring continuously for 15min, then the mixed solution is placed in the ultrasonic tank of the KQ-300B model ultrasonic instrument, and the working frequency is the ultrasonic wave of 40KHz to act for one hour; with concentrated ammonia water and deionized water volume ratio is 1: 3 aqueous ammonia solution , adjust the pH of the reaction solution ≈ 3, continue the ultrasonic action for 1 hour, then transfer to the reaction kettle, and hydrothermally under the condition of 100 ℃ for 24 hours, the components in...

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Abstract

The invention relates to a method for preparing an iron modified SBA-15 mesoporous molecular sieve, which comprises the following steps of: 1) adding nonionic surfactant and ferric nitrate nonahydrate into solution prepared from hydrochloric acid and deionized water in a volume ratio of 1 to 10 with pH of about 1, and stirring the solution at the room temperature till the solution is clear and transparent; 2) adding tetraethoxysilane into the mixed solution obtained in the step 1), placing the mixed solution into an ultrasonic pool, acting ultrasonic wave on the mixed solution for 2 hours, adjusting the pH of the mixed solution to between 3 and 4, transferring the mixed solution to a reaction kettle, and hydro-thermally crystallizing the mixed solution for 24 hours at the temperature of 100 DEG C to form the iron modified SBA-15 mesoporous molecular sieve; and 3) filtering the reaction solution obtained in the step 2), repeatedly washing a filtered substance by using water and drying the filtered substance, and calcining the filtered substance for 6 hours at the temperature of 550 DEG C to obtain the SBA-15 mesoporous molecular sieve of which iron ions are high dispersed inside and outside a skeleton. The method reduces the reactive ageing time to 2 hours from 20 hours, does not need to use a mineralizing agent NH4F, greatly shortens the reaction period, and reduces the reaction cost.

Description

technical field [0001] The invention belongs to the field of molecular sieve inorganic materials, in particular to a preparation method of iron-modified SBA-15 mesoporous molecular sieve. Background technique [0002] Mesoporous molecular sieve SBA-15 is the most promising support catalyst due to its large pore size, high surface area and good hydrothermal stability. Iron-modified SBA-15 is used as a heterogeneous catalyst to form a non-Fenton reagent with hydrogen peroxide. Degradation of toxic organic substances shows potential application prospects. However, the preparation process of iron-modified SBA-15 mesoporous materials, the dispersion performance of iron ions on the carrier, and the existence state of iron ions directly affect their catalytic degradation performance. In Li Ying's doctoral dissertation: Synthesis, characterization and catalytic performance of Al-SBA-15 and Fe-SBA-15 mesoporous materials, a preparation method of iron-modified SBA-15 mesoporous molec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 谢焕玲全学军张三港
Owner CHONGQING UNIV OF TECH
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