Method used for preparing iron-doped SBA-15 mesoporous molecular sieve under neutral conditions via one-step method

A technology of mesoporous molecular sieves and neutral conditions, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc.

Inactive Publication Date: 2017-07-04
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the disadvantage that the acid-base medium in the synthesis process of mesoporous molecular sieves cannot adopt the one-step method to dope metals to obtain multifunctional composite materials.

Method used

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  • Method used for preparing iron-doped SBA-15 mesoporous molecular sieve under neutral conditions via one-step method
  • Method used for preparing iron-doped SBA-15 mesoporous molecular sieve under neutral conditions via one-step method
  • Method used for preparing iron-doped SBA-15 mesoporous molecular sieve under neutral conditions via one-step method

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Embodiment 1

[0023] This embodiment provides the preparation method of introducing Fenton's reagent to synthesize Fe-SBA-15 mesoporous molecular sieve in one step:

[0024] Get 4g tetraethyl orthosilicate and 15g deionized water and mix together and add in the quartz vessel, stir with a stirrer at 300 rpm, add Fenton's reagent (300uL of 1M FeSO 4 ·7H 2 O aqueous solution and 600 uL mass fraction of 35% H 2 o 2 Mixing of aqueous solutions, FeSO 4 ·7H 2 O and H 2 o 2 The quality of each is 0.08g and 0.02g), stirring continuously for 1 hour, it becomes orange-yellow homogeneous solution A, 2g P 123 Mix it with 85g deionized water and add it to the beaker, stir it with a stirrer at 300 rpm for 6 hours to make it a clear solution B, add solution B dropwise to solution A at 20mL / min to obtain Fe-SBA-15 mediated Porous molecular sieve initial sol, and then continue stirring at 40°C and 300 rpm for 24 hours, then transfer it to the reactor. The total mass ratio of each reactant in the react...

Embodiment 2

[0032] This embodiment provides the preparation method of introducing Fenton's reagent (reducing Fe content) one-step synthetic Fe-SBA-15 mesoporous molecular sieve:

[0033] Take 4g of tetraethyl orthosilicate and 15g of deionized water and mix them into a quartz vessel, stir with a mixer at 300 rpm, and add Fenton's reagent (200uL, 1M FeSO 4 ·7H 2 O and 600uL, mass fraction 35%H 2 o 2 Mixing of aqueous solutions, FeSO 4 ·7H 2 O and H 2 o 2 The quality of each is 0.06g and 0.02g), stirring continuously for 1 hour, it becomes orange-yellow homogeneous solution A, 2g P 123 Mix it with 45g deionized water and add it to the beaker, stir it with a stirrer at 300 rpm for 6 hours to make it a clear solution B, add solution B dropwise to solution A at 20mL / min to obtain Fe-SBA-15 medium Porous molecular sieve initial sol, then continue to stir at 40°C and 300 rpm for 24 hours, transfer it to the reactor, so that the total mass ratio of the reactants in the reactor is TEOS:P 1...

Embodiment 3

[0036] This embodiment introduces the preparation method of Fenton's reagent (increase Fe content) one-step synthesis Fe-SBA-15 mesoporous molecular sieve:

[0037] Take 4g of tetraethyl orthosilicate and 15g of deionized water and mix them into a quartz vessel, stir with a mixer at 300 rpm, and add Fenton's reagent (500uL, 1M FeSO 4 ·7H 2 O and 1800uL, mass fraction 35%H 2 o 2 Mixing of aqueous solutions, FeSO 4 ·7H 2 O and H 2 o 2 The quality of each is 0.14g and 0.06g), stirring continuously for 1 hour, it becomes orange-yellow homogeneous solution A, 2g P 123 Mix it with 85g deionized water and add it to the beaker, stir it with a stirrer at 300 rpm for 6 hours to make it a clear solution B, add solution B dropwise to solution A at 20mL / min to obtain Fe-SBA-15 medium Porous molecular sieve initial sol, then continue to stir at 40°C and 300 rpm for 24 hours, transfer it to the reactor, so that the total mass ratio of the reactants in the reactor is TEOS:P 123 : FeSO...

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Abstract

The invention discloses a method used for preparing iron-doped SBA-15 mesoporous molecular sieve under neutral conditions via one-step method, and belongs to the technical field of mesoporous molecular sieve synthesis. According to the method, Fenton reagent is added into an ethyl orthosilicate aqueous solution for hydrolysis, an obtained product is uniformly mixed with an organic template agent P123 aqueous solution, free radical reaction is induced by hydroxyl free radicals generated by Fenton reagent, the presence of a ferric salt is beneficial for realizing of charge matching effect and self-assembling between the organic template agent and an inorganic silicon source under neutral conditions, so that preparation of the Fe-SBA-15 mesoporous molecular sieve material is realized. According to the method, the Fe-SBA-15 mesoporous molecular sieve with excellent order degree is prepared via one-step method without adding inorganic strong acid, so that synthesis of metal-doped mesoporous materials under soda acidic or alkaline conditions or via complex post-treatment is avoided. The method is capable of providing industrialized production of iron-doped SBA-15 mesoporous molecular sieve with new ideas, providing widened industrialized applications of mesoporous molecular sieve materials with conditions, and possesses industrialized application value.

Description

technical field [0001] The invention belongs to the technical field of synthesis of SBA-15 mesoporous molecular sieves, and in particular relates to a method for preparing iron-doped SBA-15 mesoporous molecular sieves by adding Fenton's reagent in the next step under neutral conditions without adding acid and alkali. Background technique [0002] SBA-15 was synthesized by Professor Stucky of the University of California in 1998. This mesoporous silicon material with a hexagonal structure (P6mm) is widely used in industrial production due to its high specific surface area and good hydrothermal stability. . However, the traditional SBA-15 synthesis method needs to be synthesized under inorganic strong acidic conditions, which will not only cause certain harm to the environment, but also the pore wall of the synthesized SBA-15 material is amorphous SiO 2 , it is difficult to apply to catalytic reactions, only by doping metals into the pore walls or channels, and organically fu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03
CPCB01J29/0333B01J35/1061
Inventor 于吉红冯国栋王健羽
Owner JILIN UNIV
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