Preparation method of Fe-MCM-41 molecular sieve with high iron content

A technology of fe-mcm-41 and molecular sieve, which is applied in the field of preparation of MCM-41 molecular sieve, can solve the problem that the iron content needs to be improved, and achieve the effect of strong application value

Inactive Publication Date: 2011-10-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Iron content in molecular sieves still needs to be improved

Method used

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  • Preparation method of Fe-MCM-41 molecular sieve with high iron content
  • Preparation method of Fe-MCM-41 molecular sieve with high iron content
  • Preparation method of Fe-MCM-41 molecular sieve with high iron content

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Dissolve a certain amount of ferric nitrate and sodium tartrate (TA) in deionized water and stir for 40 minutes at room temperature, add organic template agent cetyltrimethylammonium bromide (CTAB), stir for 60 minutes, add ethyl orthosilicate dropwise After stirring for 60 min, the pH value was adjusted to 9 with NaOH solution. After continuous stirring for 2 h, the obtained emulsion was transferred into a polytetrafluoroethylene-lined reaction tank, and statically crystallized at 110° C. for 96 h. The molar composition ratio of reactants is CTAB:SiO 2 =0.2, Fe(NO 3 ) 3 : SiO 2 =0.15,H 2 O: SiO 2 =100, TA:SiO 2 = 0.3. After crystallization of the product, cool to room temperature, filter with suction, wash until the pH of the filtrate is 7, dry at 80°C, heat up to 550°C at a rate of 1°C / min, and keep warm for 6 hours to obtain the finished product. XRF characterizes that the finished product contains 11.75wt% Fe, N 2 The specific surface area of ​​the sample me...

Embodiment 2

[0019] Dissolve a certain amount of ferric nitrate and sodium tartrate (TA) in deionized water and stir for 40 minutes at room temperature, add organic template agent cetyltrimethylammonium bromide (CTAB), stir for 60 minutes, add ethyl orthosilicate dropwise After stirring for 60 min, the pH value was adjusted to 9 with NaOH solution. After continuous stirring for 2 h, the obtained emulsion was transferred into a polytetrafluoroethylene-lined reaction tank, and statically crystallized at 110° C. for 96 h. The molar composition ratio of reactants is CTAB:SiO 2 =0.2, Fe(NO 3 ) 3 : SiO 2 =0.1,H 2 O: SiO 2 =100, TA:SiO 2 = 0.2. After crystallization of the product, cool to room temperature, filter with suction, wash until the pH of the filtrate is 7, dry at 80°C, heat up to 550°C at a rate of 1°C / min, and keep warm for 6 hours to obtain the finished product. XRF characterizes that the finished product contains 7.34wt% Fe, N 2 The specific surface area of ​​the sample meas...

Embodiment 3

[0021] Dissolve a certain amount of ferric nitrate and sodium tartrate (TA) in deionized water and stir for 40 minutes at room temperature, add organic template agent cetyltrimethylammonium bromide (CTAB), stir for 50 minutes, add ethyl orthosilicate dropwise After stirring for 100 min, the pH value was adjusted to 9 with NaOH solution. After continuous stirring for 3 h, the resulting emulsion was transferred into a polytetrafluoroethylene-lined reaction tank and statically crystallized at 110° C. for 60 h. The molar composition ratio of reactants is CTAB:SiO 2 =0.2, Fe(NO 3 ) 3 : SiO 2 =0.15,H 2 O: SiO 2 =125, TA: SiO 2 = 0.3. After crystallization of the product, cool to room temperature, filter with suction, wash until the pH of the filtrate is 7, dry at 80°C, heat up to 550°C at a rate of 1°C / min, and keep warm for 6 hours to obtain the finished product. XRF characterizes that the finished product contains 11.26wt% Fe, N 2 The specific surface area of ​​the sample ...

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Abstract

The invention relates to a preparation method of a Fe-MCM-41 molecular sieve with high iron content. The preparation method comprises the following steps: through a hydrothermal synthesis method, based on sodium tartrate (TA) as a chelant of iron ions, cetyltrimethylammonium bromide (CTAB) as an organic template and tetraethoxysilane as a silicon source, stirring for 30-120 minutes, regulating the pH value to 7-11 with inorganic base, and then stirring for 2-6 hours, wherein the molar ratio of CTAB to SiO2 is 0.1-0.25, the molar ratio of TA to SiO2 is 0.05-0.6, and the molar ratio of H2O to SiO2 is 70-150; and then crystallizing for 48-120 hours under the self-boost pressure and hydrothermal conditions at the temperature of 90-130 DEG, cooling the purified product to room temperature, carrying out vacuum filtration, washing to be neutral, drying, continuously raising the temperature to 500-600 DEG C at the speed of 1 DEG C / min and insulating for 5 hours. By using the method, the iron ions can be directly introduced to a skeleton so as to prepare the mesoporous molecular sieve with the iron content of 7wt%-14wt%, the molecular sieve has a uniform aperture, the specific surface area of the molecular sieve is 700-1200 m<2> / g<-1>, and the pore volume of the molecular sieve is 0.7-3.0 cm<3> / g<-1>.

Description

1. Technical field [0001] The invention is a preparation method of MCM-41 molecular sieve with high iron content. 2. Background technology [0002] In 1992, Mobil Corporation of the United States synthesized the ordered mesoporous molecular sieve series M41S (pore diameter 1.6-10nm) with large specific surface area, regular hexagonal arrangement and adjustable mesoporous molecular sieves (Nature, 1992, 359: 710-712). With these remarkable features, it has broad application prospects in the fields of catalysis, adsorption, and materials. In order to improve its catalytic activity, it is necessary to introduce heteroatoms into the molecular sieve framework, when the trivalent heteroatom Fe is introduced into the silicon framework 3+ After that, it will cause the charge imbalance on the skeleton to produce protonic acid B acid, therefore, the trivalent heteroatom Fe introduced into the skeleton 3+ The amount affects the catalytic activity of the modified molecular sieve. Iro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B39/04C01B39/48B01J29/76
Inventor 李保山袁涛红
Owner BEIJING UNIV OF CHEM TECH
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