Process for synthesizing mesic-porous molecular sieve SBA15

A technology of mesoporous molecular sieve and synthesis method, which is applied in the field of synthesis of mesoporous molecular sieve SBA-15, can solve the problems of dangerous synthesis process, long synthesis time, environmental pollution, etc., and achieve reduction of pollution and synthesis cost, reduction of dosage and synthesis conditions mild effect

Inactive Publication Date: 2006-01-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] But, so far, all SBA-15 synthesis processes are carried out (Science, 1998,279,548) in strong liquid acid (such as concentrated hydrochloric acid, pH value is less than 1) medium, synthetic every gram of SBA-15 consumes Concentrated hydrochloric acid (36wt%) 10-11 gram, this not only causes synthesis process very dangerous, corrosivity is serious, also can generate a large amount of environmental pollutants in aftertreatment processes such as drying, roasting; And synthetic time is long (crystallization time is in more than 24 hours)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 4 grams of template agent P123 were added to 110 grams of deionized water, stirred at room temperature for 3 hours, and then 0.65 grams of phosphomolybdic acid (H 3 PO 4 12MoO 3 24 hours 2 0), and continue to stir until P123 and phosphomolybdic acid are completely dissolved, then add 8.55 grams of ethyl orthosilicate and 0.68 gram of sodium chloride in the above solution, then, it is put into 40 ℃ of water baths and hydrolyzed for 20 hours , Next, the hydrolyzed product was transferred to a polytetrafluoroethylene hydrothermal reaction kettle, and stood at 96°C for crystallization for 24 hours. After that, the crystallized product was filtered and washed with a large amount of deionized water. The collected solid was dried at 45° C. for 48 h, and finally, the temperature was slowly raised to 550° C. under an air atmosphere, and calcined at this temperature for 8 hours. After characterization, it is known that the material is mesoporous SBA-15 with two-dimensional hex...

Embodiment 2

[0027] 4 grams of template agent P123 were added to 110 grams of deionized water, stirred at room temperature for 3 hours, and then 0.65 grams of phosphomolybdic acid (H 3 PO 4 12MoO 3 24 hours 2 0), and continue to stir until P123 and phosphomolybdic acid are completely dissolved, then add 8.55 grams of ethyl orthosilicate and 0.62 gram of sodium bromide in the above solution, then, it is put into 40 ℃ of water baths and hydrolyzed for 20 hours , Next, the hydrolyzed product was transferred to a polytetrafluoroethylene hydrothermal reaction kettle, and stood at 96° C. for 6 hours for crystallization, after which, the crystallized product was filtered and washed with a large amount of deionized water. The collected solid was dried at 45° C. for 48 h, and finally, the temperature was slowly raised to 550° C. under an air atmosphere, and calcined at this temperature for 8 hours. After characterization, it is known that the material is mesoporous SBA-15 with two-dimensional he...

Embodiment 3

[0029] 4 grams of template agent P123 were added to 110 grams of deionized water, stirred at room temperature for 3 hours, and then 0.65 grams of phosphomolybdic acid (H 3 PO 4 12MoO 3 24 hours 2O), and continue to stir until P123 and phosphomolybdic acid are completely dissolved, then add 8.55 grams of methyl orthosilicate or ethyl orthosilicate and 0.66 gram of potassium iodide to the above solution, and then put it into a water bath at 40°C Hydrolyze for 20 hours. Next, transfer the hydrolyzed product to a polytetrafluoroethylene hydrothermal reaction kettle and stand at 96°C for crystallization for 6 hours. Afterwards, filter the crystallized product and wash it with a large amount of deionized water. washing. The collected solid was dried at 45° C. for 48 h, and finally, the temperature was slowly raised to 550° C. under an air atmosphere, and calcined at this temperature for 8 hours. After characterization, it is known that the material is mesoporous SBA-15 with two-...

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Abstract

A process for synthesizing the meso-porous molecular sieve SBA-15 features that the tri-block copolymer 'polyepoxyethene-polyepoxypropane-polyepoxyethene' is used as template, the non-fluorine anionic salt as inducing agent, and the heteropoly acid as promoter and acidity regulator. Its advantages are short time and low environmental pollution and cost.

Description

technical field [0001] The invention relates to a method for synthesizing environment-friendly and high-efficiency mesoporous molecular sieve SBA-15, belonging to inorganic nanomaterials [0002] technology field. Background technique [0003] Mesoporous materials synthesized by surfactant as a template can be used in macromolecule conversion, catalysis, as a catalyst carrier, separation and purification of biomacromolecules, as a template for the preparation of carbon nanotubes and other nano-metals or oxides, and in the microstructure of electronic devices. Chemicals and chromatographic fillers have broad application prospects. [0004] Since 1992, scholars at home and abroad have synthesized many types of mesoporous molecular sieves (MCM, SBA, MSU, etc.) using different templates. However, MCM-41 and SBA-15 are the most frequently occurring words in domestic and foreign literatures, so it can be seen that these two mesoporous molecular sieves are the most representative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 罗永明侯昭胤金顶峰郑小明
Owner ZHEJIANG UNIV
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