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Double metaporous silicon dioxide material and its preparing method

A silica and double mesoporous technology, applied in the field of double mesoporous silica material and its preparation, can solve the problems of pore structure collapse and environmental pollution, and achieve the effect of concentrated pore distribution and wide pH value range

Inactive Publication Date: 2005-08-03
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the preparation method of the above-mentioned double mesoporous silicon material, the former uses two kinds of organosilicon compounds as the silicon source, and the latter uses mesitylene as the cosolvent, which is easy to pollute the environment, and both use the calcination method to remove the surfactant, which is easy to cause the pore structure the collapse of

Method used

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  • Double metaporous silicon dioxide material and its preparing method
  • Double metaporous silicon dioxide material and its preparing method
  • Double metaporous silicon dioxide material and its preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Mix 0.878g DDAC with 41g distilled water, ultrasonicate at 50°C for 2 hours to obtain a uniform and transparent surfactant solution, adjust the pH of the solution to 12.0 with NaOH, slowly add 2.0833g TEOS dropwise under stirring, stir at room temperature for 24 hours, and seal at 70°C Aged for 4 days, filtered, washed with distilled water, and dried to obtain a synthetic raw powder. The raw powder was refluxed in methanol / hydrochloric acid solution for 48 hours, washed with methanol, and dried to obtain a double mesoporous silica material. The characterization results are shown in the attached figure: figure 1 , figure 2 , image 3 (Other examples are similar to this), the small pore diameter of the material is 3.9nm, the large pore diameter is 11.6nm; the specific surface area is 718.2cm 2 / g; pore volume 1.46cm 3 / g.

Embodiment 2

[0021] Mix 0.3156g of DDAC with 41g of distilled water, ultrasonicate at 50°C for 2 hours to obtain a uniform and transparent surfactant solution, adjust the pH of the solution to 7.1, slowly add 2.0833g of TEOS dropwise under stirring, stir at room temperature for 24 hours, then seal and age at 80°C After 4 days, filter, wash with distilled water, and dry to obtain a synthetic raw powder, reflux the raw powder in methanol / hydrochloric acid solution for 48 hours, wash with methanol, and dry to obtain a double mesoporous silica material. The small pore diameter of the material is 3.6nm, the large pore diameter is 17.0nm; the specific surface area is 556.3cm 2 / g; pore volume 1.20cm 3 / g.

Embodiment 3

[0023] Mix 0.3156g DDAC with 41g distilled water, ultrasonicate at 50°C for 2 hours to obtain a uniform and transparent surfactant solution, adjust the pH of the solution to 10.9 with NaOH, slowly add 2.0833g TEOS dropwise under stirring, stir at room temperature for 24 hours, and seal at 70°C Aged for 4 days, filtered, washed with distilled water, and dried to obtain a synthetic raw powder. The raw powder was refluxed in methanol / hydrochloric acid solution for 48 hours, washed with methanol, and dried to obtain a double mesoporous silica material. The small pore diameter of the material is 3.2nm, the large pore diameter is 15.9nm; the specific surface area is 408.6cm 2 / g; pore volume 0.83cm 3 / g.

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Abstract

The double mesoporous silicon dioxide material has small pore diameter of 3.2-3.9 nm, great pore diameter of 9.4-24.5 nm, specific surface area of 408.6-718.2 sq cm / g, and pore volume of 0.53-1.8 cu cm / g. The material can meet the requirement of macromolecular shape selecting and diffusing effect on catalyst pore diameter distribution, and is one kind of latent industrial catalyst and catalyst carrier. The preparation process is one hydrolysis and condensation process with low solubility double alkyl chain quaternary ammonium salt as surfactant, dioctadecyl dimethyl ammonium chloride as template agent and ethyl silicate as silicon source and under wide pH value range and certain temperature. The preparation process is mild inreaction condition, simple and novel.

Description

1. Technical field [0001] The invention relates to a mesoporous silicon dioxide material, in particular to a double mesoporous silicon dioxide material and a preparation method thereof. 2. Background technology [0002] Using new synthetic routes to prepare materials with special properties and new structures is a hot spot in the field of materials at home and abroad. In 1992, Mobil researchers first used C n h 2n+1 Me 3 M41S series mesoporous molecular sieves were synthesized with Br(n>6) cationic surfactants as templates. Because of their high specific surface area, large pore volume, narrow pore distribution and adjustable pore , separation and new catalytic materials have potential industrial application prospects. At present, the pore diameters of mesoporous molecular sieves prepared at home and abroad mostly have a single-valued distribution, and the preparation of macromolecular catalytic cracking catalysts often requires a reasonable configuration of two-stage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/08C01B33/18C01B39/04
Inventor 秦晓琴李玉霞高春光赵永祥
Owner SHANXI UNIV
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