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Method for synthesizing highly ordered super-microporous silicon dioxide

A silica and highly ordered technology, which is applied in the field of synthetic ultra-microporous silica, can solve the problems of low commercialization of template agents, unsuitability for large-scale production and application, and difficulty in purchasing, etc., achieving low cost, The effect of high order and low cost

Inactive Publication Date: 2013-04-24
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of the above method for synthesizing ultra-microporous molecular sieves is that the template agent is not commercially available, is not easy to buy, and is not suitable for large-scale production and application.

Method used

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  • Method for synthesizing highly ordered super-microporous silicon dioxide
  • Method for synthesizing highly ordered super-microporous silicon dioxide
  • Method for synthesizing highly ordered super-microporous silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At room temperature, dissolve 1.12g of dedecyltrimethylammonium bromide and 0.136g of sodium octyl sulfate in 30ml of water, stir for 0.5h to obtain solution A, and take another 1.72g of Na 2 SiO 3 9H 2 Dissolve O in 30ml of water to obtain solution B; quickly mix solutions A and B, and add 2 mol / L sulfuric acid solution drop by drop to the above mixture under vigorous stirring until the pH is between 9-10; then at 80°C Constant temperature in the oven for 70-75 hours, the obtained solid precipitate is filtered, washed and dried in the air to obtain a composite product; the composite product is heated to 530-560°C in the air at a speed of 1.5°C / min, The product was obtained at constant temperature for 3-5 hours. XRD spectrum as figure 2 . Diffraction peaks appear around 2θ of 3, but the peaks are too broad to be indexed. The unit cell parameter a=3.13nm was calculated according to the d value on XRD. N 2 The BET surface area measured by adsorption-desorption met...

Embodiment 2

[0025] At room temperature, dissolve 1.12g of dedecyltrimethylammonium bromide and 0.180g of sodium octyl sulfate in 30ml of water, stir for 0.5h to obtain solution A, and take another 1.72g of Na 2 SiO 3 9H 2 Dissolve O in 30ml of water to obtain solution B; quickly mix solutions A and B, and add 2 mol / L sulfuric acid solution drop by drop to the above mixture under vigorous stirring until the pH is between 9-10; then at 80°C Constant temperature in the oven for 70-75 hours, the obtained solid precipitate is filtered, washed and dried in the air to obtain a composite product; the composite product is heated to 530-560°C in the air at a speed of 1.5°C / min, The product was obtained at constant temperature for 3-5 hours. XRD spectrum as image 3 . There are three obvious diffraction peaks in the figure, and the position index of the diffraction peak 2θ is confirmed as a two-dimensional hexagonal structure (2D-P6mm), and the three diffraction peaks correspond to the (100) (11...

Embodiment 3

[0027] At room temperature, dissolve 1.12g of dedecyltrimethylammonium bromide and 0.278g of sodium octyl sulfate in 30ml of water, stir for 0.5h to obtain solution A, and take another 1.72g of Na 2 SiO 3 9H 2 Dissolve O in 30ml of water to obtain solution B; quickly mix solutions A and B, and add 2 mol / L sulfuric acid solution drop by drop to the above mixture under vigorous stirring until the pH is between 9-10; then at 80°C Constant temperature in the oven for 70-75 hours, the obtained solid precipitate is filtered, washed and dried in the air to obtain a composite product; the composite product is heated to 530-560°C in the air at a speed of 1.5°C / min, The product was obtained at constant temperature for 3-5 hours. XRD spectrum as Figure 4. There are three obvious diffraction peaks in the figure, and the position index of the diffraction peak 2θ is confirmed as a two-dimensional hexagonal structure (2D-P6mm), and the three diffraction peaks correspond to the (100) (11...

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Abstract

The invention relates to a method for synthesizing highly ordered super-microporous silicon dioxide. The method includes steps: firstly, mixing decyltrimethylammonium bromide, sodium octyl sulfate, sodium silicate and water according to the molar ratio of 1:0.1-0.4:1.5:800, and stirring for 0.5 hour at room temperature; secondly, adjusting hydrogen ion concentration (PH) to range from 9 to 10 by using sulfuric acid solution with concentration of 2mol / L; and thirdly, heating the mixed liquor for 72 hours by using water with temperature of 80 DEG C, filtering, washing, drying in air, and roasting at temperature between 530 DEG C and 560 DEG C to obtain the product. The sodium silicate used in the method uses the decyltrimethylammonium bromide as a short chain positive ion surface active agent and the sodium octyl sulfate as a short chain negative ion surface active agent. The method is low in cost, temperate in reacting condition and high in order of product pore channels, and is a novel method provided for future large-scale development and utilization of the highly ordered super-microporous silicon dioxide.

Description

technical field [0001] The invention belongs to the fields of inorganic chemistry, physical chemistry, material science and catalytic chemistry, and in particular relates to a method for synthesizing ultramicroporous silicon dioxide. Background technique [0002] Supermicroporous molecular sieve refers to a porous material whose pore size is between micropores (pore size <1.0nm) and mesoporous (pore size greater than 2nm and less than 50nm). As an important "bridge" between microporous and mesoporous materials, ultramicroporous materials are of great significance in shape-selective catalysis and selective adsorption. The pore size of microporous materials is small, such as organic macromolecules and pharmaceutical intermediates, etc. are difficult to enter, while the M41s series of mesoporous molecular sieves, with a pore size above 2.0nm, is difficult to show an ideal choice for catalytic objects with a kinetic size smaller than 2.0nm Catalysis, the synthesis of ultra-m...

Claims

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Application Information

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IPC IPC(8): C01B33/18
Inventor 朱延美王仁亮陈红余冀海伟葛海燕李莉
Owner TAISHAN MEDICAL UNIV
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