Preparation method of silicon dioxide molecular sieve

A silicon dioxide and molecular sieve technology, applied in molecular sieve compounds, chemical instruments and methods, molecular sieves and alkali exchange compounds, etc., can solve the problems of unsatisfactory monodispersity of mesoporous microspheres, low industrial added value, and large environmental pressure. , to achieve the effect of obvious adsorption selectivity, high specific surface area and strong adsorption capacity

Active Publication Date: 2014-01-29
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

However, this mesoporous material has not been widely used at present, mainly because of the following problems: In order to obtain mesoporous silica molecular sieves with specific shapes, it is necessary to conduct complex and precise self-assembly systems and synthesis processes during the synthesis process. control, and requires the use of more expensive surfactants; the particle size of spherical silica mesoporous molecular sieves prepared by traditional synthesis methods is small (typical particle size range is 0.2-1 μm), which cannot meet the requirements of some fields For example, the requirement for the stationary phase in HPLC is that the particle size is not less than 5 μm, so as to ensure that it is not easy to block during use and reduce the energy consumption of fluid flow. Although non-ionic surfactants can be used to synthesize

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  • Preparation method of silicon dioxide molecular sieve

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Effect test

Embodiment approach 1

[0025] Implementation mode one: if figure 1 Shown, the preparation method of this embodiment is:

[0026] (1) Heat-treat micro-silicon powder at 500°C for 5 hours in an air atmosphere to remove C and other volatile impurities, and obtain silica powder with a particle size of 30-100nm. 95wt%, carry out acid leaching treatment (acid leaching treatment uses hydrochloric acid with a concentration of 4mol / L, the liquid-solid ratio is 10:1ml / g, and the treatment lasts for 100 minutes), and after filtering, it is cleaned. 2 The content is 97.9%;

[0027] (2) Combine the microsilica fume after acid leaching in step (1) with NaOH, structure directing agent and H 2 O according to SiO 2 : NaOH: structure directing agent: H 2 O molar ratio 1 : 0.2 : 0.1 : 200 mixed, under the condition of 90 ℃, reaction (pseudomorphic transformation) for 48 hours, then washed, filtered and dried to obtain the organic-inorganic composite intermediate product; asfigure 1 The establishment of the self-as...

Embodiment approach 2

[0029] Implementation mode two: if figure 1 Shown, the preparation method of this embodiment is:

[0030] (1) Carry out acid leaching treatment on microsilica powder (silica powder with a particle size of 200-300nm and a purity of 98wt%) (acid leaching treatment uses sulfuric acid with a concentration of 7mol / L, and the liquid-solid ratio is 50:1ml / g, treated for 90 minutes), filtered and cleaned, at this time the SiO in the silica fume 2 The maximum content is about 95.6%;

[0031] (2) Combine the microsilica fume after acid leaching in step (1) with NaOH, structure directing agent and H 2 O as SiO 2 : NaOH: structure directing agent: H 2 O molar ratio 1 : 0.4 : 0.2 : 150 mixed, under the condition of 100 ℃, reaction (pseudomorphic transformation) for 12 hours, then washed, filtered and dried to obtain the organic-inorganic composite intermediate product; as figure 1 The establishment of the self-assembled system is shown. The structure directing agent includes cationi...

Embodiment approach 3

[0034] Implementation mode three: if figure 1 Shown, the preparation method of this embodiment is:

[0035] (1) Carry out acid leaching treatment (acid leaching treatment is a mixture of hydrochloric acid and sulfuric acid with a concentration of 6mol / L in any proportion, liquid-solid Ratio of 30:1ml / g, treatment for 120 minutes), filtered and cleaned, at this time SiO in silica fume 2 The content is 98.3%;

[0036] (2) Combine the microsilica fume after acid leaching in step (1) with NaOH, structure directing agent and H 2 O as SiO 2 : NaOH: structure directing agent: H 2 O molar ratio 1 : 0.3 : 0.3 : 180 mixed, under the condition of 120 ℃, reaction (pseudomorphic transformation) for 30 hours, then washed, filtered and dried to obtain the organic-inorganic composite intermediate product; as figure 1 The establishment of the self-assembled system is shown. The structure directing agent includes cationic surfactant and nonionic surfactant, and the quality of cationic sur...

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Abstract

The invention relates to a preparation method of a silicon dioxide molecular sieve, and belongs to the technical field of porous material preparation. The preparation method comprises the following steps: carrying out thermal treatment on silica fume, then carrying out particle classification and acid leaching treatment, filtering and cleaning; mixing the silica fume subjected to the acid leaching treatment, NaOH, a structure-directing agent and H2O in a molar ratio of SiO2 to NaOH to the structure-directing agent to H2O being 1: (0.2-0.4): (0.1-0.3): (150-200), reacting for 12-48 hours at the temperature of 90-120 DEG C, washing, filtering and drying, thus obtaining an organic-inorganic composite intermediate product; mixing the organic-inorganic composite intermediate product and water in a mass ratio being 1: (30-50), stirring, carrying out hydro-thermal treatment, washing, filtering and drying an obtained solid matter, then baking the obtained solid matter, and removing the structure-directing agent, thus obtaining the spherical mesoporous silicon dioxide molecular sieve. The preparation method has the advantages that the synthetic process and condition of the spherical mesoporous silicon dioxide molecular sieve are greatly simplified, the synthetic cost is reduced, and the prepared mesoporous material has excellent heavy metal adsorption property.

Description

technical field [0001] The invention relates to a preparation method of silica molecular sieve, which belongs to the technical field of porous material preparation. Background technique [0002] Since the scientists of Mobile Company successfully synthesized the M41S series ordered mesoporous silica material in 1992, due to its unique nano-scale ordered pores, high specific surface area and easy-to-modify surface properties, it was born in the field of nanomaterials and molecular sieves. Due to its strong adsorption capacity and large adsorption capacity, MCM-41 has high application value in the field of adsorption treatment of heavy metal ions in wastewater (such as Hg, Ag, Cr, Pb, Ba and Zn, etc.), after self-assembling 3-mercaptopropyltrimethoxysilane on the surface of mesoporous material MCM-41, it has a good adsorption effect on heavy metal ions in water. Shi Jianlin, a researcher at the Shanghai Institute of Ceramics, Chinese Academy of Sciences, found that the mesopo...

Claims

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Application Information

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IPC IPC(8): C01B39/00C01B37/00B01J20/10B01J20/30
Inventor 马文会朱文杰魏奎先李明明周阳于洁谢克强伍继君秦博吕国强
Owner KUNMING UNIV OF SCI & TECH
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