Multilayer vesicular mesoporous silicon dioxide with adjustable number of layers and synthetic method thereof

A technology of mesoporous silica and multi-layer vesicles, applied in the directions of silica, silica, pharmaceutical formulations, etc., can solve the problem of uneven particle size distribution, and achieve the effect of mild reaction conditions

Active Publication Date: 2015-06-17
山东济清科技服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The vesicular mesoporous silica prepared in this patent is a single layer with uneven particle size distribution

Method used

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  • Multilayer vesicular mesoporous silicon dioxide with adjustable number of layers and synthetic method thereof
  • Multilayer vesicular mesoporous silicon dioxide with adjustable number of layers and synthetic method thereof
  • Multilayer vesicular mesoporous silicon dioxide with adjustable number of layers and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put a 100mL beaker on a magnetic stirrer, add 35mL distilled water and heat up to 30°C, add 0.142g CTAB to the distilled water under stirring, stir to form a transparent solution, add DDAB with a molar ratio of 1:0.625 to CTAB, and stir After completely dissolving, add 0.69ml of ammonia water, take 2.0g of TEOS and slowly drop into the solution under stirring after 2h, seal and stir for 24h at constant temperature. The obtained white precipitate solution was transferred to a 50ml reaction kettle, and placed in a thermostat at 100°C for 24 hours. After cooling, the white precipitate solution was filtered, and the obtained precipitate was repeatedly filtered and washed with distilled water. The obtained precipitate was dried at 50° C. for 12 hours, and then the precipitate was calcined in a tubular calciner at 550° C. for 6 hours to obtain vesicular mesoporous silica with 7 layers.

Embodiment 2

[0029] Put a 100mL beaker on a magnetic stirrer, add 35mL distilled water and heat up to 30°C, add 0.142g CTAB to the distilled water under stirring, stir to form a transparent solution, add DDAB with a molar ratio of 1:0.823 to CTAB, and stir After completely dissolving, add 0.69ml of ammonia water, take 2.0g of TEOS and slowly drop into the solution under stirring after 2h, seal and stir for 24h at constant temperature. The obtained white precipitate solution was transferred to a 50ml reaction kettle, and placed in a thermostat at 100°C for 24 hours. After cooling, the white precipitate solution was filtered, and the obtained precipitate was repeatedly filtered and washed with distilled water. The obtained precipitate was dried at 50° C. for 12 hours, and then calcined in a tubular calciner at 550° C. for 6 hours to obtain vesicular mesoporous silica with 4 layers.

Embodiment 3

[0031] Put a 100mL beaker on a magnetic stirrer, add 35mL distilled water and heat up to 30°C, add 0.142g CTAB to the distilled water under stirring, stir to form a transparent solution, add DDAB with a molar ratio of 1:1.104 to CTAB, and stir After completely dissolving, add 0.69ml of ammonia water, take 2.0g of TEOS and slowly drop into the solution under stirring after 2h, seal and stir for 24h at constant temperature. The obtained white precipitate solution was transferred to a 50ml reaction kettle, and placed in a thermostat at 100°C for 24 hours. After cooling, the white precipitate solution was filtered, and the obtained precipitate was repeatedly filtered and washed with distilled water. The obtained precipitate was dried at 50°C for 12 hours, and then the precipitate was calcined in a tubular calciner at 550°C for 6 hours to obtain vesicular mesoporous silica with 2-3 layers.

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Abstract

The invention relates to multilayer vesicular mesoporous silicon dioxide with an adjustable number of layers and a synthetic method thereof. The synthetic method comprises the following steps: adding CTAB (Cetyltrimethyl Ammonium Bromide) into distilled water at 25-30 DEG C, stirring till CTAB is dissolved; and then adding DDAB (Dimethyl Dioctadecyl Ammonium Bromide), stirring till DDAB is completely dissolved; dropwise adding a small amount of ammonium water into the stirred solution, uniformly stirring; then dropwise adding tetraethyl orthosilicate TEOS while stirring to obtain a suspension; continuously stirring the obtained suspension to react for 20-24 hours to obtain a white precipitate, and placing the white precipitate in an incubator and standing for 20-24 hours at 100-120 DEG C; and carrying out suction filtration, washing, drying and grinding on the white precipitate, and calcining for 5-6 hours under a condition of 500-600 DEG C to obtain vesicular mesoporous silicon dioxide. The prepared vesicular mesoporous silicon dioxide has uniform granularity (60-120nm) and good dispersibility, the number of layers of the vesicular mesoporous silicon dioxide can be regulated by 7-2 layers by changing the addition of DDAB.

Description

technical field [0001] The invention relates to multilayer vesicular mesoporous silica with adjustable layers and a preparation method thereof, belonging to the technical field of material synthesis. Background technique [0002] Mesoporous materials are widely used in biocatalysis, chemical adsorption, controlled drug release, sensors and color separation. Therefore, the synthesis and application of mesoporous materials have become one of the research hotspots since the researchers of Mobil Corporation in the United States used quaternary ammonium salt cationic surfactants as templates to synthesize the M4IS series of mesoporous materials in 1992. Aggregates (such as micelles, vesicles, liquid crystals, etc.) formed by surfactant molecules are used as templates, and orderly molecules with different morphologies can be synthesized through condensation, assembly, and shaping of precursors, and removal of templates by calcination or organic solvents. Mesoporous materials, suc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18A61K47/04B82Y40/00
Inventor 周国伟张彦李艳敬刘方方
Owner 山东济清科技服务有限公司
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