Ordered organic-inorganic hybrid mesoporous silica and loaded gold nanomaterials, and preparing method thereof

A mesoporous silica, organic technology, applied in the field of preparation of gold nanoparticles and its preparation, can solve the problems of uneven distribution of organic functional groups, difficulty in controlling the size distribution of gold particles, etc., and achieve environmental protection and good catalytic applications Foreground, reaction process simple effect

Active Publication Date: 2009-11-04
CHINA TOBACCO HUNAN INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation process is simple, but the size and distribution of gold particles in the channels are difficult to control due to the uneven distribution of organic functional groups in the carrier.

Method used

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  • Ordered organic-inorganic hybrid mesoporous silica and loaded gold nanomaterials, and preparing method thereof
  • Ordered organic-inorganic hybrid mesoporous silica and loaded gold nanomaterials, and preparing method thereof
  • Ordered organic-inorganic hybrid mesoporous silica and loaded gold nanomaterials, and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Dissolve 5ml of 6-mercapto-1-hexanol in 20ml of absolute ethanol with stirring at room temperature, then add 13.8g of iodine, and stir for 24 hours. After the solvent was removed by rotary evaporation, 30 ml of tert-butyl methyl ether was added, and then the iodine was extracted with 10 mg / ml sodium bisulfite solution, and the solvent was removed by rotary evaporation. Add 5 ml of thionyl chloride to the residue, stir at room temperature for 24 hours, and remove volatile substances by rotary evaporation. Finally, 5 ml of 3-ethoxysilylpropyl-4,5-dihydroimidazolium ionic liquid was added to the residue under N 2 Heating to reflux under protection for 24 hours, removing volatile matter in a vacuum to obtain a viscous liquid, that is, an imidazole-based ionic liquid organofunctional siloxane precursor containing thioether.

[0039] 2. Keep the temperature at 35°C, dissolve 4.0g P123 in 150ml 1.6M (M is mol / l) hydrochloric acid solution to make the pH of the solution rea...

Embodiment 2

[0042] 1. Dissolve 5ml of 9-mercapto-1-nonanol in 20ml of absolute ethanol with stirring at room temperature, then add 13.8g of iodine, and stir for 24 hours. After the solvent was removed by rotary evaporation, 30 ml of tert-butyl methyl ether was added, and then iodine was extracted with 15 mg / ml sodium bisulfite solution, and the solvent was removed by rotary evaporation. Add 5 ml of thionyl chloride to the residue, stir at room temperature for 24 hours, and remove volatile substances by rotary evaporation. Finally, 5 ml of 3-ethoxysilylpropyl-4,5-dihydroimidazolium ionic liquid was added to the residue under N 2 Heating to reflux under protection for 24 hours, removing volatile matter in a vacuum to obtain a viscous liquid, that is, an imidazole-based ionic liquid organofunctional siloxane precursor containing thioether.

[0043] 2. With the temperature kept at 35°C, dissolve 4.0g P123 in 150ml 1.6M hydrochloric acid solution to make the pH of the solution reach 2.0, and ...

Embodiment 3

[0046] 1. Dissolve 5ml of 3-mercapto-1-propanol in 20ml of absolute ethanol with stirring at room temperature, then add 13.8g of iodine, and stir for 24 hours. After the solvent was removed by rotary evaporation, 30 ml of tert-butyl methyl ether was added, and then iodine was extracted with 15 mg / ml sodium bisulfite solution, and the solvent was removed by rotary evaporation. Add 5 ml of thionyl chloride to the residue, stir at room temperature for 24 hours, and remove volatile substances by rotary evaporation. Finally, 5 ml of 3-ethoxysilylpropyl-4,5-dihydroimidazolium ionic liquid was added to the residue under N 2 Heating to reflux under protection for 24 hours, removing volatile matter in a vacuum to obtain a viscous liquid, that is, an imidazole-based ionic liquid organofunctional siloxane precursor containing thioether.

[0047] 2. With the temperature kept at 35°C, dissolve 4.0g P123 in 150ml 1.6M hydrochloric acid solution to make the pH of the solution reach 2.0, and...

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Abstract

The invention discloses an ordered organic-inorganic hybrid mesoporous silicon dioxide, a gold-loaded nanometer material and a preparation method thereof. In the presence of a neutral long-chain templating agent, ethyl orthosilicate is mixed with an imidazole-based ionic liquid organofunctionalized siloxane pass-through body containing a thioether, and the ionic liquid containing a thioether is synthesized at a certain temperature in the next step. Organic-inorganic hybrid mesoporous silica materials. Then auric chloride (HAuCl4) was directly reduced by utilizing the abundant hydroxyl groups on its pore surface, while the thioether organofunctional group in the organic group was used to stabilize the reduced gold particles. The preparation process is simple, no additional reducing agent is needed, and the method is beneficial to environmental protection. The prepared nano-gold particles have the characteristics of small average particle size and uniform distribution, showing good prospects for catalytic application.

Description

Technical field: [0001] The invention relates to an ordered organic-inorganic hybrid mesoporous silicon dioxide material, its loaded nano-gold particle material and its preparation method. Specifically, it relates to a bridging organic functionalized precursor in which a sulfide-containing imidazole ionic liquid is embedded in the pore wall of an organic-inorganic hybrid mesoporous silica material and a preparation method thereof. An organic-inorganic hybrid mesoporous silica material pore preparation nano-gold particles and a preparation method thereof. Background technique; [0002] Mesoporous SiO 2 Because gold nanoparticle materials can meet the special structural properties required by many catalytic reactions, researches on them have been increasing in recent years. But due to SiO 2 The isoelectric point of the surface is low (IEP ≈ 2), and it is difficult to prepare gold nanoparticles with small particle size and uniform dispersion by conventional deposition-precip...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J23/52B01J21/08
Inventor 银董红金勇刘建福喻宁亚秦亮生黎成勇
Owner CHINA TOBACCO HUNAN INDAL CORP
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