Mercapto-functionalized organic inorganic hybrid ordered mesoporous silicon material and preparation method thereof

A functionalized, mesoporous silicon technology, applied in the field of materials, can solve problems such as limitations, low content, and difficulty in maintaining an ordered structure, and achieve the effects of good complexation ability, large specific surface area, and low price

Inactive Publication Date: 2010-06-23
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the content of organic components in the blended materials is often relatively low. When the content of organic components increases, the ordered structure is difficult to maintain, and its application is limited.

Method used

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  • Mercapto-functionalized organic inorganic hybrid ordered mesoporous silicon material and preparation method thereof
  • Mercapto-functionalized organic inorganic hybrid ordered mesoporous silicon material and preparation method thereof
  • Mercapto-functionalized organic inorganic hybrid ordered mesoporous silicon material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] At 40°C, 4.00g F127 (0.32mmol) was dissolved in 15.00g anhydrous ether and stirred for 1 hour to obtain solution A; 2.384g of organosilicon source 3-mercaptopropyltriethoxysilane (10mmol) at 1.0 Hydrolyzed under the condition of g (0.2mol / L) hydrochloric acid for 30 minutes to obtain solution B.

[0038] The two solutions were mixed, 1.8 g of soluble resole resin (4.5 mmol) was added, and the reaction was stirred for 2 hours at 40°C. Then spread the mixture evenly in a petri dish and place it at room temperature for 7 hours to evaporate the organic solvent.

[0039] Finally, it is transferred to an oven at 100°C, and after low-temperature thermosetting for 24 hours, the product is refluxed in a 48wt% sulfuric acid solution at 85°C for 48 hours to remove the surfactant.

[0040] The obtained material has a two-dimensional hexagonal mesoscopic structure (space group p6mm), a pore diameter of 5.4nm, and a pore volume of 0.30cm 3 / g, the specific surface area is 223m 2 / g, sulfhy...

Embodiment 2

[0043] At 40°C, 1.60g F127 (0.13mmol) was dissolved in 10.00g absolute ethanol and stirred for 1 hour to obtain solution A; 0.405g organosilicon source 3-mercaptopropyltriethoxysilane (1.7mmol) and 1.729 g of inorganic silicon source TEOS (8.3 mmol) was hydrolyzed under 1.0 g (0.2 mol / L) hydrochloric acid for 30 minutes to obtain solution B.

[0044] The two solutions were mixed, 1.0 g of soluble resole resin (2.5 mmol) was added, and the reaction was stirred for 2 hours at 40°C. Then spread the mixture evenly in a petri dish and place it at room temperature for 7 hours to evaporate the organic solvent.

[0045] Finally transferred to a 100 ℃ oven, after low temperature thermosetting for 24 hours, the product was refluxed in a 48wt% sulfuric acid solution at 95 ℃ for 48 hours to remove the surfactant.

[0046] The obtained material has a two-dimensional hexagonal mesoscopic structure (space group p6mm), the pore diameter is 5.8nm, and the pore volume is 0.3cm 3 / g, the specific surf...

Embodiment 3

[0048] At 40°C, dissolve 2.0 g of F127 (0.16 mmol) in 10.00 g of absolute ethanol and stir for 1 hour to obtain solution A; 0.654 g of organosilicon source 3-mercaptopropyltrimethoxysilane (3.3 mmol) and 1.396 g of inorganic silicon source TEOS (6.7 mmol) was hydrolyzed under 1.0 g (0.2 mol / L) hydrochloric acid for 30 minutes to obtain solution B.

[0049] Mix the two solutions, add 1 g of soluble resole (2.5 mmol), and stir and react at 40°C for 2 hours. Then spread the mixture evenly in a petri dish and place it at room temperature for 7 hours to evaporate the organic solvent.

[0050] Finally, it is transferred to an oven at 100°C, and after low-temperature thermosetting for 24 hours, the product is refluxed in a 48wt% sulfuric acid solution at 85°C for 48 hours to remove the surfactant.

[0051] The obtained material has a two-dimensional hexagonal mesoscopic structure (space group p6mm), the pore diameter is 4nm, and the pore volume is 0.18cm 3 / g, the specific surface area is ...

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Abstract

The invention belongs to the technical field of mesoporous material preparation, in particular to a mercapto-functionalized organic inorganic hybrid ordered mesoporous silicon material and a synthesizing method thereof. The material has high content of mercapto functional group (0.1 to 15 weight percent), high specific surface area (200 to 500m<2> / g), large pore volume (0.1 to 1.0cm<3> / g), and uniform pore diameter (3 to 12nm), and has a two-dimensional hexagonal mesoscopic structure. The synthesizing method comprises the following steps: carrying out prehydrolysis on an inorganic silicon source and a mercapto-containing organic silicon sources under an acidic condition to form a silicon source precursor; mixing the precursor with nonionic surfactant, adding soluble resin in the mixture, and carrying out self-assembly in the organic solution to obtain the mercapto functionalized-nonionic surfactant composite material; and removing the surfactant through solvent reflux extraction. The material has simple operation and low cost, can be used as an adsorbent for heavy metal ions in wastewater, and opens a new way for treatment of industrial wastewater containing heavy metal.

Description

Technical field [0001] The invention relates to the field of materials, and is a mercapto functionalized organic-inorganic hybrid ordered mesoporous silicon material and a combined preparation method. Background technique [0002] In recent years, ordered mesoporous materials have developed rapidly. Due to its high specific surface area, relatively large pore volume and uniform pore size, it has been widely used in adsorption, catalysis and separation for a long time. Most of the initial synthesis focused on silica-based materials. However, in practical applications, the performance of the mesoporous silica solid framework alone is far from meeting the requirements. Therefore, further functionalization and expansion of the composition of the mesoporous materials will expand The scope of application is always the focus of development. [0003] The use of chemical modification methods in the pores to introduce organic compounds and other substances into the cage or channel can grea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30
Inventor 万颖庄鑫
Owner SHANGHAI NORMAL UNIVERSITY
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