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Process for preparing SiO2 mesoporous material-cadmium sulfide composition nano material

A technology of mesoporous materials and silicon dioxide, which is applied in the field of preparation of silica mesoporous materials-cadmium sulfide composite nanomaterials, can solve problems such as economical efficiency, low environmental protection, inability to ensure stable distribution, complicated procedures, etc., and achieve Good economy, good environmental friendliness, evenly distributed effect

Inactive Publication Date: 2007-01-24
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, the reported methods for preparing silicon-based mesoporous materials—CdS nanocomposites may require the use of expensive and highly toxic organic cadmium precursors, which are less economical and environmentally friendly (Inorganic Chemistry, 2005, 44, 2590); or it is necessary to pre-prepare CdS nanoparticles, which is not only complicated but also cannot guarantee its stable distribution in mesoporous materials (Journal of Collid and Interface Science, 2003, 268, 394)

Method used

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  • Process for preparing SiO2 mesoporous material-cadmium sulfide composition nano material
  • Process for preparing SiO2 mesoporous material-cadmium sulfide composition nano material
  • Process for preparing SiO2 mesoporous material-cadmium sulfide composition nano material

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Embodiment 1

[0021] References Science 1998, 279, 548 reported the preparation of SBA-15: 2 grams of EO 20 PO 70 EO 20 (P123) Templating agent dissolved in 15 g H 2 O and 60 g of 2mol / L HCl in a mixed solution, stirred with a magnetic stirrer until clarified. Add 4.25 g of TEOS (orthoethyl silicate), stir for 24 hours, then move into a stainless steel reactor with a polytetrafluoroethylene liner, and age at 373K for 48 hours. Filtrate the precipitate, wash it with water, and dry it, then bake it at 823K for 6 hours to obtain a silica mesoporous material with a specific surface area of ​​696m 2 g -1 , the pore size is 6.12nm.

[0022] Take by weighing 7.61 grams (0.01mol) of thiourea and 1.14 grams (0.005mol) of cadmium chloride, dissolve in 50 milliliters of deionized water, weigh 1.2 grams (0.02mol) of SBA-15 mesoporous material and put it into the above solution for immersion, After stirring at room temperature for 12 hours, filter, rinse with deionized water and ethanol in turn, a...

Embodiment 2

[0028] The preparation steps of the SBA-15 mesoporous material are the same as in Example 1, and the CdS loading operation steps and immersion time are the same as in Example 1, but the amount of thiourea is increased to 15.22 grams (0.02mol), and the amount of cadmium chloride is increased to 2.28 Gram (0.005mol).

[0029] Now the small-angle X-ray diffraction pattern (XRD) of gained SBA-15-CdS nanocomposite material is as follows figure 1 c curve shown. It can be seen from the figure that when the concentration of CdS increases and the loading amount in the SBA-15 mesoporous material increases, the hexagonal phase pore structure of the SBA-15 mesoporous material is still maintained to a certain extent, but its order degree changes. declined to a certain extent. BET test shows that the specific surface of this embodiment gained SBA-15-CdS nanocomposite material is reduced to 402m 2 g -1 ; Pore diameter also decreased from 6.12nm to 5.38nm. However, HRTEM characterization...

Embodiment 3

[0031] The preparation step of SBA-15 mesoporous material is the same as Example 1, and the CdS loading operation step is the same as Example 1, but the amount of thiourea increases to 15.22 grams (0.02mol), and the amount of cadmium chloride increases to 2.28 grams (0.005 mol). mol); the immersion time was extended from 12 hours to 24 hours.

[0032] Now the small-angle X-ray diffraction pattern (XRD) of gained SBA-15-CdS nanocomposite material is as follows figure 1 d curve shown. It can be seen from the figure that as the immersion time prolongs, the loading of CdS in the SBA-15 mesoporous material continues to increase, and the pore order of the SBA-15 mesoporous material further decreases, and the structural characteristics of the hexagonal phase have basically been lost. .

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Abstract

The present invention relates to preparation process of mesoporous SiO2-cadmium sulfide composite nanometer material, and features low material cost, low toxicity, homogeneous distribution of cadmium sulfide in the mesoporous material pore channel, being suitable for industrial production, etc. The preparation process includes the following steps: 1. preparing mesoporous SiO2 material with block copolymer of the general expression EO20PO70EO20 as templating agent and n-ethyl silicate as silicon source, and through hydrothermal crystallizing under acid condition; 2. compounding mixed water solution with cadmium chloride and thiourea in the molar ratio of 1 to 0.5-2; 3. soaking the mesoporous SiO2 material in the mixed water solution, with the molar ratio between mesoporous SiO2 material and cadmium chloride of 2-10 to 1; and 4. precipitating the soaked mixed solution, stoving the precipitate and roasting to pyrolyze in protecting N2 to obtain the product.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing a silica mesoporous material-cadmium sulfide composite nanomaterial. Background technique [0002] Nanomaterials refer to solid materials with characteristic dimensions ranging from 1 to 100 nm. Due to the three major characteristics of nanomaterials, namely, quantum size effect, surface and interface effect, small size effect and macroscopic quantum tunneling effect; nanomaterials exhibit unique properties that are obviously different from bulk materials and single molecules. ZnS, CdS and other II-VI nano-semiconductors have unique optoelectronic properties, such as wide excitation spectrum, narrow and symmetrical emission spectrum, long fluorescence lifetime, etc., which have great potential in many fields such as biological probes, fuel cells, and nonlinear optics. Broad application prospects. However, nanomaterials have very large surface energy and a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/59C01B33/113C09K11/54G01N33/48
Inventor 刘勇来国桥蒋剑雄李美江倪勇
Owner HANGZHOU NORMAL UNIVERSITY
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