Method for synthesizing silicon dioxide hollow sphere with mesoporous channel controlled by dodecyl sulfonic acid sodium salt

A technology of sodium dodecylsulfonate and silicon dioxide, which is applied in the direction of silicon oxide, etc., can solve the problems that the hole diameter and wall thickness of the hollow ball cannot be adjusted, the porosity of the hole wall cannot be controlled, and the internal and external transportation of materials cannot be realized. Achieve the effect of being conducive to internal and external transmission, low cost, and simple preparation process

Inactive Publication Date: 2008-03-19
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yeh et al. (YehY.Q., Chen B.C., Liu H.P., Tang C.Y., Langmuir, 2006, 22, 6) proposed to use P123 and anion and cation mixed templates to synthesize mesoporous shell hollow spheres in weakly acidic environment, but the material Part of the mesoporous shell channel is parallel to the mesoporous shell, resulting in the inability of molecules to transport inside and outside, and the pore diameter and wall thickness of the hollow sphere cannot be adjusted
Djojoputro et al. (Jojoputro H.D., Zhou X.F., Qiao S.Z., Wang L.Z., Yu C.Z., Lu G.Q., J.Am.Chem.Soc., 2006, 128, 6320) utilize Fluorocarbon surfant (C 3 f 7 O(CFCF 3 CF 2 CONH(CH 2 ) 3 N + (C 2 h 5 ) 2 CH 3 I - )FC 4 and cationic surfactant (cetyltrimethylammomium bromide) CTAB as a mixed template and (1,2-bis(trimethoxysily)ethane) BTME as a silicon source to synthesize organosilicon mesoporous hollow spheres, the pore wall thickness and pore size can be adjusted, but The degree of porosity of the pore wall cannot be controlled, and the internal and external transportation of larger substances cannot be realized, and the obtained spherical particle size range is generally 500-1000nm
Zhu Yufang et al. (patent application number 200510112407) used polyvinylpyrrolidone, CTAB and CTAC as mixed surfactants to synthesize hollow silicon spheres containing mesoporous channels in an alkaline environment, but did not propose a control method

Method used

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  • Method for synthesizing silicon dioxide hollow sphere with mesoporous channel controlled by dodecyl sulfonic acid sodium salt
  • Method for synthesizing silicon dioxide hollow sphere with mesoporous channel controlled by dodecyl sulfonic acid sodium salt

Examples

Experimental program
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Embodiment 1

[0029] The block copolymer P103 was dissolved in deionized water to prepare a 20 wt% aqueous solution, which was stored in a refrigerator for later use. Take 10ml of the above block copolymer aqueous solution, adjust the concentration to 2M with hydrochloric acid, the total volume is 50ml, and the P103 concentration is 2wt%. Stir in a water bath at 40° C., and then add 0.05 g of SDS and 0.3 g of NaF in sequence as template aids. After fully stirring for 30 minutes, 3 g of TEOS was added, and the mixed solution was stirred in a water bath for 24 hours. After hydrothermal heating at 100 °C for 1 day, the resulting white precipitate was filtered, washed several times with deionized water, and dried in an oven. Calcining at 400-600° C. for 6 hours in an air atmosphere to remove the template agent, the heating rate is 2° C. / min, to obtain a silica hollow sphere material with mesoporous channels.

[0030] From the scanning electron microscope photos of A and B in Figure 1, it can be...

Embodiment 2

[0032] The block copolymer P123 was dissolved in deionized water to prepare a 20 wt% aqueous solution, which was stored in a refrigerator for later use. Take 10ml of the above block copolymer aqueous solution, adjust it to a concentration of 2M with sulfuric acid, the total volume is 50ml, and the concentration of P123 is 4wt%. Stir in a water bath at 40°C, and then add template aids 0.1gSDS and 0.3gNaF in sequence. After fully stirring for 30 minutes, 3 g of TEOS was added, and the mixed solution was stirred in a water bath for 24 hours. After hydrothermal heating at 100 °C for 1 day, the resulting white precipitate was filtered, washed several times with deionized water, and dried in an oven. Calcining at 400-600° C. for 6 hours in an air atmosphere to remove the template agent, the heating rate is 2° C. / min, to obtain a silica hollow sphere material with mesoporous channels.

[0033] Through the scanning electron microscope photos of C and D in Figure 1, it can be seen th...

Embodiment 3

[0035] Dissolve the block copolymer P105 in deionized water to prepare a 20 wt% aqueous solution, and store it in a refrigerator for later use. Take 10ml of the above aqueous solution of block copolymer, adjust the concentration to 2M with nitric acid, the total volume is 50ml, and the concentration of P105 is 5wt%. Stir in a water bath at 40° C., and then add 0.2 g of SDS and 0.3 g of NaF as template aids in sequence. After fully stirring for 30 minutes, 3 g of TEOS was added, and the mixed solution was stirred in a water bath for 24 hours. After hydrothermal heating at 100 °C for 1 day, the resulting white precipitate was filtered, washed several times with deionized water, and dried in an oven. Calcining at 400-600° C. for 6 hours in an air atmosphere to remove the template agent, the heating rate is 2° C. / min, to obtain a silica hollow sphere material with mesoporous channels.

[0036] Through the scanning electron microscope photos of E and F in Figure 1, you can see th...

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Abstract

The invention belongs to an inorganic mesoporous material area, in particular to a preparation method of a controllable silica hollow sphere material in a certain diameter range. The anionic surfactant sodium dodecyl sulfonate (SDS) controls the synthesis of spherical wall, which is provided with mesoporous channels and narrow distribution of diameter. The invention uses block copolymer and sodium dodecyl sulfonate as mixing template; with the addition of silicon source, the sol is formed after mixing; under the acid condition, through the agitating and aging treatment, after hydrothermal process, filtering and drying, the template is calcined to obtain silica hollow sphere with the mesoporous channel. Through changing the content of SDS, the synthesis of different size of silica hollow spheres with the mesoporous channel can be controlled. The invention has a simple process and a low cost; the mesoporous shell thickness and the pore diameter of the prepared silica hollow sphere with the mesoporous channel can be controlled in a large range; the invention is beneficial to the internal and external transmission of guest molecules; the invention also improves the reserves of guest molecules, which realizes the controlled release effectively.

Description

technical field [0001] The invention belongs to the field of inorganic mesoporous materials, in particular to a ball wall synthesized by anionic surfactant sodium dodecylsulfonate (SDS), which has mesoporous channels and narrow particle size distribution, which can be controlled within a certain particle size range. A method for preparing a silica hollow sphere material. Background technique [0002] In 1992, researchers from Mobile Corporation in the United States first reported the M41S series with high specific surface area and high degree of order in Nature (Kresge C.T., LeonowiczM.E., Roth W.J., Vartuli J.C., Beck J.S., Nature, 1992, 359, 710). Since the introduction of mesoporous materials, the study of mesoporous materials has become a research hotspot in the fields of chemistry and materials. Especially from Zhao reported in Science (Zhao D., Feng J., Huo Q., Melosh N., Stucky G.D., Science, 1998,279,548) that there are larger apertures with non-ionic surfactants as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/113C04B38/06
Inventor 刘会洲羊彬郭晨
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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