A kind of method for preparing mesoporous silica

A mesoporous silica and silicon source technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of potential safety hazards, low solvent volatilization efficiency, environmental pollution, etc., achieve mild reaction conditions, facilitate large-scale production, Simple and efficient preparation process

Inactive Publication Date: 2011-12-28
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of volatilizing the solvent is to transfer the obtained sol to an evaporating dish, crucible or porcelain boat, or directly apply it to glass sheets, silicon chips, plastics and other carriers by "dip coating method" or "spin coating method". Low volatilization efficiency and easy pollution to the environment and potential safety hazards in the production process

Method used

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  • A kind of method for preparing mesoporous silica
  • A kind of method for preparing mesoporous silica
  • A kind of method for preparing mesoporous silica

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Dissolve 1g of styrene-butadiene-styrene triblock copolymer and 24.79g of mercaptopropyltriethoxysilane in 48mL of dioxane, and stir evenly at 10-45°C; then Add 0.17 g of azobisisobutyronitrile and disperse evenly, then gradually raise the temperature to 60°C and react for 1 day. After precipitation, suction filtration and drying, an organosiloxane-modified styrene-butadiene-styrene triblock copolymer is obtained;

[0038] (2) Dissolve 0.2010g of organosiloxane-modified styrene-butadiene-styrene triblock copolymer and 1.8015g of ethyl orthosilicate in 5mL of tetrahydrofuran in a closed container at 10-45°C and stirring constantly, then add 0.6544g deionized water and 0.6568g 1M hydrochloric acid drop by drop, along with the carrying out of stirring, the generation of sol-gel reaction makes the system viscosity rise gradually; Stop stirring after about 25 minutes, keep the reactor 10 It was sealed at -45°C for 14 days; then it was degraded at high temperature in a t...

Embodiment 2

[0040] (1) Dissolve 1g of styrene-butadiene-styrene triblock copolymer and 24.79g of mercaptopropyltriethoxysilane in 48mL of dioxane, and stir evenly at 10-45°C; then Add 0.17 g of azobisisobutyronitrile and disperse evenly, then gradually raise the temperature to 60°C and react for 1 day. After precipitation, suction filtration and drying, an organosiloxane-modified styrene-butadiene-styrene triblock copolymer is obtained;

[0041] (2) Dissolve 0.4002g of organosiloxane-modified styrene-butadiene-styrene triblock copolymer and 1.6039g of ethyl orthosilicate in 5mL of tetrahydrofuran in a closed container at 10-45°C and stirring continuously, then add 0.6175g deionized water and 0.6300g 1M hydrochloric acid drop by drop, along with the carrying out of stirring, the occurrence of sol-gel reaction makes the viscosity of the system gradually increase; stop stirring after about 15 minutes, keep the reactor for 10 It was sealed at -45°C for 14 days; then it was degraded at high t...

Embodiment 3

[0043] (1) Dissolve 1g of styrene-butadiene-styrene triblock copolymer and 24.79g of mercaptopropyltriethoxysilane in 48mL of dioxane, and stir evenly at 10-45°C; then Add 0.17 g of azobisisobutyronitrile and disperse evenly, then gradually raise the temperature to 60°C and react for 1 day. After precipitation, suction filtration and drying, an organosiloxane-modified styrene-butadiene-styrene triblock copolymer is obtained;

[0044] (2) Dissolve 0.6024g of organosiloxane-modified styrene-butadiene-styrene triblock copolymer and 1.4080g of ethyl orthosilicate in 5mL of tetrahydrofuran in a closed container at 10-45°C and stirring constantly, then add 0.5807g deionized water and 0.5764g 1M hydrochloric acid dropwise, along with the carrying out of stirring, the occurrence of sol-gel reaction makes the viscosity of the system gradually increase; stop stirring after about 8 minutes, keep the reactor for 10 It was sealed at -45°C for 14 days; then it was degraded at high temperat...

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Abstract

The invention relates to a method for preparing mesoporous silicon dioxide, the method is characterized in that mercapto-vinyl can be used for a free radical addition reaction, organo-silicone containing a mercapto group and polybutadiene block of triblock copolymer of styrene-butadiene-styrene are reacted, an organo-siloxane modified styrene-butadiene-styrene triblock copolymer can be obtained, then the organo-siloxane modified styrene-butadiene-styrene triblock copolymer is carried out a sol-gel reaction with a silicon source under the acidic or alkaline condition to form gel, the mesoporous silicon dioxide is obtained after cracking the gel. Compared with the prior art, the mesoporous silicon dioxide material has the average pore diameter of 5-18nm, the pore volume of 0.24-0.30 cm<3>/g, the specific surface area of 418-480 cm<2>/g, and has the advantages of cheap raw material and easy raw material acquisition, mild reaction condition, simple and high efficient preparation process, safety and environmental protection, and is convenient for large scale production.

Description

technical field [0001] The invention relates to a method for preparing inorganic materials, in particular to a method for preparing mesoporous silicon dioxide. Background technique [0002] Mesoporous silica has a large nano-scale pore size and is suitable for many purposes such as macromolecular separation, catalysis, and microreactors. However, there is still a lack of simple and practical methods for the synthesis of mesoporous silica. [0003] Chinese patent CN 1872684A reports a preparation method of mesoporous silica, dissolving template agent and water-soluble polymer in water, adding acid to adjust the pH value to between 0.3-0.4; adding silicate to obtain reaction solution , stirred and hydrolyzed at room temperature for 4-20 hours, transferred to a autogenous pressure reactor, crystallized at 80-120°C for 24 hours, filtered off, washed, dried, and finally calcined in a muffle furnace at 550°C for 6 hours to obtain mesoporous silica. The template used in the meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12
Inventor 郑思珣于人同
Owner SHANGHAI JIAO TONG UNIV
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