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Synthetic method of organic functional mesoporous silicon oxide

A technology of mesoporous silica and synthesis method, applied in the directions of silica, dyed organosilicon compound treatment, silica, etc., can solve the problems of low degree of functionalization, collapse of pores, etc., and achieve excellent performance, increase output, wide The effect of the application foreground

Active Publication Date: 2017-05-31
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with other functionalization methods, the copolymerization method is easy to operate, with mild reaction conditions and uniform distribution of functional groups, but its functionalization degree is low, and the proportion of organosilane coupling agents as the source of functional groups in the total silicon source is generally not If it exceeds 25%, otherwise it will cause the collapse of the channel, so how to break through the limitation of the functionalization of the copolymerization method has become a research hotspot

Method used

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  • Synthetic method of organic functional mesoporous silicon oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: Synthesis of 10% methylated mesoporous hydrogenated silica

[0032] Dissolve 5.0 g of P123 in 200 ml of 0.01 M hydrochloric acid solution at room temperature, and control the speed of the magnetic stirrer at about 450 rpm. The solution was transferred to a 250ml round-bottomed flask, 10g of solid sodium chloride (NaCl) and 5ml of n-butanol were added, and the stirring was continued for 1 hour at a rotation speed of 450rpm. Mix 1.35ml of methyltriethoxysilane and 12.15ml of triethoxysilane evenly, then quickly pour it into the above-mentioned mixed solution, continue to stir for 12 hours, keep the temperature at room temperature at 25°C, and mix the obtained milky white liquid at 9000rpm ( Rotating speed can be adjusted according to the actual situation) After centrifugation, discard the supernatant, transfer the white precipitate to the filter paper tube, and place it in a Soxhlet extractor for extraction for 24 hours to wash away the surfactant, wherein the ...

Embodiment 2

[0033] Example 2: Synthesis of 50% vinylated mesoporous hydrogenated silica

[0034]Dissolve 5.0 g of P123 in 180 ml of 0.1 M hydrochloric acid solution (HCl) at room temperature, and control the speed of the magnetic stirrer at about 450 rpm. The solution was transferred to a 250ml round bottom flask, 9g of solid sodium chloride (NaCl) and 0.5ml of n-butanol were added, and the stirring was continued for 1 hour at a rotation speed of 450rpm. The total amount of silicon source is 13.5ml, and the proportion of vinyltriethoxysilane is 50% of the total amount. Mix 6.75ml of vinyltriethoxysilane and 6.75ml of triethoxysilane evenly, then quickly pour it into the above mixed solution, continue to stir for 16 hours, keep the temperature at room temperature 25°C, and mix the milky white liquid obtained at 9000rpm ( Rotating speed can be adjusted according to the actual situation) After centrifugation, discard the supernatant, transfer the white precipitate to the filter paper tube, ...

Embodiment 3

[0035] Example 3: Synthesis of 80% methylated mesoporous hydrogenated silica

[0036] Dissolve 5.0 g of P123 in 100 ml of 1 M hydrochloric acid solution (HCl) at room temperature, and control the rotation speed of the magnetic stirrer at about 450 rpm. The solution was transferred to a 250ml round bottom flask, 4g of solid sodium chloride (NaCl) and 0.5ml of n-butanol were added, and the stirring was continued for 1 hour at a rotation speed of 450rpm. Adjust the total amount of silicon source to 10 ml, and the proportion of methyltriethoxysilane to be 80% of the total amount. Mix 8ml of methyltriethoxysilane and 2ml of triethoxysilane evenly, then quickly pour it into the above mixed solution, continue to stir for 14 hours, keep the temperature at room temperature 25°C, and mix the milky white liquid obtained at 9000rpm (speed can Adjust according to the actual situation) after centrifugation, discard the supernatant, transfer the white precipitate to a filter paper tube, and...

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Abstract

The invention relates to a synthetic method of organic functional mesoporous silicon oxide. The method comprises the steps of coupling an organic functional group to ordered mesoporous silicon oxide through a copolymerization method in one step in an acidic condition to obtain the organic functional mesoporous silicon oxide, the functional degree of which is far greater than the grafting rate of a conventional copolymerization method, by taking triethoxy silane and tri alkoxy organic silane coupling agents as a silicon source and a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) as a surfactant. In a reaction process, by controlling the proportion of adding amount of the organic silane coupling agent and triethoxy silane, the functional degree of the mesoporous silicon oxide and the degree of order of ducts can be regulated.

Description

technical field [0001] The invention relates to a method for synthesizing organic functional mesoporous silicon oxide, which belongs to the field of synthesizing surface functionalized mesoporous materials. Background technique [0002] Due to its high specific surface area, specific pore volume, and good hydrothermal stability, mesoporous silica materials are widely used in the fields of controlled drug release, pollutant adsorption, industrial catalysis, and immobilization and separation of biological macromolecules. The surface functionalization of silicon oxide materials is one of the important prerequisites for their application. Copolymerization is a commonly used surface functionalization method, which refers to the one-step synthesis of organosilane coupling agent and inorganic silicon source under acid-base conditions through structure-guided factor co-polymerization and condensation to introduce functional groups into mesoporous channels. Compared with other funct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12C09C3/12C09C1/28
CPCC01B33/12C09C1/28C09C3/12
Inventor 谢卓颖谢凡顾忠泽
Owner SOUTHEAST UNIV
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