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Long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of core-hollow-shell structure and preparation method thereof

A chain thioether and mesoporous technology, which is applied in the field of mesoporous organic-inorganic hybrid spheres and its preparation, can solve problems such as the inability to prepare silicon-based materials, and overcome the inability to transform into egg yolk-eggshell mechanisms and synthesis methods The effect of simplicity and low equipment requirements

Inactive Publication Date: 2014-11-19
NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, organic-inorganic hybrid silicon-based materials containing egg yolk-eggshell structures bridged by long-chain organic groups cannot be prepared under such relatively low temperature and atmospheric pressure conditions.

Method used

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  • Long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of core-hollow-shell structure and preparation method thereof
  • Long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of core-hollow-shell structure and preparation method thereof
  • Long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of core-hollow-shell structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Mix 1ml of concentrated ammonia water (the NH contained in the concentrated ammonia water 3 The mass percent concentration is 25%) mixed with 30ml ethanol and 75ml water, then 0.16g hexadecyltrimethylammonium bromide was dissolved in the mixed solution, and 0.25ml orthosilicon was mixed at 35°C with 980rpm stirring Acid tetraethyl ester and 0.1ml of bis-[3-(triethoxysilyl)propyl]tetrasulfide were added to the aqueous alcohol solution and reacted for 24h to obtain a white solution. The solution was centrifuged and washed once with ethanol;

[0039] (2) Add ethanol to the product obtained in step (1) to dilute to 30ml, take 5ml and centrifuge, disperse in 30ml of water, transfer to a reaction kettle, and react overnight in an oven at 150°C and 1.0MPa;

[0040] (3) The reaction product obtained in step (2) was centrifuged, washed once with ethanol, transferred to a mixed solution of 500 μl concentrated hydrochloric acid and 250 ml ethanol, and heated in a water bath a...

Embodiment 2

[0046] (1) Mix 1ml of concentrated ammonia water (the NH contained in the concentrated ammonia water 3 The mass percent concentration is 25%) mixed with 30ml ethanol and 75ml water, then 0.08g hexadecyltrimethylammonium bromide was dissolved in the mixed solution, and 0.25ml orthosilicon Acid tetraethyl ester and 0.1ml of bis-[3-(triethoxysilyl)propyl]tetrasulfide were added to the aqueous alcohol solution and reacted for 24h to obtain a white solution. The solution was centrifuged and washed once with ethanol;

[0047] (2) Add ethanol to the product obtained in step (1) to dilute to 30ml, take 5ml and centrifuge, disperse in 30ml of water, transfer to a reaction kettle, and react overnight in an oven at 150°C and 1.0MPa;

[0048] (3) The reaction product obtained in step (2) was centrifuged, washed once with ethanol, transferred to a mixed solution of 500 μl concentrated hydrochloric acid and 250 ml ethanol, and heated in a water bath at 60° C. for 3 hours;

[0049] (4) Ste...

Embodiment 3

[0052] (1) Mix 1ml of concentrated ammonia water (the NH contained in the concentrated ammonia water 3 The mass percentage concentration is 25%) mixed with 30ml ethanol and 75ml water, then 0.12g hexadecyltrimethylammonium bromide was dissolved in the mixed solution, and 0.25ml orthosilicon Acid tetraethyl ester and 0.1ml of bis-[3-(triethoxysilyl)propyl]tetrasulfide were added to the aqueous alcohol solution and reacted for 24h to obtain a white solution. The solution was centrifuged and washed once with ethanol;

[0053] (2) Add ethanol to the product obtained in step (1) to dilute to 30ml, take 5ml and centrifuge, disperse in 30ml of water, transfer to a reaction kettle, and react overnight in an oven at 150°C and 1.0MPa;

[0054] (3) The reaction product obtained in step (2) was centrifuged, washed once with ethanol, transferred to a mixed solution of 500 μl concentrated hydrochloric acid and 250 ml ethanol, and heated in a water bath at 60° C. for 3 hours;

[0055] (4) ...

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Abstract

The invention discloses a long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of a core-hollow-shell structure and a preparation method thereof. The hybrid ball comprises a mesoporous ball skeleton, wherein the mesoporous ball skeleton contains a long-chain functional organic group-thioether bond and has the core-hollow-shell structure, uniform adjustable particle diameter, radial ordered mesopores and large specific surface area and pore volume. The preparation method comprises the steps of adding tetraethyl orthosilicate and bi-[3-(triethoxy silicon) propyl] tetrasulfide into a mixed solution of ethanol containing surfactant and ammonia and water, so as to prepare a solid ball containing the thioether bond, then etching off the middle layer of the solid ball in a water solution under the conditions of high temperature and high perssure, and removing the surfactant, so as to obtain a final product. The long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball has great application potentials in the fields of drug delivery, bioimaging and the like, the synthetic method is simple and convenient, and the defect that a silicon-based solid ball which contains the long-chain organic group cannot be changed into a yolk-eggshell mechanism under the conditions of low temperature and normal pressure is overcome.

Description

technical field [0001] The invention relates to a nanomaterial with a core-shell structure of a long-chain heteroatom functional group in the field of inorganic materials and a preparation method thereof, in particular to a mesoporous core-hollow-shell structure containing a long-chain sulfide bond Organic-inorganic hybrid sphere and its preparation method. Background technique [0002] Currently, ordered mesoporous silicon-based materials synthesized via surfactants have attracted extensive attention due to their great potential in the fields of separation, catalysis, and drug delivery. Organic functionalization and morphology control of mesoporous Si-based materials are of great importance for their performance and practical applications. Organofunctionalized mesoporous silicon-based materials are usually post-grafted or cocondensed with trialkoxysilane ((R′O) 3 SiR) obtained. However, post-grafting modification methods often lead to problems such as uneven distribution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 孙佳滕兆刚卢光明刘莹王守巨吴江
Owner NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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