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Preparation method of isothiocyano functionalized silicon dioxide material

A silicon dioxide, isothiocyanate technology, applied in the direction of silicon dioxide, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problem of low selectivity, decreased production of silicon dioxide materials, toxic and other problems, to achieve the effect of cheap and easily available raw materials, good biomedical application prospects, and good reaction selectivity

Active Publication Date: 2021-01-01
WUHAN INSTITUTE OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing process for synthesizing isothiocyanate-functionalized silica material, the steps are to first synthesize 3-isothiocyanatopropyltriethoxysilane, Coupling it with silica material has unavoidable technical defects, one of which will use cyanamide when synthesizing 3-isothiocyanatopropyltriethoxysilane, which is a poisonous and extremely A compound that is easy to hydrolyze and polymerize, and the synthesis conditions require an anhydrous system, there are many side reactions, and the selectivity is not very high; the second is to combine 3-isothiocyanatopropyltriethoxysilane with silica materials During coupling, the reaction conditions are easy to oxidize, decompose, and isomerize the isothiocyanate functional group, which further reduces the yield of the synthesized isothiocyanate-functionalized silica material (only 20-40%)

Method used

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  • Preparation method of isothiocyano functionalized silicon dioxide material
  • Preparation method of isothiocyano functionalized silicon dioxide material
  • Preparation method of isothiocyano functionalized silicon dioxide material

Examples

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Embodiment 1

[0033] A kind of isothiocyanate functionalized silica material, its preparation method comprises the steps:

[0034] 1) Preparation of Amino-modified Silica Nanoparticles

[0035] Add 7.2mL of ammonia water (25wt%) dropwise to 150mL of absolute ethanol and stir at room temperature to obtain a mixed solution I. Add 3mL of tetraethoxysilane and 1mL of 3-aminopropyltriethoxysilane into 30mL of ethanol and mix and stir for 0.5h , then poured into the mixed solution I and stirred at room temperature for 12h, concentrated the liquid with a rotary evaporator, collected by centrifugation (10000rpm, 10min), washed and dispersed with deionized water and absolute ethanol several times, dried (60°C, 12h), and obtained amino Modified silica nanoparticles (for a schematic diagram, see figure 1 a);

[0036] 2) Preparation of isothiocyano-functionalized silica nanoparticles

[0037] Disperse 3g of amino-modified silica nanoparticles into 50mL of absolute ethanol, add dropwise 4.0mL of am...

Embodiment 2

[0041] A kind of isothiocyanate functionalized silica material, its preparation method comprises the steps:

[0042] 1) Preparation of Amino-modified Silica Nanoparticles

[0043] Add 7.2mL of ammonia water (25wt%) dropwise to 180g of water and stir at room temperature to obtain a mixed solution I, add 1.5mL of tetraethoxysilane and 0.4mL of 3-aminopropyltrimethoxysilane into 30mL of ethanol, mix and stir for 0.5h, then pour Put it into the mixed solution I and stir at room temperature for 12h, concentrate the liquid with a rotary evaporator, collect by centrifugation (10000rpm, 10min), wash and disperse with deionized water and absolute ethanol several times, and dry (60°C, 12h) to obtain amino-modified dioxide Silicon nanoparticles;

[0044] 2) Preparation of isothiocyano-functionalized silica nanoparticles

[0045] Disperse 3g of amino-modified silica nanoparticles into 50mL of tetrahydrofuran, add 4mL of ammonia water (25wt%), stir at 15°C for 0.5h, add dropwise 1.6mL of...

Embodiment 3

[0047] A kind of isothiocyanate functionalized silica material, its preparation method comprises the steps:

[0048] 1) Preparation of Amino-modified Silica Nanoparticles

[0049] Add 7.2mL of ammonia water (25wt%) dropwise to 180g of water and stir at room temperature to obtain a mixed solution I, add 1.5mL of tetraethoxysilane and 0.4mL of 3-aminopropyltrimethoxysilane into 30mL of ethanol, mix and stir for 0.5h, then pour Put it into the mixed solution I and stir at room temperature for 12h, concentrate the liquid with a rotary evaporator, collect by centrifugation (10000rpm, 10min), wash and disperse with deionized water and absolute ethanol several times, and dry (60°C, 12h) to obtain amino-modified dioxide Silicon nanoparticles;

[0050] 2) Preparation of isothiocyano-functionalized silica nanoparticles

[0051] Disperse 3 g of amino-modified silica nanoparticles into 50 mL of tetrahydrofuran, add 3.5 mL of triethylamine, stir at 15 °C for 0.5 h, add 1.6 mL of carbon...

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Abstract

The invention discloses a preparation method of an isothiocyano functionalized silicon dioxide material, which comprises the following steps: 1) carrying out functional modification on a silicon dioxide material by using a silane coupling agent with an amino functional group to obtain an amino modified silicon dioxide material; and 2) dispersing the amino-modified silicon dioxide material in a solvent, then introducing an alkali source and carbon disulfide, carrying out a stirring reaction in a solution system or under a sol condition, and then carrying out centrifugal collection, washing anddrying to obtain the isothiocyano functionalized silicon dioxide material. The preparation method provided by the invention is simple and mild in reaction conditions, the obtained isothiocyano functionalized silicon dioxide material is good in stability, an obvious functional group absorption peak can be detected by using an infrared spectrum, the preparation method is suitable for popularizationand application, and the problems of harsh reaction conditions, multiple side reactions and relatively low target product yield of an existing preparation method can be effectively solved; the material has a good biomedical application prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic functional materials, and in particular relates to a preparation method of an isothiocyanate-functionalized silica material. Background technique [0002] At present, mesoporous silica nanomaterials are used in the fields of catalyst carriers, drug sustained release and other fields due to their highly ordered pores, uniform and adjustable mesoporous pore size, and stable skeleton structure. However, a single silica nanomaterial has its own limitations. When the amorphous silica nanomaterial is modified, its application range has also been greatly expanded. [0003] The C located in the isothiocyanate group (-N=C=S) in the isothiocyanate molecule is highly electrophilic and can undergo nucleophilic addition reactions with nucleophiles. Amino groups, hydroxyl groups, thiols, β-carbonyl groups, carboxylic acids, etc. as nucleophiles can undergo nucleophilic addition reactions with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y30/00B82Y5/00
CPCC01B33/12B82Y30/00B82Y5/00C01P2002/82
Inventor 陈龙姜兴茂
Owner WUHAN INSTITUTE OF TECHNOLOGY
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