Amidoxime modified silicon dioxide nano microsphere composite material and preparation method thereof

A technology of silica and nano-microspheres, which is applied in the field of materials, can solve the problem of fewer adsorption sites, achieve the effect of increasing saturated adsorption capacity, mild reaction conditions, and good selective adsorption performance

Active Publication Date: 2019-11-29
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its modified amidoxime functional groups are small molecules with relatively few adsorption sites.

Method used

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  • Amidoxime modified silicon dioxide nano microsphere composite material and preparation method thereof
  • Amidoxime modified silicon dioxide nano microsphere composite material and preparation method thereof
  • Amidoxime modified silicon dioxide nano microsphere composite material and preparation method thereof

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preparation example Construction

[0061] Preferably, the preparation method of the amidoxime modified silica nanosphere composite material of the present invention includes:

[0062] (1) SiO 2 -NH 2 Preparation

[0063] Take SiO with a particle size of 280~320nm in anhydrous state 2 Microspheres, preferably 300nm SiO 2 Mix the microspheres, toluene and APTES, stir and react at 95~100℃ for 18~20h to obtain SiO 2 -NH 2 ; The SiO 2 The mass ratio of microspheres, toluene and APTES: 1.0~1.2: 17.32~19.05: 1.89~2.08;

[0064] (2) BIBB modified SiO 2 -NH 2 Preparation of SiO 2 -Br

[0065] Take SiO 2 -NH 2 , Toluene and triethylamine, stir at 0℃ (in an ice-water mixture water bath) and add a uniform mixed solution of BIBB and toluene, react for 3-6h, heat up to room temperature and react for 12-14h to prepare SiO 2 -Br;

[0066] SiO in step (2) 2 -NH 2 , The mass ratio of toluene and triethylamine is: 1.0~1.2:12.99~17.32:1.46~1.60; The mass ratio of BIBB and toluene in the uniform mixed solution of BIBB and toluene is: 3.72~4....

Embodiment 1

[0097] A kind of amidoxime polymer brush modified SiO 2 The specific steps of the preparation method of nano-microsphere composite material are as follows:

[0098] (1) SiO 2 Preparation of nanospheres: Take 100mL of absolute ethanol, 6.0mL of distilled water, and 8.0mL of ammonia in a beaker in turn. After stirring evenly, place in a 40℃ oil bath, magnetically stir for 2h, make the system fully stirred and mix, then take 6.0mL ethyl orthosilicate was slowly added dropwise into a three-necked flask at a dropping rate of 0.1mL / min, and then continued to stir for 12h, a milky white colloidal solution would be obtained; take out the prepared silica microsphere colloidal solution and centrifuge at 8000rpm , Pour out the clear liquid, add deionized water and anhydrous ethanol to wash twice, and place the final product in a vacuum drying oven at 60°C for 24 hours to obtain silica microspheres SiO 2 .

[0099] (2) SiO 2 -NH 2 The specific operations are as follows:

[0100] Accurately weig...

Embodiment 2

[0116] A kind of amidoxime polymer brush modified SiO 2 The specific steps of the preparation method of nano-microsphere composite material are as follows:

[0117] (1) SiO 2 Preparation of nano-microspheres: Take 110mL of absolute ethanol, 6.5mL of distilled water, and 8.2mL of ammonia in a beaker. After stirring, place in an oil bath at 45°C and magnetically stir for 3 hours to fully stir and mix the system, and then take it 8.0mL ethyl orthosilicate was slowly added dropwise into a three-necked flask with a dropping rate of 0.2mL / min, and then continued to stir for 12h, a milky white colloidal solution would be obtained; take out the prepared silica microsphere colloidal solution and centrifuge at 8000rmp , Pour out the clear liquid, add deionized water and absolute ethanol to wash twice, and place the final product in a vacuum drying oven at 65°C for 36 hours to obtain silica microspheres SiO 2 .

[0118] (2) SiO 2 -NH 2 The specific operations are as follows:

[0119] Accuratel...

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Abstract

The invention relates to an amidoxime modified silicon dioxide nano microsphere composite material and a preparation method thereof, belonging to the technical field of materials. The preparation method of the amidoxime modified silicon dioxide nano microsphere composite material comprises the following processes: SiO2 microspheres to SiO2-NH2 to SiO2-BR to SiO2-PAN to SiO2-PAO. Compared with thetraditional method, the method for grafting acrylic acid onto silicon dioxide has mild reaction conditions, is insensitive to the oxygen content in the system, has complete reaction, and can achieve the purpose of controlling the grafting rate by controlling the amount of acrylonitrile. The amidoxime modified silicon dioxide nano microsphere composite material prepared by the invention has more adsorption sites, high saturation adsorption capacity and high efficiency of uranium adsorption.

Description

Technical field [0001] The invention relates to an amidoxime modified silica nano-microsphere composite material and a preparation method thereof, and belongs to the field of material technology. Background technique [0002] Uranium is an important element of nuclear fuel, and it is of great significance to my country's industry, national defense, and scientific and technological development. Adopting reasonable and efficient technical methods to adsorb and recover the uranium resources in the uranium-containing solution can not only increase the utilization rate of uranium resources, but also reduce the environmental damage caused by uranium-containing wastewater. [0003] Organic / inorganic nanocomposite materials have good performance characteristics and are widely used in many fields. Among the many inorganic nanomaterials, silica has a wide range of sources, low price, good radiation resistance stability, strong mechanical properties, good biocompatibility and many other adva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30G21F9/12G21F9/20C22B3/24C22B60/02
CPCB01J20/22B01J20/28007B01J20/28016G21F9/20G21F9/12C22B3/24C22B60/0265
Inventor 匙芳廷曾毅杨肖寒丁艺潘宁丁聪聪苟涵梁丹吴昊岩张爱
Owner SOUTHWEAT UNIV OF SCI & TECH
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