Amidoxime-modified silica nano-microsphere composite material and preparation method thereof

A technology of silicon dioxide and nano-microspheres, applied in the field of materials, can solve the problem of less adsorption sites, and achieve the effects of increasing the saturated adsorption capacity, selecting good adsorption performance, and mild reaction conditions

Active Publication Date: 2022-04-15
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 silica nano-microsphere composite material and preparation method thereof
  • Amidoxime-modified silica nano-microsphere composite material and preparation method thereof
  • Amidoxime-modified silica nano-microsphere composite material and preparation method thereof

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preparation example Construction

[0061] Preferably, the preparation method of amidoxime modified silica nano-microsphere composite material of the present invention comprises:

[0062] (1) SiO 2 -NH 2 preparation of

[0063] Take SiO with a particle size of 280-320nm in anhydrous state 2 Microspheres, preferably 300nm SiO 2 Mix microspheres, toluene and APTES, stir and react at 95-100°C for 18-20 hours to obtain SiO 2 -NH 2 ; the SiO 2 The mass ratio of microspheres, toluene and APTES is: 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, stirred at 0°C (in an ice-water mixture water bath) and added a uniform mixed solution of BIBB and toluene, reacted for 3 to 6 hours, raised the temperature to room temperature and reacted for 12 to 14 hours to obtain SiO 2 -Br;

[0066] Step (2) described SiO 2 -NH 2 1. The mass ratio of toluene and triethylamine is: 1.0~1.2:12.99~17.32:1.46~1.60; the mass rati...

Embodiment 1

[0097] A kind of amidoxime polymer brush modified SiO 2 The specific steps of the preparation method of the 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 water in a beaker in sequence, stir evenly, place in a 40°C oil bath, and stir magnetically for 2 hours to fully stir the system, then take Slowly add 6.0mL tetraethyl orthosilicate into the three-neck flask drop by drop at a rate of 0.1mL / min, and then continue to stir for 12 hours to obtain a milky white colloidal solution; take out the prepared colloidal solution of silica microspheres and centrifuge at 8000rmp , Pour out the supernatant, add deionized water and absolute ethanol to wash twice by centrifugation, put the final product in a vacuum drying oven at 60°C for 24 hours, and then prepare silica microspheres SiO 2.

[0099] (2) SiO 2 -NH 2 preparation, the specific operations are as...

Embodiment 2

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

[0117] (1) SiO 2 Preparation of nanospheres: Take 110mL of absolute ethanol, 6.5mL of distilled water, and 8.2mL of ammonia water in a beaker in sequence, stir evenly, place in an oil bath at 45°C, and stir magnetically for 3 hours to fully stir and mix the system, then take Add 8.0mL tetraethyl orthosilicate slowly into the three-neck flask drop by drop at a rate of 0.2mL / min, and then continue to stir for 12 hours to obtain a milky white colloidal solution; take out the prepared colloidal solution of silica microspheres and centrifuge at 8000rmp , Pour out the supernatant, add deionized water and absolute ethanol to wash twice by centrifugation, put the final product in a vacuum drying oven at 65°C for 36h, and then prepare silica microspheres SiO 2 .

[0118] (2) SiO 2 -NH 2 preparation, the specific operation...

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Abstract

The invention relates to an amidoxime-modified silica nano-microsphere composite material and a preparation method thereof, belonging to the field of material technology. The process of the preparation method of the amidoxime modified silica nano-microsphere composite material of the present invention is as follows: SiO 2 Microsphere → SiO 2 ‑NH 2 → SiO 2 ‑Br→SiO 2 ‑PAN→SiO2 2 ‑PAOs. The method for grafting acrylonitrile onto silica of the present invention has milder reaction conditions than traditional methods, is insensitive to the oxygen content in the system, and reacts thoroughly. The purpose of controlling the grafting rate can be achieved by controlling the amount of acrylonitrile . The amidoxime-modified silicon dioxide nano-microsphere composite material prepared by the invention has more adsorption sites, high saturated adsorption capacity and can efficiently adsorb uranium.

Description

technical field [0001] The invention relates to an amidoxime-modified silica nano-microsphere composite material and a preparation method thereof, belonging to the field of material technology. Background technique [0002] Uranium is an important component of nuclear fuel, and it is of great significance to my country's industry, national defense and technological development. Adsorption and recycling of uranium resources in uranium-containing solutions by reasonable and efficient technical methods can not only improve the utilization rate of uranium resources, but also reduce the damage caused by uranium-containing wastewater to the environment. [0003] Organic / inorganic nanocomposites have good performance characteristics and are widely used in many fields. Among many inorganic nanomaterials, silica has many advantages such as wide sources, low price, good radiation resistance stability, strong mechanical properties, and good biocompatibility. Materials with good proper...

Claims

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Application Information

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Patent Type & Authority Patents(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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