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Amidoximated mesoporous silica microsphere adsorbent and preparation method thereof

A mesoporous silica and microsphere adsorption technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of high production cost, low production efficiency, and low adsorption capacity , to achieve the effects of short adsorption equilibrium time, improved production efficiency, and high uranium adsorption capacity

Inactive Publication Date: 2017-06-30
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production of mesoporous silica microspheres usually uses tetraethyl orthosilicate as raw material, but its production cost is high, and it requires a long reaction time (24-120h), which leads to low production efficiency, while mesoporous silica The adsorption capacity of microspheres to uranium is usually low; therefore, how to effectively reduce the production cost of mesoporous silica microsphere adsorbents, improve production efficiency, and improve the adsorption capacity of mesoporous silica microspheres to uranium is the use of mesoporous silica microspheres. Important problems that must be solved for the separation and enrichment of uranium from uranium-containing wastewater by adsorption of porous silica microspheres

Method used

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  • Amidoximated mesoporous silica microsphere adsorbent and preparation method thereof
  • Amidoximated mesoporous silica microsphere adsorbent and preparation method thereof
  • Amidoximated mesoporous silica microsphere adsorbent and preparation method thereof

Examples

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Effect test

Embodiment 1

[0023] A preparation method of amidoxime mesoporous silica microsphere adsorbent, the specific steps are as follows:

[0024] (1) Synthesis of amidoximated organosilane functionalization reagent (AOES)

[0025] Add 120 mg (3-cyanopropyl) triethoxysilane (CP-TES), 387.2 mg hydroxylamine (AO) and 275 mg Na 2 CO 3 , heated under reflux at 70°C for 12 hours, and purified by Soxhlet extraction to obtain an amidoximated organosilane functional reagent ((3-amidoximopropyl)triethoxysilane), the reaction formula is as follows:

[0026]

[0027] (2) Preparation of amidoxime mesoporous silica microsphere adsorbent (according to AOES / Na 2 SiO 3 Mass ratio 10wt.% implementation)

[0028] Take 60mL of absolute ethanol, 80mL of deionized water, 30mL of acetic acid solution (25wt.%) and 2.0mL of P123 and place them in a container for rapid stirring and mixing. While stirring, add 50mL of sodium silicate solution (containing 10.0g of silicon NaOH) and 1.0 g of AOES were thoroughly mixe...

Embodiment 2

[0031] A preparation method of amidoxime mesoporous silica microsphere adsorbent, the specific steps are as follows:

[0032] (1) Synthesis of amidoximated organosilane functionalization reagent (AOES)

[0033] Add 120 mg (3-cyanopropyl) triethoxysilane (CP-TES), 387.2 mg hydroxylamine (AO) and 275 mg Na 2 CO 3 , heated under reflux at 70°C for 12 hours, and purified by Soxhlet extraction to obtain an amidoximated organosilane functional reagent ((3-amidoximopropyl)triethoxysilane), the reaction formula is as follows:

[0034]

[0035] (2) Preparation of amidoxime mesoporous silica microsphere adsorbent (according to AOES / Na 2 SiO 3 Mass ratio 20wt.% implementation)

[0036] Take 60mL of absolute ethanol, 80mL of deionized water, 30mL of acetic acid solution (25wt.%) and 2.0mL of P123 and place them in a container and stir quickly; while stirring, add 50mL of sodium silicate solution (containing 10.0g of silicon NaOH) and 2.0g AOES were thoroughly mixed to obtain a mix...

Embodiment 3

[0039] A preparation method of amidoxime mesoporous silica microsphere adsorbent, the specific steps are as follows:

[0040] (1) Synthesis of amidoximated organosilane functionalization reagent (AOES)

[0041]Add 120 mg (3-cyanopropyl) triethoxysilane (CP-TES), 387.2 mg hydroxylamine (AO) and 275 mg Na 2 CO 3 , heated under reflux at 70°C for 12 hours, and purified by Soxhlet extraction to obtain amidoximated organosilane functionalization reagent ((3-amidoximopropyl)triethoxysilane), the reaction formula is as follows:

[0042]

[0043] (2) Preparation of amidoxime mesoporous silica microsphere adsorbent (according to AOES / Na 2 SiO 3 Mass ratio 30wt.% implementation)

[0044] Take 60mL of absolute ethanol, 80mL of deionized water, 30mL of acetic acid solution (25wt.%) and 2.0mL of P123 and place them in a container for rapid stirring and mixing. While stirring, add 50mL of sodium silicate solution (containing 10.0g of silicon NaOH) and 3.0g AOES were thoroughly mixed...

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Abstract

The invention provides an amidoximated mesoporous silica microsphere adsorbent. According to the invention, sodium silicate is used as a main raw material for synthesis of the adsorbent via a microwave hydrothermal method, and since sodium silicate is far cheaper than ethyl orthosilicate, production cost can be effectively reduced; reaction time can be substantially shortened to 12 to 18 h by using microwave hydrothermal synthesis, so production efficiency is enhanced; moreover, microwave hydrothermal synthesis can promote spontaneous nucleation and enables nucleation to be more uniform; furthermore, a functional group (an amidoxime group) is introduction via copolycondensation for modification of the adsorbent during microwave hydrothermal synthesis of the mesoporous silica microsphere adsorbent, so the prepared amidoximated mesoporous silica microsphere adsorbent has a well-developed ordered mesoporous structure and good mechanical strength and chemical stability, facilitates rapid entry of uranium into pore channels for adsorption and is applicable to separation and recovery of uranium in uranium-containing waste water.

Description

technical field [0001] The invention relates to the technical field of inorganic functional materials, in particular to an amidoximated mesoporous silica microsphere adsorbent and a preparation method thereof. Background technique [0002] The concentration of uranium in the uranium-containing wastewater generated during the production of uranium reaches the mg / L level. Using new adsorption materials to separate and enrich uranium from uranium-containing wastewater can not only effectively recover uranium resources in wastewater, but also reduce the discharge of uranium-containing wastewater environmental pollution; mesoporous silica microspheres not only have good chemical stability and radiation resistance, but also have high mechanical strength and large specific surface area, and their highly developed ordered pore structure facilitates the rapid adsorption of uranyl ions, so It is an ideal uranium adsorption material. The production of mesoporous silica microspheres us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30G21F9/12
Inventor 周利民
Owner EAST CHINA UNIV OF TECH
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