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Phosphoric acid modified silicon dioxide microspheres as well as preparation method and application thereof

A silica and microsphere technology, applied in the field of water treatment, can solve the problems of low chemical and thermal stability, poor recycling performance, slow adsorption kinetics, etc., and achieve the effects of simple preparation method, few steps, and efficient synthesis

Pending Publication Date: 2022-08-02
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional adsorption materials usually have several problems: (I) low chemical and thermal stability; (II) low adsorption capacity; (III) relatively slow adsorption kinetics and relatively poor selectivity; (IV) reusable performance poor
Although MOFs and COFs have adjustable pores and large specific surface area, they have certain application prospects in the removal of oxoacid ions, but the synthesis cost is high and it is difficult to prepare on a large scale.
Although metal oxides can interact with a variety of oxoacid ions, their selectivity is relatively poor

Method used

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  • Phosphoric acid modified silicon dioxide microspheres as well as preparation method and application thereof
  • Phosphoric acid modified silicon dioxide microspheres as well as preparation method and application thereof
  • Phosphoric acid modified silicon dioxide microspheres as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1 Preparation of phosphoric acid modified silica microsphere material

[0047] 1) Disperse 6.2 g of silica microspheres in 70 mL of anhydrous toluene under the action of ultrasound, add 4 mL of 3-aminopropyltrimethoxysilane dropwise, and reflux the final mixture in an oil bath at 103 °C for 24 h, take out the The silica microspheres were washed with absolute ethanol, and then dried in a vacuum drying oven at 80 °C for 24 h to obtain 3-aminopropyl-functionalized silica microspheres (SiO 2 @NH 2 );

[0048] 2) Take 2g SiO 2 @NH 2 It was dispersed into 70 mL of acetonitrile under the action of ultrasound, and then 16 mL of triethylamine was added, and then 6 mL of phosphorus oxychloride was slowly added dropwise to it, and the reaction was carried out in an oil bath at 40 °C for 24 h. Then it was dried in a vacuum drying oven at 80°C for 24 hours to obtain phosphoric acid modified silica microspheres (SiO 2 @NH 2 @H 2 PO 3 ).

Embodiment 2

[0049] Example 2 Preparation of phosphoric acid modified silica microsphere material

[0050] 1) Disperse 5 g of silica microspheres in 30 mL of anhydrous toluene under the action of ultrasound, add 4 mL of 3-aminopropyltrimethoxysilane dropwise, and reflux the final mixture in an oil bath at 103 °C for 24 h, take out the dioxide The silicon microspheres were washed with absolute ethanol, and then dried in a vacuum drying oven at 80 °C for 24 h to obtain 3-aminopropyl functionalized silica microspheres (SiO 2 @NH 2 );

[0051] 2) Take 1g SiO 2 @NH 2 Disperse into 30 mL of acetonitrile under the action of ultrasound, then add 16 mL of triethylamine, then slowly dropwise add 6 mL of phosphorus oxychloride to it, react in an oil bath at 40 °C for 24 h, and wash the product with acetonitrile, water, and anhydrous ethanol in turn, Then it was dried in a vacuum drying oven at 80°C for 24 hours to obtain phosphoric acid modified silica microspheres (SiO 2 @NH 2 @H 2 PO 3 ). ...

Embodiment 3

[0052] Example 3 Preparation of phosphoric acid modified silica microsphere material

[0053] 1) Disperse 10 g of silica microspheres in 100 mL of anhydrous toluene under the action of ultrasound, add 4 mL of 3-aminopropyltrimethoxysilane dropwise, and reflux the final mixture in an oil bath at 103 °C for 24 hours, take out the dioxide The silicon microspheres were washed with absolute ethanol, and then dried in a vacuum drying oven at 80 °C for 24 h to obtain 3-aminopropyl functionalized silica microspheres (SiO 2 @NH 2 );

[0054] 2) Take 2g SiO 2 @NH 2 Disperse into 50 mL of acetonitrile under the action of ultrasound, then add 16 mL of triethylamine, and then slowly add 6 mL of phosphorus oxychloride dropwise to it, react in an oil bath at 40 °C for 24 h, and wash the product with acetonitrile, water, and absolute ethanol in turn. Then it was dried in a vacuum drying oven at 80°C for 24 hours to obtain phosphoric acid modified silica microspheres (SiO 2 @NH 2 @H 2 P...

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Abstract

The invention relates to phosphoric acid modified silicon dioxide microspheres as well as a preparation method and application thereof. During preparation, firstly, 3-aminopropyl is introduced to the surfaces of the silicon dioxide microspheres, then phosphoric acid is grafted to the surfaces of the 3-aminopropyl functionalized silicon dioxide microspheres, and the silicon dioxide microsphere material with the surface modified with phosphoric acid is prepared. The material is simple in preparation process and mild in reaction condition, and is successfully applied to removal of oxyacid radical ion pollutants in water.

Description

technical field [0001] The invention belongs to the field of water treatment, in particular to a phosphoric acid modified silica microsphere and a preparation method thereof, and its application in the adsorption of oxyacid ions in water. Background technique [0002] Water pollution is a major global problem, causing serious harm to health and the environment. The U.S. Environmental Protection Agency considers some inorganic pollutants, especially oxoacid ions, as pollutants that require priority control among inorganic pollutants in water (Reference 1. Keith et.al "ES&T Special Report: Priority pollutants: I-aperspective" view", "Environmental Science & Technology" 1979, 13, (4), 416-423. Literature 2. Mon et.al "Metal-organic framework technologies for water remediation: towards a sustainable ecosystem", "Journal of Materials Chemistry A" 2018 , 6, (12), 4912-4947.). [0003] Industrial wastewater contaminated with oxoacid ions, such as CrO 4 2- / Cr 2 O 7 2- and HA...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/10C02F101/22
CPCB01J20/22B01J20/28021B01J20/3085C02F1/281C02F2101/10C02F2101/22Y02W10/37
Inventor 黄光梁世琪李磊
Owner NANJING MEDICAL UNIV
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