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A kind of microporous carboxylated silica gel, preparation method and application thereof

A carboxylation, silica gel technology, applied in chemical instruments and methods, inorganic chemistry, other chemical processes, etc., can solve the problems of difficulty in repeated use, poor adsorption capacity, etc., and achieve the effect of simple and easy operation.

Active Publication Date: 2021-05-04
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the problems existing in the above-mentioned prior art, the present invention provides a microporous carboxylated silica gel with a large specific surface area, which improves the adsorption selectivity, adsorption efficiency, and adsorption rate of silica gel for removing heavy metal pollution in water, and solves the problem of traditional silica gel for the adsorption of heavy metal pollution. Poor capacity, difficult to reuse the problem

Method used

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  • A kind of microporous carboxylated silica gel, preparation method and application thereof
  • A kind of microporous carboxylated silica gel, preparation method and application thereof
  • A kind of microporous carboxylated silica gel, preparation method and application thereof

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Embodiment 1

[0037] A kind of preparation method of microporous carboxylated silica gel, reacts according to following formula:

[0038]

[0039] Specifically include the following steps:

[0040] 1) Weigh 10g of inorganic silica gel mSiO 2 ·nH 2 O and 3mL of 3-aminopropyltriethoxysilane were dissolved in 100mL of toluene solvent, and stirred and refluxed in a reflux device for 16h under the condition of an oil bath at 110°C;

[0041] 2) After the reaction in step 1) is completed, the reaction product is cooled and filtered, and firstly adopts 150 mL of mass concentration to be 50% toluene solution for centrifugal cleaning, and then adopts 150 mL of mass concentration for 50% acetone solution for centrifugal cleaning, and then at 105° C. Dry for 4 hours;

[0042] 3) Weigh 3.35g of nitrilotriacetic acid and 4.05g of the reaction product obtained in step 2), dissolve in 400mL of pyridine solvent, and stir under reflux for 3h in an oil bath at 90°C;

[0043] 4) After the reaction in st...

Embodiment 2

[0057] A preparation method of microporous carboxylated silica gel, specifically comprising the following steps:

[0058] 1) Weigh 5g of inorganic silica gel mSiO with different specific surface areas 2 ·nH 2 O and 1.5mL of silane coupling agent 3-aminopropyltriethoxysilane containing different chemical groups were dissolved in 80mL of toluene solvent, and stirred and refluxed in a reflux device for 10h under the condition of an oil bath at 100°C;

[0059] 2) After the reaction in step 1) is finished, the reaction product is cooled and filtered, and firstly adopt 120mL mass concentration of 2% toluene solution for centrifugal cleaning, then adopt 120mL mass concentration of 2% acetone solution for centrifugal cleaning, and then place the reaction product at 100°C Dry for 3 hours;

[0060] 3) Weigh 2.5 g of nitrilotriacetic acid and 3.5 g of the reaction product obtained in step 2), dissolve it in 250 mL of pyridine solvent, and stir under reflux for 1 h under the condition o...

Embodiment 3

[0066] A preparation method of microporous carboxylated silica gel, specifically comprising the following steps:

[0067] 1) Weigh 15g of inorganic silica gel mSiO with different specific surface areas 2 ·nH 2 O and 5mL of silane coupling agent 3-aminopropyltriethoxysilane containing different chemical groups were dissolved in 120mL of toluene solvent, and stirred and refluxed in a reflux device for 20h under the condition of an oil bath at 120°C;

[0068] 2) After the reaction in step 1) is finished, the reaction product is cooled and filtered, and the toluene solution with a mass concentration of 180 mL of 99% is used for centrifugal cleaning, and then the acetone solution with a mass concentration of 180 mL for 99% is used for centrifugal cleaning, and then at 110° C. Dry for 5 hours;

[0069] 3) Weigh 5g of nitrilotriacetic acid and 5g of the reaction product obtained in step 2), dissolve in 450mL of pyridine solvent, and stir under reflux for 5h in an oil bath at 100°C;...

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Abstract

The invention discloses a microporous carboxylated silica gel, a preparation method and application thereof, and belongs to the technical field of modified silica gel. The microporous carboxylated silica gel has a porous structure and its specific surface area is 335-350m 2 / g, and the pore size is 1.05-1.25nm; the microporous carboxylated silica gel is first aminated with inorganic silica gel, then surface modified with nitrilotriacetic acid, and combined with aminocarboxamide. The present invention adopts silica gel as material, first amination, and then carry out nitrilotriacetic acid surface modification; Used raw material is cheap and easy to get, and makes cheap and efficient silica gel adsorbent, is used for the treatment of heavy metal ions (such as lead, copper, cadmium, etc.) in waste water ), not only the method is simple and easy to operate, but also can be recycled and reused; the heavy metals in the water environment can be adsorbed and removed within 2 minutes at the fastest, and the adsorption efficiency can reach more than 80%.

Description

technical field [0001] The invention relates to a microporous carboxylated silica gel, a preparation method and an application thereof, belonging to the technical field of modified silica gel. Background technique [0002] Heavy metal pollution is a prominent problem in the field of water environment pollution. The accumulation of heavy metals lead, copper, and cadmium in the environment directly or indirectly affects the healthy growth and life of the earth's organisms, such as lead, cadmium, etc. may cause damage to the lungs, kidneys, liver, and reproductive organs. Due to their high toxicity and non-biodegradability, it is extremely urgent to find effective ways to remove heavy metal pollution in water environment. [0003] At present, various treatment technologies have been applied to remove toxic heavy metal pollution in water, such as ion exchange, filtration / chemical deposition, solvent extraction, adsorption, etc. Although most methods have been used, adsorption ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/20
CPCB01J20/22B01J20/28061B01J20/2808C02F1/285C02F2101/20
Inventor 孔令涛李玉莲刘锦淮
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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