A kind of preparation and application method of cu(II) solid phase extractant based on carbon nanotubes

A solid-phase extraction agent, carbon nanotube technology, applied in chemical instruments and methods, water/sludge/sewage treatment, water pollutants, etc., can solve problems such as lack, achieve good adsorption selectivity, and wide pH range. , high adsorption selectivity and specificity

Inactive Publication Date: 2011-12-07
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, mature commercial products are still relatively lacking, so it is still of great significance to develop new efficient, simple and fast Cu(II) solid phase extraction materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 0.5-1 g of commercially available polycarboxylated carbon nanotubes (MC3, Chengdu Organic Chemistry Co., Ltd., Chinese Academy of Sciences) and 20 mL of thionyl chloride into a round-bottomed flask, stir and reflux at 60-90 °C for 1-2 days, and react After suction filtration, the filter residue was washed 3 times with anhydrous tetrahydrofuran, and then vacuum-dried overnight to obtain the acylated carbon nanotube product; Amine and 100mL of anhydrous N,N-dimethylformamide mixed solution, 100 ℃ under the protection of nitrogen, reflux reaction for 48h, after the reaction is complete, filter with suction, wash the filter residue with absolute ethanol 3 times, vacuum dry 1-2 Days, the final 2,2'-dipyridylamine modified carbon nanotube product is a Cu(II) solid phase extraction agent based on carbon nanotubes.

Embodiment 2

[0019] The solid-phase extraction agent that the enrichment lead ion of embodiment 1 gained is used carries out each index experiment

[0020] 1) Weigh 10 mg of Cu(II) solid-phase extractant product based on carbon nanotubes, add it to 10 mL of Cu(II) (1 mg / L) solution, fully shake under different pH conditions, and perform Cu(II) extraction. Adsorption experiment, the experiment proves that when the pH of the system is ≥ 4.5, the adsorption rate increases rapidly, reaching over 95%.

[0021] In order to achieve complete adsorption of Cu(II), pH=6 was selected as the pH condition for other experiments below.

[0022] 2) Select pH=6 as the system pH condition, 10mg Cu(II) solid phase extractant product, 10mL of the same Cu(II) ion solution (1mg / L) as 1), and carry out Cu(II) ion adsorption time test , the test shows that it only takes 5 minutes for the product to reach the adsorption saturation of Cu(II).

[0023] 3) By studying the adsorption amount change curve of the produ...

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Abstract

The invention relates to a preparation and application method of a Cu(II) solid-phase extraction agent based on carbon nanotubes. Firstly, reflux 0.5-1g of carboxylated carbon nanotubes and 20mL of anhydrous thionyl chloride at 60-90°C for 1-2 day, suction filtration, and the filter residue was washed with anhydrous tetrahydrofuran and vacuum-dried overnight to obtain acylated carbon nanotubes; the acylated carbon nanotubes were dispersed in 0.1g 2,2′-dipyridylamine, 3mL triethylamine and 100mL anhydrous In a mixed solution composed of N,N-dimethylformamide in water, under the protection of nitrogen, reflux at 100°C for 48 hours, filter with suction, wash the filter residue three times with absolute ethanol, and dry it in vacuum for 1-2 days to obtain carbon nanotube-based Cu(II) solid phase extractant. Measure 5-20 mg of Cu(II) solid-phase extraction agent and fill it in a 6mL solid-phase extraction column of a solid-phase extraction device, and perform dynamic Cu(II) extraction on water samples containing 1-5 μg / L Cu(II) Enrichment, use 5mL of 1 ~ 3M dilute nitric acid to elute and detach the solid phase extractant enriched with Cu(II), the recovery rate of Cu(II) reaches 97%, and the solid phase extractant of Cu(II) after detachment The phase extractant can be recycled 4 to 5 times.

Description

technical field [0001] The invention relates to a preparation and application method of a Cu(II) solid phase extraction agent based on carbon nanotubes, in particular to a solid phase for enriching trace heavy metal copper ions (Cu(II)) in environmental water bodies and liquid samples Preparation of extractant and its application method. The invention belongs to the technical field of separation, analysis and detection. Background technique [0002] Copper metal is an element that exists widely in nature. Due to its good physical and chemical properties, copper metal has a wide range of uses in industry, and with the development of science and technology, its application range is continuously expanding, which makes copper in the environment sustainable. increase, leading to copper pollution in the environment. [0003] Copper is extremely toxic to aquatic organisms. When the concentration of copper (Cu(ID) in water is 0.5mg / L, it can kill 35-100% of freshwater plants, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/30B01D15/08C02F1/28C02F1/62C02F101/20
Inventor 郜洪文胡张军刘姗贾江雁
Owner TONGJI UNIV
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