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Thiol-functional carbon nano tube (CNT) and preparation method and application thereof

A technology of carbon nanotubes and functionalization, which is applied in the field of preparation of mercapto-functionalized carbon nanotubes, can solve the problems of destroying the surface characteristics of gold electrodes, low economic benefits, cumbersome steps, etc., achieve saving of reagents, simple equipment requirements, and easy preparation The effect of process safety

Inactive Publication Date: 2015-02-18
HUNAN UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

However, there are two problems now: (1) In the application of bare gold electrodes, mercury and gold will form unwanted gold amalgam, and gold amalgam will destroy the surface characteristics of gold electrodes
(2) Gold-based electrodes are often affected by the interference of some surface active compounds and metal ions
Jiali Wei et al. first prepared carbon nanotubes modified with diphenyl disulfide polymer layers with 4,4'-diaminodiphenyl disulfide, and then reduced them with sodium borohydride to obtain mercapto-functionalized carbon nanotubes. Through two steps Sulfhydryl-functionalized carbon nanotubes have been prepared for the detection of mercury ions, but this method has cumbersome steps, low economic benefits, and low yields (Jiali Wei, Duangguang Yang, Hongbiao Chen, Yong Gao, Huaming Li. Stripping voltammetric determination of mercury (II) based on SWCNT-PhSH modified gold electrode. Sensors and Actuators B: Chemical. 2014, 190: 968-974.)

Method used

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  • Thiol-functional carbon nano tube (CNT) and preparation method and application thereof
  • Thiol-functional carbon nano tube (CNT) and preparation method and application thereof
  • Thiol-functional carbon nano tube (CNT) and preparation method and application thereof

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Embodiment 1

[0028] The required carbon nanotubes should be dried at 70°C for 24 h in advance, weigh 0.6 g of 4-aminothiophenol into a three-necked flask, add 15 mL, 1 N, HCl solution, and heat slowly under stirring To 53°C, the flask was removed to cool. Weigh 0.828 g of sodium nitrite and dissolve it in 20 mL of deionized water, add the solution into a three-necked flask under continuous stirring, and dissolve carbon nanotubes and 0.3 g of sodium dodecyl sulfate in 30 mL of deionized water , sonicated for 45 min, the solution was added to the flask, and reacted overnight under ice bath and continuous stirring. The solution obtained by the reaction was washed sequentially with acetone, ethanol and a large amount of deionized water until neutral, and dried in vacuum to obtain thiol-functionalized carbon nanotubes (CNT-Ph-SH).

Embodiment 2

[0030] Weigh 5 mg of mercapto-functionalized carbon nanotubes into 5 mL of DMF solution, ultrasonically disperse for 40 min, and centrifuge at a speed of 5000 r / min for 15 min to separate the upper layer of black carbon nanotube dispersion. Grinding and polishing with alumina powder of 1.0, 0.3, 0.05 μm, ultrasonication in deionized water for 5 min, activation in sulfuric acid solution, drying the gold electrode with nitrogen, and immersing in the DMF dispersion of mercapto-functionalized carbon nanotubes for 20 h, the electrode was taken out and dried with nitrogen to obtain a gold electrode modified with mercapto-functionalized carbon nanotubes.

[0031] The adsorption of mercury ions (Hg(II)) We used a three-electrode system for electrochemical adsorption. The gold electrode modified with sulfhydryl-functionalized carbon nanotubes was placed in a solution containing 50 nM Hg(II). Collect for 15 minutes, then transfer the electrode to 0.1M HCl solution and reduce it at -0.1V...

Embodiment 3

[0033]Take 50 mg of mercapto-functionalized carbon nanotubes and put them into 25 mL of mercuric nitrate solution with an initial concentration of 760 mg / L and stir and adsorb for 72 hours. ) content was titrated and tested, and the experiment showed that the adsorption capacity was 330 mg / g.

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Abstract

The invention discloses a preparation method and application of a thiol-functional carbon nano tube (CNT). The thiol-functional CNT is successfully prepared by adopting a one-step method, has the characteristics of simple steps, short reaction time, high grafting rate and the like, is good in performance and wide in application and can serve as a mercury ion adsorbent, and the measured maximum adsorption amount is 2300mg / g, namely 2.3g of mercury can be adsorbed by 1g of adsorbent. The thiol-functional CNT also can serve as an electrochemical sensor for measuring the mercury ion concentration in sewage. Experiments prove that the detection limit of a modified electrode on mercury ions Hg (II) is 3.0nM (S / N=3), the linear range is 5-90nM, the CNT can be used for detecting Hg (II) in an actual water sample, and the recovery rate is in a range from 90 percent to 95 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical separation and chemical detection, and specifically relates to a preparation method and application of a mercapto-functionalized carbon nanotube. Background technique [0002] Mercury and its compounds have a significant impact on environmental quality and human health. Even a small amount of intake can cause acute or chronic damage to the human body, and its toxic effects include damage to the brain, kidneys, and lungs of the human body. In addition, mercury poisoning can lead to diseases including extremity pain, Hunter-Russell syndrome, and Minamata disease due to the high reactivity of mercury with selenium, an important nutrient component of 25 different selenium-containing enzymes. several diseases. Therefore, the search for new methods for the detection of mercury at a non-hazardous level is one of the most attractive topics today due to its practical applicability. Traditionally, mercu...

Claims

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Application Information

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IPC IPC(8): G01N27/333G01N27/26
Inventor 欧宝立何聪刘俊成
Owner HUNAN UNIV OF SCI & TECH
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