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Preparing method of dithiocarbamic acid-based functionalized carbon nano tube

A technology of dithiocarbamic acid and carbon nanotubes, applied in the field of nanomaterials, can solve the problems of easy aggregation of carbon nanotubes, insufficient mechanical strength, and low specific surface area, and achieve good adsorption effect, good mechanical strength, and large specific surface area Effect

Inactive Publication Date: 2017-04-26
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of dithiocarbamate functionalized carbon nanotubes, so as to overcome the easy aggregation of carbon nanotubes, insufficient mechanical strength of organic dithiocarbamic acid modified materials, low specific surface area and poor stability Shortcomings

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  • Preparing method of dithiocarbamic acid-based functionalized carbon nano tube

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Embodiment 1

[0027] A method for preparing dithiocarbamate-based functionalized carbon nanotubes includes the following steps:

[0028] (1) Take 10 parts of multi-walled carbon nanotubes in a flask, add 1000 parts of mixed acid, where the mixed acid is made by mixing a 98% sulfuric acid solution with a mass concentration of 50% nitric acid solution, and the volume ratio is 3:1. The reaction was carried out at 80° C. for 3 hours under stirring. After the reaction was completed, the reaction was cooled, diluted with water, vacuum filtered, washed, and vacuum dried at 80° C. for 12 hours to obtain acid-treated carbon nanotubes.

[0029] (2) Take 10 parts of the above-mentioned acid-treated carbon nanotubes and disperse them in 1000 parts of organic solvent N,N-dimethylformamide (DMF), and add 500 parts of thionyl chloride (SOCl 2 ), and then turn on the temperature controller, make the reaction system reflux at 80° C. for 5 hours to remove the residual thionyl chloride. Add 100 parts of polyethyl...

Embodiment 2

[0032] A method for preparing dithiocarbamate-based functionalized carbon nanotubes includes the following steps:

[0033] (1) Take 10 parts of multi-walled carbon nanotubes in a flask, add 500 parts of mixed acid, where the mixed acid is made by mixing 80% sulfuric acid solution with mass concentration and 50% nitric acid solution with mass concentration, and the volume ratio is 3:1, react at 90°C for 5 hours with stirring, cool after the reaction, dilute with water, vacuum filter, wash, and dry at 50°C for 12 hours to obtain acid-treated carbon nanotubes.

[0034] (2) Take 10 parts of the above-mentioned acid-treated carbon nanotubes, disperse them in 500 parts of organic solvent N,N-dimethylformamide (DMF), and add 50 parts of thionyl chloride (SOCl 2 ), and then turn on the temperature controller to make the reaction system reflux at 65°C for 5 hours to remove the residual thionyl chloride. Add 50 parts of ethylenediamine to the above reaction system, reflux at 70°C for 3h, vac...

Embodiment 3

[0037] A method for preparing dithiocarbamate-based functionalized carbon nanotubes includes the following steps:

[0038] (1) Take 10 parts of multi-walled carbon nanotubes in a flask and add 700 parts of mixed acid, where the mixed acid is made by mixing a sulfuric acid solution with a mass concentration of 90% and a nitric acid solution with a mass concentration of 60%, and the volume ratio is 3:1, react at 80°C under stirring for 4h, cool after the reaction, dilute with water, vacuum filter, wash, and dry under vacuum at 60°C for 12h to obtain acid-treated carbon nanotubes.

[0039] (2) Take 10 parts of the above acid-treated carbon nanotubes and disperse them in 700 parts of organic solvent N,N’-dimethylacetamide DMAC, add 200 parts of thionyl chloride (SOCl 2 ), and then turn on the temperature controller, and make the reaction system reflux at 70°C for 3 hours to remove the residual thionyl chloride. Add 80 parts of cyclohexylamine to the above reaction system, reflux at 80°...

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Abstract

The invention discloses a preparing method of a dithiocarbamic acid-based functionalized carbon nano tube. The preparing method comprises the first step of conducting hybrid reaction between the carbon nano tube and mixed acid, and then drying the mixture to obtain acid-treated carbon nano tube; the second step of putting the acid-treated carbon nano tube into an organic solvent, adding thionyl chloride into the solvent, conducting backflow for 1-5 h under the condition that the temperature is 65-80 DEG C, then adding amine into the solvent, conducting the backflow for 3-10 h under the condition that the temperature is 60-90 DEG C, and then drying the mixture to obtain an amination carbon nano tube; the third step of adding the amination carbon nano tube into a sodium hydroxide solution, and then adding carbon disulfide into the sodium hydroxide solution to be subjected to reaction to obtain the dithiocarbamic acid-based functionalized carbon nano tube. According to the preparing method, the dithiocarbamic acid-based functionalized carbon nano tube prepared through the preparing method has good dispersibility in a water system, a contact area between the carbon nano tube and pollutant heavy metals is increased, the surface of the carbon nano tube contains a large number of activated functional groups at the same time, the advantages of the carbon nano tube can be given play to the maximum, and the adsorptive property of the carbon nano tube is improved.

Description

Technical field [0001] The invention relates to the field of nanomaterials, in particular to a method for preparing dithiocarbamate-based functionalized carbon nanotubes. Background technique [0002] There are a lot of trace heavy metal ions in the water, such as: Cu 2+ , Zn 2+ , Pb 2+ , Cd 2+ , Co 2+ , Hg 2+ , Cr 6+ Etc., these heavy metal ions have always been a focus of attention because they have toxic effects on aquatic plants, animals, humans and the environment. Wastewater discharged from many factories, especially electroplating plants, contains one or more toxic heavy metal ions. It is necessary to remove these heavy metal ions from the waste water before discharging the waste water into the environment. With the advancement of science and technology, the emergence of many new materials has promoted the rapid development of water treatment technology. Among them, nanomaterials are becoming more and more popular in water treatment due to their superior properties and per...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/174B01J20/22
CPCB01J20/22B01J20/205B01J2220/46B01J2220/4806B01J2220/4812
Inventor 葛圆圆李志礼熊飘
Owner GUANGXI UNIV
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