Preparation method of nitrogen-doped graphene quantum dot hybrid membrane for selective adsorption of copper ions from mixed metal solutions

A technology of mixing metal and copper ions, applied in graphene, chemical instruments and methods, adsorbed water/sewage treatment, etc., can solve the problems of difficult separation and classification of heavy metal ions, few cycles of use, limited application value, etc., to eliminate metal ions. The effect of ion pollution, simple operation, easy recycling and reuse

Active Publication Date: 2022-06-24
HEFEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The obtained adsorption material has good adsorption properties to methylene blue, but it has no adsorption property to heavy metal ions, so it is difficult to separate and classify heavy metal ions in wastewater, and its application value is limited.
[0004] Chinese patent 201911173039.2 proposes a method for preparing a hybrid membrane for selective separation of copper from mixed metal solutions. The hybrid precursor is prepared by sol-gel reaction of graphene oxide and silane coupling agent KH-792 , the obtained hybrid precursor is added to polyvinyl alcohol aqueous solution for reaction, and the obtained material is left to stand for degassing to obtain a coating liquid, and then the film is coated to obtain a hybrid film, which is used to select from mixed metal ion solutions can effectively separate copper ions; however, the hybrid film is 2+ The amount of adsorption is small, and the number of cycles is less (the [0047] paragraph of the specification, embodiment 2, the adsorption amount of the hybrid membrane B is the largest, and it has the greatest effect on Cu 2+ The adsorption capacity can reach about 3.5mg / g), therefore, the application value is limited
[0005] There are no related invention patents and literature reports on nitrogen-doped graphene quantum dot hybrid membranes for preferential adsorption and removal of copper ions from mixed metal solutions

Method used

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  • Preparation method of nitrogen-doped graphene quantum dot hybrid membrane for selective adsorption of copper ions from mixed metal solutions
  • Preparation method of nitrogen-doped graphene quantum dot hybrid membrane for selective adsorption of copper ions from mixed metal solutions
  • Preparation method of nitrogen-doped graphene quantum dot hybrid membrane for selective adsorption of copper ions from mixed metal solutions

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Experimental program
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Effect test

Embodiment 1

[0036] Preparation of nitrogen-doped graphene quantum dots (N-GQDs) precursors:

[0037] With the molar ratio of citric acid (carbon source) and urea (nitrogen source) as 1:3, 0.21 g (1 mmol) of citric acid and 0.18 g (3 mmol) of urea were dissolved in 5 mL of water, and stirred to obtain a clear solution. It was placed in a polytetrafluoroethylene-lined reaction kettle, heated to 160° C., and kept for 4 h. The reaction solution was cooled to room temperature in the reactor, opened the solution in the reactor, and the solution was a clear yellow solution (such as figure 1 (a) shown on the left). As a zero-dimensional material, graphene quantum dots, in addition to having abundant edge effects, exhibit bright blue fluorescence under UV light at 365 nm.

[0038] In order to further confirm that the clear yellow solution taken out from the reaction kettle is the N-GQDs precursor, the clear yellow solution is detected by ultraviolet absorption spectrum, and the maximum ultraviol...

Embodiment 2

[0043] At room temperature, take a certain amount of N-GQDs precursor powder prepared in Example 1, add 10 mL of water, stir for 10 min, until the N-GQDs precursor powder is completely dissolved, then add PVA (5wt%) solution, and stir at room temperature for 1 h , and then add glutaraldehyde, ethyl orthosilicate and silane coupling agent WD-51 with a concentration of 25% by mass respectively under stirring conditions, and continue stirring for 4 hours to obtain a solution. The solution was placed in an ultrasonic cleaner, sonicated at 100KHz for 20 min to remove air bubbles in the solution, and allowed to stand for 12 h to obtain a film-forming liquid. The support PTFE sheet was separated, and then the membrane was dried at 40 °C for 12 h, and the N-GQDs hybrid membrane without support was obtained after cooling.

[0044] The content of N-GQDs precursor, glutaraldehyde, WD-51, TEOS and other raw materials in the hybrid membrane was changed, and the effect of the composition of...

Embodiment 3

[0050] According to the experimental results of Example 2, it can be seen that the addition amount of the N-GQDs precursor powder and the addition amount of the silane coupling agent WD-51 have the greatest influence on the performance of the N-GQDs hybrid film. Among them, it is suitable that the amount of N-GQDs precursor powder added does not exceed 0.5 g, and the amount of silane coupling agent WD-51 added is suitable in the range of 0.2 to 0.5 mL. Accordingly, by optimizing the ratio of raw materials (see Table 2), a series of N-GQDs hybrid membranes for adsorption and separation of metal ions from mixed metal solutions were prepared, which were marked as hybrid membranes A to G, respectively. Among them, the addition amount of N-GQDs precursor powder in A-D hybrid films increases sequentially, and the addition amount of silane coupling agent WD-51 in E-G hybrid films increases sequentially.

[0051] Table 2. Raw material ratio table of N-GQDs hybrid membrane A~G

[0052...

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Abstract

The invention discloses a method for preparing a nitrogen-doped graphene quantum dot hybrid film for selectively adsorbing copper ions from a mixed metal solution. Firstly, nitrogen-doped graphene quantum dot N-GQDs precursor and silane WD ‑51. The sol‑gel reaction between tetraethyl orthosilicates prepares a hybrid precursor solution, which is then added to an aqueous solution of polyvinyl alcohol for reaction. After standing for defoaming, a coating solution is obtained. The coating solution Coating a film on the support body to obtain a diaphragm; the coating solution can also be dissolved in a solvent first, and then coated to obtain a diaphragm, and after drying, a nitrogen-doped graphene that can be used to selectively adsorb copper ions from a mixed metal solution can be obtained Quantum dot hybrid membrane, which can be supported or not supported; it has selective adsorption for copper ions in a variety of mixed metal ion solutions, and membrane adsorption can be used to preferentially remove copper in mixed metal ion solutions Ions can be used for fractional separation of copper ions in wastewater containing various metal ions.

Description

technical field [0001] The invention belongs to the technical field of heavy metal wastewater treatment, in particular to the preparation of a nitrogen-doped graphene quantum dot hybrid membrane for selectively adsorbing copper ions from a mixed metal solution by utilizing a hydrothermal synthesis method and a sol-gel reaction. Background technique [0002] Heavy metal wastewater pollution has attracted more and more attention. How to remove heavy metal ions in wastewater and eliminate its harm is a key technical problem in the field of wastewater treatment. Therefore, it is more and more urgent to develop new separation technologies. [0003] Chinese patent 201610260866.5 proposes a method for preparing a chitosan-modified graphene oxide quantum dot adsorption material. The method is to add a crosslinking agent and graphene oxide quantum dots to an acetic acid solution of chitosan, and at a certain pH, Magnetic stirring and mixing at a certain temperature, followed by repe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184B01J20/30B01J20/20C02F1/28C02F101/20
CPCC01B32/184B01J20/205B01J20/0259C02F1/281C02F2101/20
Inventor 刘俊生庞博文王凤侠
Owner HEFEI UNIV
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