Compound grapheme absorption agent, method for preparing compound grapheme absorption agent and application of compound grapheme absorption agent

A technology of graphene and adsorbent, which is applied in the field of composite graphene adsorbent and its preparation, can solve the problems of restricting the application of pollutant removal, reducing the specific surface area of graphene, and less application of graphene materials, so as to improve the dispersion and The effect of hydrophilicity, low cost of treatment process, and easy control of conditions

Inactive Publication Date: 2014-01-01

SOUTH CHINA UNIV OF TECH

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AI-Extracted Technical Summary

Problems solved by technology

However, graphene materials have fewer applications in the environment

Studies have shown that graphene can remove pollutants such as organic pollutants, but the agglomeration of graphene n...

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Abstract

The invention discloses a compound grapheme absorption agent which comprises grapheme, nanometer zero-valent iron and cetyl trimethyl ammonium bromide. The invention further discloses a method for preparing the compound grapheme absorption agent. The method for preparing the compound grapheme absorption agent includes the following steps that firstly, oxidized grapheme is dispersed in water with ultrasonic waves and oxidized grapheme suspension liquid is obtained; secondly, the nanometer zero-valent iron and the cetyl trimethyl ammonium bromide are added into the oxidized grapheme suspension liquid obtained in the first step, fully stirred and fully reacted and a reaction solution is obtained; thirdly, the reaction solution obtained in the second step is added with reductive agents and fully reacted and black flocks are obtained; fourthly, the black flocks obtained in the third step are filtered, washed and dried to obtain the compound grapheme absorption agent. The compound grapheme absorption agent is efficient, green, economic, friendly to environment, and suitable for large-scale production. The preparing method is simple and conditions are easy to control.

Application Domain

Other chemical processesWater/sewage treatment by sorption

Technology Topic

Cvd grapheneGraphite oxide +5

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Examples

Experimental program(3)
Effect test(1)

Example Embodiment

[0041] Example 1

[0042] The preparation method of the composite graphene adsorbent of this embodiment includes the following steps:

[0043] (1) Disperse graphene oxide in water, and obtain a graphene oxide suspension with a concentration of 4mg/mL after 30 minutes of ultrasonic dispersion;

[0044] The graphene oxide in this example was synthesized by the modified Hummers method. The specific steps are as follows: slowly add 10g graphite and 5g sodium nitrate into a flask containing 230ml concentrated sulfuric acid, and stir in a mixture of ice and water. After 30 minutes, slowly add 30g Potassium permanganate, during the stirring process, control the reaction temperature to always be less than 15°C and keep it for 90min; transfer the reaction system to a constant temperature water bath at 35°C, keep the reaction temperature at 35°C, and stir for 30min; add 460mL to the reaction system Deionized water, the reaction temperature is controlled at 80℃~95℃, the stirring time is 30min; then add 100mL, 30% hydrogen peroxide solution, after the solution turns bright yellow, filter while hot, and use 500mL of 5% hydrochloric acid Wash the solution with 1400mL deionized water for three times until the solution is free of sulfate ions (use barium chloride solution for detection). Dry the obtained sample in a vacuum freeze dryer at 50°C for 48 hours to constant weight to obtain graphene oxide. The microstructure is shown in figure 1.

[0045] (2) Add nano zero valent iron and cetyl trimethyl ammonium bromide to the graphene oxide suspension obtained in step (1); among them, nano zero valent iron, graphene oxide and cetyl trimethyl ammonium bromide The mass ratio of ammonium bromide is 1:2:7, fully stirred, reacted at 55°C for 3h, and the reaction solution is obtained after complete reaction;

[0046] The synthesis method of nano zero-valent iron in this embodiment is as follows:

[0047] 11.12g FeSO at room temperature 4 ·7H 2 O is dissolved in 200mL ethanol aqueous solution (ethanol:water=3:7). As for a 1000mL three-necked flask, under nitrogen protection and mechanical stirring, quickly add 200mL potassium borohydride solution with a concentration of 0.12mol/L to FeSO 4 In the solution, continue to stir and react for 30 minutes. After standing for 5 minutes, vacuum filter, wash several times with ultrapure water and absolute ethanol, and vacuum dry to constant weight to obtain nano-zero-valent iron. Its microstructure is shown in figure 2.

[0048] (3) Heat the reaction solution obtained in step (2) to 80°C, add the reducing agent sodium borohydride, and obtain a black flocculent precipitate after full reaction; the quality of the reducing agent is 10 times that of the graphene oxide;

[0049] (4) The black flocculent precipitate obtained in step (3) is suction filtered, washed and dried to obtain a composite graphene adsorbent.

[0050] The microstructure of the composite graphene adsorbent obtained in this example is as image 3 Shown, with figure 1 Compared with agglomerated graphene, image 3 The graphene becomes thinner, showing a lamellar structure, and the lamellar spacing increases. This may be attributed to the introduction of cetyltrimethylammonium bromide, and from image 3 It can be clearly seen that the nano-zero-valent iron particles are uniformly attached to the graphene surface or sheet.

[0051] Figure 4 It is a schematic diagram of Fourier transform infrared comparison between graphene and the composite graphene adsorbent prepared in this embodiment. The composite graphene adsorbent prepared in this example is at 2918 cm -1 and2849cm -1 The methylene and methyl C-H stretching vibrations appeared in the band of, which proved that the composite graphene adsorbent contained cetyltrimethylammonium bromide; the composite graphene adsorbent was at 1643cm -1 There is a carbonyl stretching vibration in the band of 3201cm -1 The stretching vibration of the intermolecular O-H bond appeared in the band of, which proves that the composite graphene adsorbent contains nano-zero-valent iron. The functional groups on the surface of graphene are mainly distributed on the edge or surface. The functional groups in the nano-zero-valent iron are combined with the functional groups on the graphene surface, so that the nano-zero-valent iron is inserted or embedded in the edge or surface of the layered graphene through chemical bonds.

[0052] Figure 5 It is the thermogravimetric curve of graphene and the composite graphene adsorbent prepared in Example 1. It can be seen from the figure that the composite graphene adsorbent prepared in this embodiment contains about 56% of graphene, about 10% of nano-zero-valent iron, and about 14% of the cationic surfactant cetyltrimethyl by mass percentage. Ammonium bromide and about 20% impurities.

Example Embodiment

[0053] Example 2

[0054] The preparation method of the composite graphene adsorbent of this embodiment includes the following steps:

[0055] (1) Disperse graphene oxide in water, and obtain a graphene oxide suspension with a concentration of 6 mg/mL after 60 minutes of ultrasonic dispersion;

[0056] (2) Add nano zero-valent iron and cetyl trimethyl ammonium bromide to the graphene oxide suspension obtained in step (1); among them, nano zero-valent iron, graphene oxide and cetyl trimethyl ammonium bromide The mass ratio of base ammonium bromide is 1:2:9, fully stirred, react at 50°C for 5 hours, and obtain a reaction solution after complete reaction;

[0057] (3) Heat the reaction solution obtained in step (2) to 85°C, add the reducing agent potassium borohydride, and obtain a black flocculent precipitate after full reaction; the quality of the reducing agent is 9 times that of the graphene oxide;

[0058] (4) The black flocculent precipitate obtained after step (3) is suction filtered, washed and dried to obtain a composite graphene adsorbent.

[0059] The microstructure and infrared spectrum analysis results of the composite graphene adsorbent prepared in this example are similar to those of Example 1.

Example Embodiment

[0060] Example 3

[0061] The preparation method of the composite graphene adsorbent of this embodiment includes the following steps:

[0062] (1) Disperse graphene oxide in water, and obtain a graphene oxide suspension with a concentration of 5 mg/mL after 40 minutes of ultrasonic dispersion;

[0063] (2) Add nano zero-valent iron and cetyl trimethyl ammonium bromide to the graphene oxide suspension obtained in step (1); among them, nano zero-valent iron, graphene oxide and cetyl trimethyl ammonium bromide The mass ratio of ammonium bromide is 1:2:8, fully stirred, and reacted at 52°C for 4 hours, and the reaction solution is obtained after complete reaction;

[0064] (3) Heat the reaction solution obtained in step (2) to 82°C, add the reducing agent sodium borohydride, and obtain a black flocculent precipitate after full reaction; the total mass of the reducing agent is 11 times the mass of graphene oxide;

[0065] (4) The black flocculent precipitate obtained after step (3) is suction filtered, washed and dried to obtain a composite graphene adsorbent.

[0066] The microstructure and infrared spectrum analysis results of the composite graphene adsorbent prepared in this example are similar to those of Example 1.

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Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Reduce reunion
High specific surface area

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Improve adsorption performance Raw materials are easy to obtain Low cost of preparation Simple preparation process Conditions are easy to control Sorbent Ferric Reducing agent

Compound grapheme absorption agent, method for preparing compound grapheme absorption agent and application of compound grapheme absorption agent

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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