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Preparation method of graphene oxide and magnetic mesoporous silica composite material capable of adsorbing pollutants in water

A technology of mesoporous silica and composite materials, which is applied in the fields of adsorption water/sewage treatment, alkali metal oxides/hydroxides, chemical instruments and methods, etc. Low cost of raw materials and efficient adsorption

Inactive Publication Date: 2013-12-11
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method is basically to develop an adsorption material or adsorption technology for a single pollutant. People have also made some attempts in the simultaneous adsorption of two or more pollutants [Wang X.K., et al., Environ. Sci. Technol., 2011, 45, 3621-3627], but there are pollutants competing to occupy the surface of the adsorbent, so it is often difficult to play a synergistic removal effect

Method used

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  • Preparation method of graphene oxide and magnetic mesoporous silica composite material capable of adsorbing pollutants in water
  • Preparation method of graphene oxide and magnetic mesoporous silica composite material capable of adsorbing pollutants in water
  • Preparation method of graphene oxide and magnetic mesoporous silica composite material capable of adsorbing pollutants in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1. 0.86 g FeCl 3 ·6H 2 O and 2.0 g sodium acetate are dissolved in 30 mL appropriate amount of ethylene glycol, quickly mechanically stirred to dissolve, put into a 50mL capacity PTFE lining, plus a stainless steel jacket, in a muffle furnace or blast drying box, Set the temperature to 200°C, and the reaction proceeded for 8 hours. After natural cooling, it was washed three times with ethanol and water to obtain inorganic magnetic particles with an average particle size of 330 nm. Wash it ultrasonically for 15 minutes in a hydrochloric acid aqueous solution with a concentration of 1M, and wash until neutral.

[0034] Disperse 150 mg of the seeds obtained after washing in a mixed solvent of deionized water and absolute ethanol (v / v=30 / 70), add an appropriate amount of ammonia water, adjust the pH of the system between 9.0-9.5, and add under ultrasonic mechanical stirring 80.4 μL of tetraethyl orthosilicate, the reaction was mechanically stirred for 24 h at room t...

Embodiment 2

[0038] Example 2. The same method is used to prepare silica magnetic composite microspheres. By increasing the amount of sodium acetate to 3.0 g, magnetic microspheres with a particle size of 220 nm can be prepared; using the same silicon coating process, in different proportions of deionized water and In a mixed solvent of water and ethanol (v / v=10 / 90), silica magnetic microspheres with a particle size of about 250 nm were prepared; as seeds, the same mesoporous silica coating process was used, and orthosilicic acid was changed. The amount of tetraethyl and hexadecyltriethoxysilane can be used to prepare mesoporous silica magnetic microspheres with an average particle size of about 310 nm. Using the same basic method of PEI modification and increasing the amount of PEI to 30 mg, more amine groups can be introduced on the surface of the mesoporous silica magnetic microspheres. On the one hand, it can strengthen the binding efficiency with graphene oxide, and it can also improv...

Embodiment 3

[0039] Example 3. The graphene oxide mesoporous silica magnetic composite material obtained in the above Examples 1 and 2 was used for the adsorption experiment of Pb(II) and HA. The adsorption experiment is carried out at 25℃. Generally, 1.0 mg of the composite material is dispersed in a 10 mL liquid glass tube, and different initial concentrations of Pb(II) are configured, such as 5,10,20,50,80,100 mg / L, adjust the pH of the solution close to neutral, shake and combine at 150 rpm at room temperature for 24 h. When the adsorption reaches equilibrium, place the sample on the magnet for full separation. Use ICP-AES to test the absorbance of the remaining heavy metal ions in the solution, using the above formula 1. To calculate the adsorption capacity. See attached for typical adsorption isotherms Figure 4 .

[0040] The composite material can also synergistically adsorb humic acid and heavy metal ions. We used HA and without HA to investigate the adsorption characteristics of...

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Abstract

The invention relates to a preparation method of a composite material prepared by graphene oxide and magnetic mesoporous silica microspheres through chemical bonding interaction. The magnetic particles are prepared by a hydrothermal process; after acid ultrasonic treatment, the magnetic particles are firstly coated with a thin silicon oxide shell layer by a sol-gel method; after that, long-chain alkane is taken as a pore-forming agent, the magnetic particles are copolymerized with tetraethyl orthosilicate (TEOS) in the sol-gel reaction, and then the pore-forming agent is removed by thermal etching, so that the magnetic mesoporous silica particles with certain hydroxyl on the surfaces can be obtained; polyetherimide (PEI) surface modification is carried out on the magnetic mesoporous silica particles, and strong interaction between PEI and silicon hydroxyl is utilized; finally, the carboxyl on ethylene dichloride (EDC) activated graphene oxide reacts with amino on the PEI, so that the graphene oxide magnetic mesoporous silica composite material can be obtained. The preparation method is simple, convenient and controllable and is favorable for amplification preparation. The composite material has large specific surface area and good magnetic controllability, and can adsorb humic acid and heavy metal ions Pb (II) at the same time by virtue of surface groups.

Description

field of invention [0001] The invention belongs to the technical field of preparation of inorganic nanocomposite materials, and in particular relates to a preparation method of a magnetic graphene oxide mesoporous silicon oxide composite material capable of absorbing pollutants in water. Background technique [0002] With the improvement of people's awareness of environmental protection and the continuous improvement of the quality of life, the requirements for the characteristics of new adsorbents for water treatment are getting higher and higher. Pollutants in water, including organic matter such as humic acid, antibiotics, and heavy metal ions are relatively common pollutants that need to be removed urgently. Activated carbon, macroporous polymer adsorption resin, flocculation precipitant, etc. have been used in the adsorption and removal of these pollutants. In recent years, nanomaterials have gradually become the main body of new adsorbents due to their unique physicoc...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F1/62C02F1/58
Inventor 王祎龙唐玉霖郭方方
Owner TONGJI UNIV
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