CN112191230A - Preparation of graphene functionalized magnetic silicon dioxide and application of graphene functionalized magnetic silicon dioxide in water treatment - Google Patents
Preparation of graphene functionalized magnetic silicon dioxide and application of graphene functionalized magnetic silicon dioxide in water treatment Download PDFInfo
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Abstract
The invention discloses a preparation method of graphene functionalized magnetic silicon dioxide and application of the graphene functionalized magnetic silicon dioxide in water treatment2/Fe3O4) (ii) a Then, modifying the magnetic silica by using a siloxane coupling agent (3-aminopropyl trimethyl silane KH 550) to obtain amino functionalized modified magnetic silica; finally, graphene oxide and amino functionalized magnetic silica are subjected to condensation reaction to prepare graphene functionalized magnetic silica (GN/SiO)2/Fe3O4). Graphene/silicon dioxide/ferroferric oxide nano composite material (GN/SiO) prepared by the invention2/Fe3O4) The adsorbent can effectively adsorb pollutants in water, can be recycled, can be used as an efficient adsorbent for treating sewage, and has a wide application prospect.
Description
Technical Field
The invention relates to a preparation method and application of an organic pollutant adsorbent, in particular to preparation of graphene functionalized magnetic silica (graphene/silica/ferroferric oxide nano composite material) and application of the graphene functionalized magnetic silica in water treatment.
Background
Silica has a high specific surface area, a large pore diameter, a large amount of silicon hydroxyl groups on the surface and the like, and is always a hotspot for research in the field of adsorption, but in the practical application of adsorption materials, the performance of the adsorption materials can not meet the requirements of various applications, and the adsorption performance of the adsorption materials on metal ions is improved by the functionalized modification of organic micromolecules on the silica, so that the adsorption materials become a hotspot for research, but the adsorption effect on organic pollutants is general.
Graphene is a novel two-dimensional planar nano material with a single atomic layer structure, and has many novel characteristics, such as: higher Young's modulus, thermal conductivity and the like, particularly excellent stability and higher specific surface area (the theoretical value of 2630 m)2The/g) and the unique planar polycyclic aromatic hydrocarbon lattice structure have good adsorption performance on aromatic organic pollutants, and the characteristics enable the graphene to be expected to be the most excellent adsorption material.
The magnetic nano particles have the physical and chemical properties of superparamagnetism, high adsorption capacity and the like, can be applied to magnetic separation, and have the advantages of cyclic utilization, high treatment efficiency, low operation cost and the like, so the magnetic nano particles have huge application prospects in the field of water treatment.
However, it is noteworthy that: the method for preparing the graphene/silicon dioxide/ferroferric oxide nano-adsorption material by using graphene to perform functional modification on magnetic silicon dioxide by adopting a covalent bond grafting method is not reported. Here, a siloxane coupling agent containing an amino group is grafted to the surface of magnetic nano silica, and then the amino group is used for condensation reaction with a carboxyl group on the surface of graphene oxide, so that the graphene functionalized and modified silica nano adsorption material is obtained.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene/silicon dioxide/ferroferric oxide nano composite material and an application of the graphene/silicon dioxide/ferroferric oxide nano composite material in water treatment, and aims to solve the technical problem of improving the adsorption performance of silicon dioxide used as an adsorbent.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation method of the graphene functionalized magnetic silica comprises the following steps:
1) preparation of magnetic silica:
adding ferroferric oxide nanoparticles into ethanol solvent, ultrasonically stirring for 1-2h, adding appropriate amount of ethyl orthosilicate and ammonia water, continuously ultrasonically stirring for reaction for 5-6h, washing with water and acetone, and drying to obtain magnetic silica nanoparticles (SiO)2/Fe3O4）。
Wherein: the ratio of the ferroferric oxide nanoparticles to the tetraethoxysilane is 1 g: 15-35 mL;
2) amino functionalized magnetic Silica (SiO)2-NH2/Fe3O4) The preparation of (1):
adding appropriate amount of 3-aminopropyltrimethylsilane (KH 550) and anhydrous toluene solvent into magnetic silica, heating and refluxing for 72 h, cooling, filtering, washing with dichloromethane, and drying to obtain amino functionalized magnetic silica solid powder.
Wherein: the ratio of magnetic silica to 3-aminopropyltrimethylsilane was 1 g: 5-8 mL;
the ratio of magnetic silica to toluene solvent was 1 g: 30 mL.
3) Graphene functionalized magnetic silica (GN/SiO)2/Fe3O4) The preparation of (1):
adding a proper amount of graphene oxide into a solvent N, N-Dimethylformamide (DMF), performing ultrasonic dispersion uniformly, then adding a proper amount of condensing agent 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDC.HCl) and N-hydroxysuccinimide (NHS), stirring and reacting for 2-3 h at room temperature, then adding the amino functionalized magnetic silicon dioxide obtained in the step 2), and continuing stirring and reacting for 24-48 h to obtain the graphene/silicon dioxide/ferroferric oxide nanocomposite.
Wherein: the ratio of graphene oxide to N, N-Dimethylformamide (DMF) was 10 mg: 1-2 mL;
the mass ratio of graphene oxide to EDC, HCl and NHS is 1: 5-10: 3-5.
The mass ratio of the graphene oxide to the amino-functionalized magnetic silica is 1: 3-6.
The application of the graphene functionalized magnetic silicon dioxide in water treatment comprises the following steps:
adding the graphene/silicon dioxide/ferroferric oxide nanocomposite into an aqueous solution containing organic pollutants, oscillating for 20-30 min to enable the organic pollutants and the graphene/silicon dioxide/ferroferric oxide nanocomposite to reach adsorption-desorption balance, and performing magnetic separation to remove the organic pollutants in the water by adsorption.
Wherein: the mass ratio of the graphene/silicon dioxide/ferric oxide adsorbent to the organic pollutants is 150-500: 1;
the organic pollutants comprise common aromatic organic pollutants such as malachite green, methylene blue, methyl orange, rhodamine B and the like.
According to the invention, on the basis of combining the advantages of the magnetic nanoparticles, the silicon dioxide and the graphene, the prepared graphene functionalized magnetic silicon dioxide (namely graphene/silicon dioxide/ferroferric oxide nano composite material) is used as a ternary nano adsorbent, and finally controllable preparation of the graphene functionalized magnetic silicon dioxide (graphene/silicon dioxide/ferroferric oxide nano composite material) and efficient adsorption and recycling of organic pollutants in sewage treatment are realized. The method has good repeatability, the composite material can effectively adsorb pollutants in water, can be recycled, can be used as an efficient adsorbent for treating sewage, and has wide application prospect.
Drawings
FIG. 1 is a photograph of a graphene/silica/ferroferric oxide nanocomposite material according to the present invention;
FIG. 2 is a recycling experiment of a graphene/silicon dioxide/ferroferric oxide nanocomposite material for adsorbing a rhodamine B aqueous solution;
FIG. 3 is a diagram of a rhodamine B aqueous solution after adsorption treatment by a graphene/silicon dioxide/ferroferric oxide nanocomposite.
Detailed Description
Example 1:
1. preparation of magnetic silica:
adding 0.12g of ferroferric oxide nano particles into 40mL of ethanol solvent, carrying out ultrasonic stirring for 1h, adding 10mL of ammonia water and 4mL of tetraethoxysilane, and continuing to carry out ultrasonic stirring reaction for 6 h. Washing with water and acetone, and drying at 60 deg.C to obtain 0.82 g magnetic silica nanoparticles (SiO)2/Fe3O4）。
2. Amino functionalized magnetic Silica (SiO)2-NH2/Fe3O4) The preparation of (1):
0.5 g of magnetic silica and 3 mL of 3-aminopropyltrimethylsilane (KH 550) were added to 15 mL of anhydrous toluene, and the reaction was heated under reflux for 72 hours. Then cooling, decompressing and filtering, washing by dichloromethane, and drying at 60 ℃ to obtain 0.45 g of amino functionalized magnetic silicon dioxide solid powder.
3. Graphene functionalized magnetic silica (GN/SiO)2/Fe3O4) The preparation of (1):
adding 50 mg of graphene oxide into 10mL of N, N-Dimethylformamide (DMF), performing ultrasonic dispersion uniformly, adding 0.3g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDC.HCl) and 0.17g N-hydroxysuccinimide (NHS) as condensing agents, stirring and reacting for 2h at room temperature, then adding 0.18g of the amino-functionalized magnetic silica obtained in the step 2, and continuing to stir and react for 24 h to obtain the graphene-functionalized magnetic silica (graphene/silica/ferroferric oxide nanocomposite, as shown in FIG. 1).
4. Adsorption of pollutants:
and (2) adding 0.02 g of the graphene/silicon dioxide/ferroferric oxide nanocomposite obtained in the step (3) into 5ml of solution (with the concentration of 10 mg/L) containing rhodamine B, oscillating for 20-30 min to enable the rhodamine B and the graphene/silicon dioxide/ferroferric oxide nanocomposite to reach adsorption-desorption balance, and after magnetic separation, enabling the adsorption rate to reach 99.8% (shown in figure 2).
5. Graphene functionalized silica (GN/SiO)2/Fe3O4) The recycling of (2):
and (3) adding the graphene/silicon dioxide/ferroferric oxide nano composite material adsorbing rhodamine B in the step (4) into 10mL of ethanol, oscillating for 15 min, carrying out magnetic separation, desorbing the rhodamine B from the graphene/silicon dioxide/ferroferric oxide nano composite material, and repeating the operation for 4 times. And (3) reusing the regenerated graphene/silicon dioxide/ferroferric oxide nanocomposite adsorbent in the adsorption experiment of the rhodamine B-containing aqueous solution in the step (4) to investigate the recycling condition of the graphene/silicon dioxide/ferroferric oxide nanocomposite. Experimental results show that the graphene/silicon dioxide/ferroferric oxide nanocomposite adsorbent still shows excellent adsorption performance and regenerability after being regenerated for 10 times (as shown in figure 3), and the adsorption rate is 99.0% after being recycled for 10 times.
Example 2:
1. preparation of magnetic silica:
adding 0.2g of ferroferric oxide nano particles into 40mL of ethanol solvent, carrying out ultrasonic stirring for 1h, adding 10mL of ammonia water and 4mL of tetraethoxysilane, and continuing to carry out ultrasonic stirring reaction for 6 h. Washing with water and acetone, and drying at 60 deg.C to obtain 1.44 g magnetic silica nanoparticles (SiO)2/Fe3O4）。
2. Amino functionalized magnetic Silica (SiO)2-NH2/Fe3O4) The preparation of (1):
1.33 g of magnetic silica and 10mL of 3-aminopropyltrimethylsilane (KH 550) were added to 24 mL of anhydrous toluene, and the reaction was heated under reflux for 72 hours. Then cooling, decompressing and filtering, washing by dichloromethane, and drying at 60 ℃ to obtain 1.31 g of amino functionalized silicon dioxide solid powder.
3. Graphene functionalized magnetic silica (GN/SiO)2/Fe3O4) The preparation of (1):
adding 220 mg of graphene oxide into 25 mL of N, N-Dimethylformamide (DMF), performing ultrasonic dispersion uniformly, adding 1.29 g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDC.HCl) and 0.75 g N-hydroxysuccinimide (NHS) as condensing agents, stirring and reacting for 2 hours at room temperature, then adding 0.81 g of amino functionalized magnetic silicon dioxide obtained in the step 2, and continuing to stir and react for 36 hours to obtain the graphene/silicon dioxide/ferroferric oxide nanocomposite.
4. Adsorption of pollutants:
adding 0.02 g of the graphene/silicon dioxide/ferroferric oxide nano composite material obtained in the step 2 into 10mL of solution (with the concentration of 10 mg/L) containing rhodamine B, oscillating for 20-30 min to ensure that the rhodamine B and the graphene/silicon dioxide/ferroferric oxide nano composite material adsorbent reach adsorption-desorption balance, after magnetic separation, the rhodamine B in water can be effectively adsorbed, the adsorption rate is 99.4%,
example 3:
1. preparation of magnetic silica:
adding 0.4g of ferroferric oxide nano particles into 80mL of ethanol solvent, carrying out ultrasonic stirring for 1h, adding 20mL of ammonia water and 8mL of tetraethoxysilane, and continuing to carry out ultrasonic stirring reaction for 6 h. Washing with water and acetone, and drying at 60 deg.C to obtain 2.72 g magnetic silica nanoparticles (SiO)2/Fe3O4）。
2. Amino functionalized magnetic Silica (SiO)2-NH2/Fe3O4) The preparation of (1):
3.0 magnetic silica and 15 mL of 3-aminopropyltrimethylsilane (KH 550) were added to 30 mL of anhydrous toluene, and the reaction was heated under reflux for 72 hours. Then 2.95 g of amino-functionalized silicon dioxide solid powder is obtained after cooling, decompression and suction filtration, washing by dichloromethane and drying at 60 ℃.
3. Graphene functionalized magnetic silica (GN/SiO)2/Fe3O4) The preparation of (1):
adding 288 mg of graphene oxide into 50 mL of N, N-Dimethylformamide (DMF), performing ultrasonic dispersion uniformly, adding 2.57 g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDC.HCl) and 1.46 g N-hydroxysuccinimide (NHS) serving as condensing agents, stirring and reacting for 3 hours at room temperature, then adding 1.57 g of amino functionalized magnetic silicon dioxide obtained in the step 2, and continuing to stir and react for 48 hours to obtain the graphene/silicon dioxide/ferroferric oxide nanocomposite.
5. Adsorption of pollutants:
0.015 g of the obtained graphene/silicon dioxide/ferroferric oxide nanocomposite is added into 10mL of aqueous solution (the concentration is 10 mg/L) containing rhodamine B, oscillation is carried out for 20-30 min, so that the adsorption-desorption balance of the rhodamine B and the graphene/silicon dioxide/ferroferric oxide nanocomposite adsorbent is achieved, and the adsorption rate of the rhodamine B after magnetic separation is 98.5%.
Claims (4)
1. The preparation method of the graphene functionalized magnetic silica is characterized by comprising the following steps:
1) preparation of magnetic silica:
adding ferroferric oxide nanoparticles into ethanol serving as a solvent, ultrasonically stirring for 1-2 hours, adding a proper amount of tetraethoxysilane and ammonia water, continuously ultrasonically stirring for reacting for 5-6 hours, washing with water and acetone, and drying to obtain magnetic silicon dioxide nanoparticles;
the ratio of the ferroferric oxide nanoparticles to the tetraethoxysilane is 1 g: 15-35 mL;
2) preparation of amino-functionalized magnetic silica:
adding magnetic silica nanoparticles and 3-aminopropyltrimethylsilane into an anhydrous toluene solvent, heating and refluxing for reaction for 72 hours, then cooling, filtering, washing with dichloromethane, and drying to obtain amino functionalized magnetic silica solid powder;
the ratio of the magnetic silicon dioxide to 3-aminopropyltrimethylsilane was 1 g: 5-8 mL; the ratio of magnetic silica to toluene solvent was 1 g: 30 mL;
3) preparing graphene functionalized magnetic silicon dioxide:
adding a proper amount of graphene oxide into a solvent N, N-dimethylformamide, ultrasonically dispersing uniformly, then adding a proper amount of condensing agent 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, stirring and reacting for 2-3 h at room temperature, then adding the amino functionalized magnetic silicon dioxide obtained in the step 2), and continuously stirring and reacting for 24-48 h to obtain graphene functionalized magnetic silicon dioxide;
the ratio of graphene oxide to N, N-dimethylformamide is 10 mg: 1-2 mL; the mass ratio of the graphene oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the N-hydroxysuccinimide is 1: 5-10: 3-5; the mass ratio of the graphene oxide to the amino-functionalized magnetic silica is 1: 3-6.
2. The application of the graphene functionalized magnetic silica prepared according to claim 1 in water treatment is characterized by comprising the following steps:
adding graphene functionalized magnetic silica into an aqueous solution containing organic pollutants, oscillating for 20-30 min to enable the organic pollutants and the graphene functionalized magnetic silica to achieve adsorption-desorption balance, and performing magnetic separation to remove the organic pollutants in the water.
3. The use of graphene-functionalized magnetic silica according to claim 2 in water treatment, wherein:
the mass ratio of the graphene functionalized magnetic silicon dioxide to the organic pollutants is 150-: 1.
4. the use of graphene-functionalized magnetic silica according to claim 2 or 3 in water treatment, wherein:
the organic pollutants comprise malachite green, methylene blue, methyl orange and rhodamine B.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113634226A (en) * | 2021-08-10 | 2021-11-12 | 致慧医疗科技(上海)有限公司 | Fe3O4/GO composite nano material and preparation method and application thereof |
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| CN103432996A (en) * | 2013-08-27 | 2013-12-11 | 同济大学 | Preparation method of graphene oxide and magnetic mesoporous silica composite material capable of adsorbing pollutants in water |
| CN106540658A (en) * | 2016-12-05 | 2017-03-29 | 湖南工业大学 | A kind of graphene oxide covalent bond coated magnetic nano composition and preparation method thereof |
| CN110302752A (en) * | 2019-06-18 | 2019-10-08 | 湖南工业大学 | A kind of graphene oxide cladding Fe3O4Nano-cluster composite material and preparation method |
| CN111203187A (en) * | 2020-01-15 | 2020-05-29 | 中国地质科学院水文地质环境地质研究所 | Repair material for removing pollutants in underground water, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0573446A1 (en) * | 1991-02-27 | 1993-12-15 | Laporte Industries Limited | Adsorbent material |
| CN103432996A (en) * | 2013-08-27 | 2013-12-11 | 同济大学 | Preparation method of graphene oxide and magnetic mesoporous silica composite material capable of adsorbing pollutants in water |
| CN106540658A (en) * | 2016-12-05 | 2017-03-29 | 湖南工业大学 | A kind of graphene oxide covalent bond coated magnetic nano composition and preparation method thereof |
| CN110302752A (en) * | 2019-06-18 | 2019-10-08 | 湖南工业大学 | A kind of graphene oxide cladding Fe3O4Nano-cluster composite material and preparation method |
| CN111203187A (en) * | 2020-01-15 | 2020-05-29 | 中国地质科学院水文地质环境地质研究所 | Repair material for removing pollutants in underground water, preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113634226A (en) * | 2021-08-10 | 2021-11-12 | 致慧医疗科技(上海)有限公司 | Fe3O4/GO composite nano material and preparation method and application thereof |
| CN113634226B (en) * | 2021-08-10 | 2023-08-18 | 致慧医疗科技(上海)有限公司 | Fe 3 O 4 GO composite nano material and preparation method and application thereof |
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