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Preparation method for modified graphene oxide adsorption material

A technology of adsorption materials and oxidized stones, which is applied in chemical instruments and methods, adsorption water/sewage treatment, and other chemical processes. It can solve the problems of high condition requirements and long reaction cycle, and achieve uniform distribution of pore channels and excellent adsorption performance. , The effect of enhancing the adsorption capacity

Active Publication Date: 2017-12-22
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is the same as the existing EDTA-modified graphene oxide method, most of which use silanization reagents as intermediates, and the silanization method generally has defects such as long reaction cycle and high condition requirements.

Method used

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  • Preparation method for modified graphene oxide adsorption material
  • Preparation method for modified graphene oxide adsorption material
  • Preparation method for modified graphene oxide adsorption material

Examples

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Embodiment 1

[0015] This embodiment includes the following steps:

[0016] (1) Take 100 mg of graphene oxide (commercially available) in a three-neck round bottom flask, add 50 mL of anhydrous DMF to ultrasonically disperse for 1 h, add 1 mL of MDI, and stir at 60 °C for 4 h; cool down after the reaction, and the reaction product Washing with anhydrous DMF for 3 times (using 15 ml of anhydrous N,N-dimethylformamide each time), centrifuging, and vacuum drying to obtain diphenylmethane diisocyanate functionalized graphene oxide;

[0017] (2) Take 0.1 g of diphenylmethane diisocyanate functionalized graphene oxide obtained in step (1) and 2 g of EDTA, grind and mix them evenly in an agate mortar, then place them in a ball mill, control the ratio of ball to material to 3:1, and the speed is 60rad / min, ball milling for 6h, washing with a sodium bicarbonate (NaHCO3) solution with a pH of 8.0 until no bubbles emerge, and then freeze-drying to obtain EDTA / diphenylmethane diisocyanate / graphene oxid...

Embodiment 2

[0019] This embodiment includes the following steps:

[0020] (1) Take 100 mg of graphene oxide (commercially available) in a three-neck round bottom flask, add 50 mL of anhydrous DMF for ultrasonic dispersion for 1 h, add 3 mL of MDI, and stir for 4 h at 60 °C; The product was washed 3 times with anhydrous DMF (15 ml of anhydrous N,N-dimethylformamide each time), centrifuged, and vacuum-dried to obtain diphenylmethane diisocyanate functionalized graphene oxide;

[0021] (2) Grind 0.1 g of diphenylmethane diisocyanate functionalized graphene oxide obtained in step (1) and 4 g of EDTA in an agate mortar, mix them uniformly and place them in a ball mill, control the ratio of ball to material to 3:1, and the speed is 60rad / min, ball milled for 6h, washed with a sodium bicarbonate (NaHCO3) solution with a pH of 8.0 until no bubbles emerged, and then freeze-dried to obtain an EDTA / MDI / graphene oxide composite material.

Embodiment 3

[0023] This embodiment includes the following steps:

[0024] (1) Take 100 mg of graphene oxide (commercially available) and place it in a three-neck round bottom flask, add 50 mL of anhydrous DMF for ultrasonic dispersion for 1 h, add 3 mL of MDI, and stir at 80 ° C for 2 h; after the reaction is completed, cool the reaction product Wash 3 times with anhydrous N,N-dimethylformamide (DMF) (15 ml of anhydrous N,N-dimethylformamide each time), centrifuge and dry in vacuo to obtain diphenylmethane di Isocyanate functionalized graphene oxide;

[0025] (2) Take 0.1 g of diphenylmethane diisocyanate functionalized graphene oxide obtained in step (1) and 2 g of EDTA, grind and mix them evenly in an agate mortar, and then place them in a ball mill, controlling the ratio of ball to material to 3:1, and the speed is 100rad / min, ball milled for 3 hours, washed with a sodium bicarbonate (NaHCO3) solution with a pH of 8.0 until no bubbles emerged, and then freeze-dried to obtain EDTA / MDI...

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Abstract

The invention provides a preparation method for a modified graphene oxide adsorption material. The preparation method comprises the following steps: (1) ultrasonically dispersing graphene oxide in anhydrous N,N-dimethylformamide, then adding diphenylmethane diisocyanate and carrying out a reaction; and (2) uniformly mixing diphenylmethane diisocyanate-functionalized graphene oxide with ethylenediaminetetraacetic acid, and successively carrying out grinding, washing and freeze-drying so as to obtain the modified graphene oxide adsorption material. According to the invention, isocyanate is used as a bridge body, and a composite material is prepared through amidation and urethanization; an adsorbent prepared by using the method contains both polycarboxy functional groups and polyhydroxyl functional groups, has excellent adsorption effect on heavy metal ions in wastewater, and can overcome the defect that a chelate is dissolved in water and cannot be separated when EDTA is individually used for heavy metal removal.

Description

technical field [0001] The invention relates to a preparation method of a modified graphene oxide adsorption material. Background technique [0002] Graphene oxide is a carbon-based material with a two-dimensional planar honeycomb lattice structure formed by a single layer of carbon atoms tightly packed. It has a large specific surface area and is rich in activities such as -COOH, -OH, and epoxy groups on the surface. Oxygen-containing groups are a cost-effective heavy metal ion adsorbent. These oxygen-containing functional groups can not only chelate with heavy metal ions, but also form a network of cage molecules with adsorbates through hydrogen bonds. At the same time, the oxygen-containing functional groups also provide chemical reactivity for the functional modification of the graphene oxide surface. site, showing more active physical and chemical properties and easy chemical modification and other excellent properties. However, the dispersibility of graphene oxide is...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F101/20
CPCB01J20/20B01J20/22C02F1/283C02F1/285C02F2101/20
Inventor 杨焰余云杨宁宁黄彬廖有为
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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