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Graphene oxide, preparation method and application thereof

A graphene and natural graphite technology, applied in graphene oxide and its preparation, in the field of removing pollutants in water, can solve the problems of no adsorption of bisphenol A, single surface structure, poor effect, etc., achieve complete adsorption and ensure the degree of oxidation , the effect of easy large-scale preparation

Inactive Publication Date: 2015-05-13
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Activated carbon and expanded graphite have a single surface structure, only benzene rings, so good results can only be achieved when adsorbing non-polar organic substances, and the effect is not good for adsorbing polar organic substances and inorganic ions
Experiments show that expanded graphite has good adsorption on pyrene, but basically no adsorption on bisphenol A.
[0009] It can be seen that none of the above existing methods can effectively treat the two pollutions of BPA and heavy metal ions in sewage simultaneously.

Method used

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  • Graphene oxide, preparation method and application thereof
  • Graphene oxide, preparation method and application thereof
  • Graphene oxide, preparation method and application thereof

Examples

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Embodiment 1

[0047] The preparation of embodiment 1 graphene oxide

[0048] Present embodiment provides a kind of graphene oxide, such as figure 1 As shown, it was prepared by the following method:

[0049] (1) Oxidation:

[0050] a. Low temperature reaction: Add 20mL of concentrated sulfuric acid and a magnet to a 250ml round bottom flask, slowly add 1g of sodium nitrate under stirring at 40-60rpm, after it dissolves, cool in an ice bath to 0°C, and continue stirring , then add 1g of 325-mesh natural graphite, and then add 6g of potassium permanganate to ensure that the temperature of the reaction system is at 0-4°C, keep warm and react for 2h under slow stirring;

[0051] b. Medium-temperature reaction: remove the ice bath, use a 35°C water bath, continue to stir, control the temperature of the reaction system at 35±5°C, react for 20-40min, then slowly drop 40mL deionized water into the reaction system to keep the temperature of the reaction system Rise up, and control the temperature...

Embodiment 2

[0058] Embodiment 2 is to the adsorption and analysis method of heavy metal

[0059] Preparation of standard solution: use 2100mL Instrument Calibration Standard produced by Perkin Elmer.Inc., in which the concentration of each element is 100ppm, take 1mL of the original solution with a pipette, dilute with pure water to obtain a 1ppm metal ion mixed solution.

[0060] Experimental steps:

[0061] 1. Add 100mL of pure water into a plastic bottle, insert a magnet, add 50mg of the graphene oxide prepared in Example 1, stir and ultrasonically properly disperse it;

[0062] 2. Add 2mL of pre-prepared 1ppm heavy metal solution with a pipette gun, so that the concentration of heavy metal ions in the system is 20ppb, start timing from the time of addition, and take out 4mL at 5min, 15min, 25min, 50min, 100min, 150min and 200min Mix the liquid, close the lid when not taking the solution to prevent the solution from evaporating, centrifuge immediately after taking it out, and centrifu...

Embodiment 3

[0065] Embodiment 3 to the adsorption and analysis method of BPA

[0066] Instrument model: high performance liquid chromatography (Waters 2695), column model: C-18 column (Waters XBridge), flow rate: 1mL / min, mobile phase: a mixed solution of 70% methanol and 30% water, detector model: fluorescence Detection (Waters 2475), excitation wavelength: 278nm, fluorescence wavelength 315nm.

[0067] Experimental steps:

[0068] 1. Prepare the graphene oxide aqueous solution prepared by the embodiment 1 of 0.5 mg / mL in a 250mL beaker, and the specific operations are the same as in the embodiment 2;

[0069] 2. Add 0.2mL of pre-prepared 10ppm BPA methanol solution with a glass micro-injector, so that the BPA concentration in the system is 20ppb, start timing from the time of addition, and take out 4mL at 5min, 15min, 25min, 50min and 100min Mix the liquid, centrifuge immediately after taking it out, centrifuge at 11000rpm for 10 minutes, take out the supernatant and filter it with a ...

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Abstract

The invention provides graphene oxide, a preparation method and application thereof. The preparation method of the graphene oxide comprises the following steps: under a stirring condition, adding natural graphite, sodium nitrate and potassium permanganate into concentrated sulfuric acid, continuing to stir at 0-4 DEG C and taking a reaction for 2 hours; raising the temperature to 35+ / -5 DEG C, continuing to stir, and taking a thermal insulation reaction for 20-40 minutes; raising the temperature to 90-95 DEG C, continuing to stir and performing the thermal insulation reaction for 15-30 minutes; then adding hydrogen peroxide, centrifuging the solution, washing the supernatant with diluted hydrochloric acid, centrifuging the washed supernatant until sulfate ions cannot be detected out from the supernatant, washing the solution with pure water and centrifuging until the supernatant is neutral; after freeze drying, obtaining the graphene oxide. The invention further provides the application of the graphene oxide in removal of pollutants from water. The graphene oxide provided by the invention can be used for quickly and efficiently adsorbing pollutants such as BPA and heavy metal ions in water, so that the treated water quality can reach the drinking water standard.

Description

technical field [0001] The invention relates to a graphene oxide and its preparation method and use, in particular to a graphene oxide and its preparation method, and the use of the graphene oxide for removing pollutants in water, belonging to the technical field of sewage treatment. Background technique [0002] In modern society, water pollution has become a major public hazard. There is a common saying: "In the 1960s, rice was washed and vegetables were washed; in the 1970s, drinking water was irrigated; in the 1980s, the water quality deteriorated; in the 1990s, fish and shrimp became extinct." It can be seen that the control of water pollution in our country is urgent. Among the numerous pollutants, heavy metal pollutants and estrogen-like substances, such as bisphenol A, are particularly noticeable. [0003] Heavy metal ions are an important class of pollutants in water bodies, mainly including arsenic, lead, mercury, chromium, cadmium, barium, etc., which are charact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 崔昕毅缪峰夏栩笙
Owner NANJING UNIV
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