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Preparation method of magnetic graphene oxide and application thereof

A technology of stone oxide and graphene, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve unfavorable solid-liquid separation and adsorbent recovery, increase cost and energy consumption, and centrifugal separation Problems such as high energy consumption can achieve the effect of optimizing heating time, reducing preparation cost and saving time

Active Publication Date: 2015-09-23
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional graphite oxide preparation process will produce toxic and harmful gases containing chlorine or nitrogen. In order to achieve a higher oxidation effect, it is necessary to increase the dosing ratio of the oxidant and the oxidation time, which increases the cost and energy consumption.
At the same time, due to the small size of graphene oxide, it is not conducive to solid-liquid separation and adsorbent recovery after adsorption in aqueous solution. At the same time, high-speed centrifugal separation consumes a lot of energy, which limits practical applications.

Method used

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  • Preparation method of magnetic graphene oxide and application thereof
  • Preparation method of magnetic graphene oxide and application thereof
  • Preparation method of magnetic graphene oxide and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] First prepare the magnetic adsorption material-magnetic graphene oxide according to the following process:

[0029] (1) Measure 46mL of concentrated sulfuric acid (mass concentration 98%) and concentrated phosphoric acid (mass concentration 85%) mixed solution with a volume ratio of 9:1, add 2.0g flake graphite powder in the mixed solution, place in a constant temperature magnetic stirrer Stir magnetically in an ice-water bath at 0°C for 30-60 minutes until uniform dispersion; slowly add 6.0g of potassium permanganate, and continue stirring for 30-60 minutes until the mixture is dark green; heat up to 35°C, and stir to react 60 minutes; raise the temperature to 60°C, add 98mL of deionized water continuously dropwise, raise the temperature to 98°C and stir for 30-60 minutes at a constant temperature; Concentration of 5% hydrochloric acid solution and 20mL of mass concentration of 5% hydrogen peroxide solution, the supernatant turned golden yellow, stirred for 30 minutes;...

Embodiment 2

[0034] Take 8 parts of methylene blue solution with an initial concentration of 100mg / L, and in each part according to the concentration of 500mg / L, 1000mg / L, 1500mg / L, 2000mg / L, 2500mg / L, 3000mg / L, 3500mg / L and 4000mg / L respectively Dosage Add the magnetic graphene oxide prepared in Example 1, and adjust the pH value of each solution to be greater than 5, and oscillate and absorb in a constant temperature oscillator at 30°C, the oscillating speed is 150 rpm, and the oscillating time is 6 hours . After the shaking is completed, magnetic separation is carried out under the condition of an external magnetic field, the concentration of methylene blue in the supernatant is measured, and the removal effect is analyzed. Such as image 3 As shown, when the dosage is greater than 1000mg / L, the removal rate is above 99%; as the dosage increases, the saturated adsorption capacity gradually decreases.

Embodiment 3

[0036] Take 12 parts of methylene blue solution with an initial concentration of 100mg / L, adjust the pH values ​​to 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13 and 14, and add 1000mg / L The magnetic graphene oxide prepared in Example 1 was added in a large amount, and the adsorption was oscillated in a constant temperature oscillator at 30° C., the oscillating speed was 150 rpm, and the oscillating time was 6 hours. After shaking, perform magnetic separation, measure the concentration of methylene blue in the supernatant, and analyze the removal effect. Such as Figure 4 As shown, when the pH value is greater than 5, the removal rate is above 90%, and the pH value decreases after the adsorption is completed.

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Abstract

The invention discloses a preparation method of magnetic graphene oxide and application thereof. The preparation method comprises the following steps: 1 preparing mother liquor; 2 measuring the content of graphene oxide in the mother liquor; 3 obtaining an adsorbing material, namely the magnetic graphene oxide, by utilizing the mother liquor, FeCl[3].6H[2]O, FeSO[4].7H[2]O and stronger ammonia water. The magnetic graphene oxide prepared through the method is used for processing waste water containing methylene blue. According to the method, the graphene oxide is compounded through the improved Hummers method, ferroferric oxide nano-particles are loaded on a graphene oxide layer according to a certain proportion through a coprecipitation method, the obtained magnetic adsorbing material is used for the absorption treatment of a methylene blue solution, the synthetic process is simplified, the oxidation effect is guaranteed, and meanwhile the energy consumption is reduced, the time is saved, and the preparation cost is reduced; the magnetic adsorbing material which is applicable to different magnetic field environments and methylene blue waste water of different types of concentration is obtained, and the material can be recycled repeatedly.

Description

technical field [0001] The invention relates to a preparation method and application of a graphene oxide-based magnetic adsorption material (magnetic graphene oxide), and belongs to the technical fields of environmental functional materials and sewage treatment. Background technique [0002] With the rapid development of my country's industrial production, the amount of industrial wastewater discharged into the environmental water body continues to increase. The printing and dyeing industry consumes a lot of water, and the printing and dyeing wastewater produced has the characteristics of large discharge, complex water quality and high difficulty in treatment, which has been extensively studied in recent years. Methylene blue, also known as alkaline lake blue, is a relatively common cationic dye, which can be used for dyeing cotton, linen, silk fabrics, paper, and bamboo and wood. Methylene blue dye wastewater has a large chroma and has certain toxic effects. Discharging in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30C02F1/28
Inventor 李玉江张北吴涛孙德军陈云唐寅寅
Owner SHANDONG UNIV
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