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Method for preparing magnetic graphene oxide by using NH3.H2O-NH4NO3 solution

A technology of stone oxide and graphene is applied in the field of preparing magnetic graphene oxide by using NH3·H2O-NH4NO3 solution, and it can solve the problems of corrosion damage, unstable product performance, unsuitable for open system, etc. To achieve the effect of reducing corrosion, expanding layer spacing, and good dissociation effect

Active Publication Date: 2018-03-02
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the traditional preparation of magnetic graphene oxide, people mostly use NaOH or NH 3 ·H 2 O creates the necessary alkaline conditions, but during the synthesis process, due to the continuous consumption of hydroxide ions, the pH value of the system will also decrease, resulting in the deterioration of the quality of magnetic graphene oxide and the instability of product performance, and It is difficult to implement the industrial production of magnetic graphene oxide
[0005] At present, those skilled in the art will use ultrasonic means in the synthesis of magnetic graphene oxide, but ultrasonic is carried out continuously before graphite oxide is loaded with ferric oxide, and its effect is only to improve the dispersion of graphene oxide to a certain extent. and dissociation effect, this method is only a simple physical dispersion dissociation method, which cannot achieve the modification or modification effect of ferric oxide on graphene oxide.
In addition, there are still many problems in the use of ultrasonic reactors, such as the corrosion and damage of the ultrasonic reactor probe by the reaction liquid, it is not suitable for an open system that maintains the pH of the reaction liquid by dropping raw materials, etc., and an external heat source is required to control the reaction temperature, etc.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) Preparation of graphene oxide suspension: mix 6g of graphite and 3g of sodium nitrate and place in an ice-water bath, under stirring, slowly drop in 100mL of 98% concentrated sulfuric acid for 1 hour; add 18g of potassium permanganate and react for 6 hours Then add 18g of potassium permanganate, and continue to react for 12h; cool, wash, sonicate, take the upper layer suspension, and concentrate to 1 / 4 volume;

[0023] (2) Preparation of magnetic graphene oxide: graphene oxide suspension, FeCl-containing 2 and FeCl 3 mixed solution and NH 3 ·H 2 O-NH 4 NO 3 The solution was mixed, heated to 50°C, then placed in an ultrasonic cell pulverizer, (repeated by ultrasonication for 5s / interval of 10s), heated to 70°C, and the total reaction was 40min (including ultrasonic time and interval time), cooled, washed, and freeze-dried ; Among them, FeCl 2 and FeCl 3 The molar ratio is 1:2, NH 3·H 2 O-NH 4 NO 3 The molar ratio of the two is 3:1.

Embodiment 2

[0025] (1) Preparation of graphene oxide suspension: mix 4g of graphite and 2g of potassium nitrate and place in an ice-water bath, under stirring, slowly drop in 90mL of 98% concentrated sulfuric acid for 1h; add 30g of hydrogen peroxide, react for 6h before adding 30g hydrogen peroxide, continue to react for 12h; cool, wash, sonicate, take the upper suspension, concentrate to 1 / 4 volume;

[0026] (2) Preparation of magnetic graphene oxide: graphene oxide suspension, FeCl-containing 2 and FeCl 3 mixed solution and NH 3 ·H 2 O-NH 4 NO 3 The solutions were mixed, heated to 60°C, then placed in an ultrasonic cell pulverizer, (repeated by ultrasonication for 6s / interval of 12s), heated to 80°C, and the total reaction was 60min (including ultrasonic time and interval time), cooled, washed, and freeze-dried ; Among them, FeCl 2 and FeCl 3 The molar ratio is 1:2, NH 3 ·H 2 O-NH 4 NO 3 The molar ratio is 2:1.

Embodiment 3

[0028] (1) Preparation of graphene oxide suspension: mix 9g of graphite with 4g of sodium nitrate and place in an ice-water bath, under stirring, slowly drop in 120mL of 98% concentrated sulfuric acid for 1 hour; add 24g of potassium permanganate and react for 6 hours Then add 24g of potassium permanganate, and continue to react for 12h; cool, wash, sonicate, take the upper layer suspension, and concentrate to 1 / 4 volume;

[0029] (2) Preparation of magnetic graphene oxide: graphene oxide suspension, FeCl-containing 2 and FeCl 3 mixed solution and NH 3 ·H 2 O-NH 4 NO 3 The solution was mixed, heated to 70°C, then placed in an ultrasonic cell pulverizer, (repeated by ultrasonication for 8s / interval of 15s), heated to 90°C, and the total reaction was 80min (including ultrasonic time and interval time), cooled, washed, and freeze-dried ; Among them, FeCl 2 and FeCl 3 The molar ratio is 1:2, NH 3 ·H 2 O-NH 4 NO 3 The molar ratio is 4:1.

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Abstract

The invention discloses a method for preparing magnetic graphene oxide by using an NH3.H2O-NH4NO3 solution. The method comprises the following steps: preparing a graphene oxide solution, mixing the graphene oxide solution, an iron salt solution and the NH3.H2O-NH4NO3 solution, heating the obtained solution to 50-70 DEG C, and heating the solution to 70-90 DEG C under an ultrasonic condition to prepare the magnetic graphene oxide. The method has the remarkable advantages of stabilization of the production process through effectively combining ultrasonic treatment with the NH3.H2O-NH4NO3 solution, simplicity in operation, and production of the magnetic graphene oxide having superior performances.

Description

technical field [0001] The invention relates to a method for preparing magnetic graphene oxide, in particular to a method using NH 3 ·H 2 O-NH 4 NO 3 The invention discloses a method for preparing magnetic graphene oxide from a solution, belonging to the field of graphene oxide. Background technique [0002] In today's society, with the rapid development of modern industry, the problem of water pollution is becoming more and more serious, which has seriously affected the sustainable development of the national economy and the improvement of people's quality of life. In particular, toxic substances such as organic solvents and heavy metal ions have a more serious damage to water quality, which has caused many accidents and caused great harm to the health of the people. [0003] Graphene oxide is a two-dimensional carbon material with a large specific surface area and a large number of active reactive groups. It has a strong adsorption capacity for many organic solvents an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198C01G49/08
CPCC01G49/08C01P2004/04C01P2002/72C01P2004/80
Inventor 章峻王达炜沈健何磊冯福玲莫宏司玲
Owner NANJING NORMAL UNIVERSITY
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