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A kind of method utilizing ice-water mixture to dilute concentrated sulfuric acid in preparing graphite oxide

A technology of ice-water mixture and concentrated sulfuric acid, applied in the field of diluting concentrated sulfuric acid with ice-water mixture in the preparation of graphite oxide, can solve the problems of difficult control system temperature, long reaction time, high equipment requirements, etc., achieve good thermal conductivity and low equipment requirements , The process is simple and stable

Inactive Publication Date: 2011-12-14
THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently used graphite oxide preparation methods all have problems such as difficulty in controlling the system temperature when diluting concentrated sulfuric acid, long reaction time and high requirements for equipment.

Method used

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  • A kind of method utilizing ice-water mixture to dilute concentrated sulfuric acid in preparing graphite oxide
  • A kind of method utilizing ice-water mixture to dilute concentrated sulfuric acid in preparing graphite oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for diluting concentrated sulfuric acid with ice-water mixture in the preparation of graphite oxide of the present invention comprises the following preparation steps:

[0024] 1. Weigh 25g of Baichuan 200 mesh natural flake graphite powder, pour it into a round bottom flask with a funnel, take 1L of concentrated sulfuric acid with a weight percentage of 98% and slowly pour it into the round bottom flask, and connect it to an electric stirrer;

[0025] 2. Set the stirring speed to 100 rpm, weigh 87.5g of potassium permanganate, and gradually add it to the concentrated sulfuric acid graphite powder solution within 20 minutes;

[0026] 3. Soak the round bottom flask in a water bath, set the temperature of the water bath to 35°C for 2 hours, and set the stirring speed to 200 rpm;

[0027] 4. After the reaction is finished, quickly add it into a beaker containing 6L of deionized ice-water mixture (ice: water mass ratio is 1:1), and the stirring speed of the connect...

Embodiment 2

[0032] A method for diluting concentrated sulfuric acid with ice-water mixture in the preparation of graphite oxide of the present invention comprises the following preparation steps:

[0033] 1. Weigh 25g of Baichuan 200 mesh natural flake graphite powder, pour it into a round bottom flask with a funnel, take 1L of concentrated sulfuric acid with a weight percentage of 98% and slowly pour it into the round bottom flask, and connect it to an electric stirrer;

[0034] 2. Set the stirring speed to 100 rpm, weigh 87.5g of potassium permanganate, and gradually add it to the concentrated sulfuric acid graphite powder solution within 20 minutes;

[0035] 3. Soak the round bottom flask in a water bath, set the temperature of the water bath to 35°C for 2 hours, and set the stirring speed to 200 rpm;

[0036] 4. After the reaction is finished, quickly add it into a beaker containing 5L of deionized ice-water mixture (ice: water mass ratio is 1: 1), and the stirring speed of the connec...

Embodiment 3

[0041] A method for diluting concentrated sulfuric acid with ice-water mixture in the preparation of graphite oxide of the present invention comprises the following preparation steps:

[0042] 1. Weigh 25g of Baichuan 200 mesh natural flake graphite powder, pour it into a round bottom flask with a funnel, take 1.25L of 98% concentrated sulfuric acid by weight and slowly pour it into the round bottom flask, and connect it to an electric stirrer;

[0043] 2. Set the stirring speed to 100 rpm, weigh 87.5g of potassium permanganate, and gradually add it to the concentrated sulfuric acid graphite powder solution within 20 minutes;

[0044] 3. Soak the round bottom flask in a water bath, set the temperature of the water bath to 35°C for 1 hour, and set the stirring speed to 200 rpm;

[0045] 4. After the reaction is completed, quickly add it to a beaker containing 6.25L of deionized ice-water mixture (the mass ratio of ice: water is 3:2), and the stirring speed of the electric stirr...

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Abstract

The invention relates to a method for diluting concentrated sulfuric acid with a mixture of ice and water in the preparation of graphite oxide, which comprises the following steps: firstly take graphite powder and place it in a first reaction vessel, then add concentrated sulfuric acid and stir; add high Potassium manganate and stirring; the first reaction vessel is heated in a water bath at 30 to 40°C; the mixed reactant in the first reaction vessel is added to the second reaction vessel containing a deionized ice-water mixture and stirred; Add hydrogen peroxide dropwise into the second container until no bubbles are generated; filter the insoluble matter in the suspension and wash them several times with dilute hydrochloric acid and deionized water; Dry at room temperature in the box, and obtain graphite oxide after vacuum drying. The method of the invention has the advantages of rapidity, simple and stable process, low requirement on equipment and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of graphite oxide preparation, in particular to a method for diluting concentrated sulfuric acid with a mixture of ice and water in the preparation of graphite oxide. Background technique [0002] Graphene, English name Graphene, is a two-dimensional lattice structure in which carbon atoms are arranged in a hexagonal manner. As a single-layer carbon-atom planar material, graphene can be obtained by exfoliating graphite materials. Graphene has become the focus of scientific and industrial attention since the graphite crystal film was discovered by scientists at the University of Manchester in 2004. The thickness of graphene is only 0.335 nanometers, which is not only the thinnest among known materials, but also very firm and hard; as a simple substance, it transfers electrons faster than all known conductors and semiconductors at room temperature (graphene Electrons move at 1 / 300 the speed of light). Due t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00
Inventor 蔡燕温祝亮
Owner THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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