US 9,266,737 B2 · Method and apparatus for manufacturing graphite oxide

Abstract

There is provided a method and an apparatus for preparing graphite oxide. In accordance with the present disclosure, when an oxidizer is added by stages into a sequencing batch oxidizer mixer connected in multiple stages at a constantly low temperature, the oxidizer is mixed therein while suppressing an oxidation reaction. During an oxidation reaction of graphite, in a risky range of overheating and explosion, a tube type reactor equipped within a heat exchanger is used to accurately control a local temperature and the oxidizer can permeate between layers of the graphite with increased efficiency under ultrasonication. In an additional reaction range out of the risky range, a continuous stirred tank reactor is used to mature the oxidation reaction, so that a risk of explosion during manufacturing of graphite oxide can be reduced and a great amount of graphite oxide can be mass-produced economically.

Claims20

Dependent claims

A method for manufacturing graphite oxide, the method comprising:

preparing graphite slurry by mixing graphite and a sulfuric acid;
mixing the graphite slurry with an oxidizer selected from the group consisting of a permanganic acid, permanganate, and a permanganate sulfuric acid solution by supplying the oxidizer by stages into sequencing batch oxidizer mixers connected to one another in multiple stages;
making an intermediate reaction by pressing a reaction mixture mixed with the oxidizer into a tube type reactor equipped within a thermostat bath to be applied with ultrasonic waves;
making an additional reaction by supplying a reaction mixture of the intermediate reaction into a continuous stirred tank reactor;
mixing a reaction mixture of the additional reaction with water added;
adding a hydrogen peroxide aqueous solution to the reaction mixture mixed with the water and mixing them to terminate an oxidation reaction;
washing and separating graphite oxide from the reaction mixture of the terminated oxidation reaction;
and
drying the separated graphite oxide.

6 more elements

An apparatus for manufacturing graphite oxide, the apparatus comprising:

a graphite slurry mixer configured to prepare graphite slurry by mixing graphite and a sulfuric acid;
sequencing batch oxidizer mixers connected to the graphite slurry mixer in multiple stages from about two stages to about ten stages in series;
a tube type reactor having an inner diameter in a range of from about 5 mm to about 50 mm, a residence time in a range of from about 0.2 hours to about 5 hours, and a length in a range of from about 10 m to about 1000 m that is sequentially connected to the sequencing batch oxidizer mixers and equipped within a thermostat bath to be applied with ultrasonic waves to prepare an intermediate reaction mixture;
a continuous stirred tank reactor that is connected to the tube type reactor and makes an additional reaction with the intermediate reaction mixture;
a water mixer configured to add water to a reaction and mixing the water with a reaction mixture of the additional reaction;
a hydrogen peroxide mixer configured to add and mix a hydrogen peroxide aqueous solution to a reaction mixture mixed with the water and mixing them to terminate an oxidation reaction;
a washing and separating unit configured to wash and separate graphite oxide from a reaction mixture of the terminated oxidation reaction;
and
a dryer configured to dry the separated graphite oxide.

6 more elements

Dependencies are inferred from the claim text.

Method and apparatus for manufacturing graphite oxide

Life of this patent

Method and apparatus for manufacturing graphite oxide

Life of this patent

Abstract

Claims20