A kind of continuous preparation and purification device and method of graphene oxide

A purification device, graphene technology, applied in the direction of graphene, single-layer graphene, chemical instruments and methods, etc., can solve the problems such as the inability to achieve continuous stripping and purification, the oxidation stripping reaction is not easy to control, and the oxidation stripping reaction time is prolonged. , to achieve the effect of promoting oxidation reaction and stripping again, improving the efficiency of continuous preparation and purification, and shortening the time of stripping

Active Publication Date: 2021-05-25
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the oxidative exfoliation reaction in the traditional preparation method of graphene oxide is not easy to control, resulting in uneven size of graphene oxide, and the preparation process needs to be carried out in multiple steps, which cannot achieve continuous exfoliation and purification.
On the other hand, a large amount of concentrated sulfuric acid solution is used as a reactant to exfoliate graphene oxide by diluting sulfuric acid to release heat. The preparation process needs to prolong the oxidation exfoliation reaction time to avoid violent reactions, and there is a large amount of waste acid polluting the environment.
At the same time, centrifugation or dialysis is used to remove metal ions in graphene oxide, which has the problems of low efficiency and waste of water.

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  • A kind of continuous preparation and purification device and method of graphene oxide

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Embodiment 1

[0040] Such as figure 1 As shown, the continuous preparation and purification device of graphene oxide in this embodiment includes a reactor 6 and a concentrated sulfuric acid solution storage bottle 1 and a water / hydrogen peroxide storage bottle 2 connected to the reactor 6 through a delivery pipe respectively. There is a three-way valve 4, the concentrated sulfuric acid solution storage bottle 1 is connected to the three-way valve 4 through the first delivery branch pipe 3-1, and the water / hydrogen peroxide storage bottle 2 is connected to the three-way valve 4 through the second delivery branch pipe 3-2 , the reactor 6 is connected to the three-way valve 4 through the first delivery pipe 3-3, the first peristaltic pump 5 is arranged on the first delivery pipe 3-3, and the ultrasonic plate 11, the first lifting platform 9 is arranged directly above the reactor 6, and the first lifting platform 9 is respectively provided with holes for the feeder 7 and the reactor 6 to commun...

Embodiment 2

[0044] The preparation method of the graphene oxide of the present embodiment comprises the following steps:

[0045] Step 1, 250mL mass concentration is that the concentrated sulfuric acid solution of 98% is packed in the concentrated sulfuric acid solution storage bottle 1, water is packed in the water / hydrogen peroxide storage bottle 2, 5g flake graphite is packed in the reactor 6, open and adjust The three-way valve 4 communicates with the concentrated sulfuric acid solution storage bottle 1 and the reactor 6 and starts the first peristaltic pump 5, so that the 250mL concentrated sulfuric acid solution all enters the reactor 6, and then adds 15g of oxidizing agent in the reactor 6 through the feeder 7. Potassium manganate carries out oxidation reaction 1h, then opens stirring paddle 8 and ultrasonic plate 11 and continues to start the first peristaltic pump 5, feeds air in reactor 6, promotes the carrying out of oxidation reaction;

[0046] Step 2. After the oxidation reac...

Embodiment 3

[0053] The preparation method of the graphene oxide of the present embodiment comprises the following steps:

[0054] Step 1, put 250mL mass concentration of 98% concentrated sulfuric acid solution into the concentrated sulfuric acid solution storage bottle 1, put hydrogen peroxide into the water / hydrogen peroxide storage bottle 2, put 20g flake graphite into the reactor 6, open and adjust The three-way valve 4 communicates with the concentrated sulfuric acid solution storage bottle 1 and the reactor 6 and starts the first peristaltic pump 5, so that the 250mL concentrated sulfuric acid solution all enters the reactor 6, and then adds 20g of oxidizing agent in the reactor 6 through the feeder 7. Potassium manganate carries out oxidation reaction 5h, then opens stirring paddle 8 and ultrasonic plate 11 and continues to start the first peristaltic pump 5, feeds air in reactor 6, promotes the carrying out of oxidation reaction;

[0055] Step 2. After the oxidation reaction descri...

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Abstract

The invention discloses a continuous preparation and purification device for graphene oxide, which includes a reactor, a concentrated sulfuric acid solution storage bottle and a water / hydrogen peroxide storage bottle connected to the reactor through a delivery pipe, and a three-way valve is arranged on the delivery pipe. Directly below and directly above are correspondingly equipped with an ultrasonic plate, a feeder, a stirring paddle, and a first lifting platform connected to the reactor through a discharge pipe, and the discharge pipe is connected to the filter column through a second conveying pipe provided with a second peristaltic pump. The filter column is connected to the graphene oxide storage bottle through the third conveying pipe provided with the third peristaltic pump; the invention also discloses a preparation method of graphene oxide: the strong acid and the oxidant are separately fed and oxidized with graphite, and then stripped and purification to obtain graphene oxide. The device of the present invention is provided with a concentrated sulfuric acid solution storage bottle, a feeder, a reactor and a filter, and realizes the continuous preparation and purification of graphene oxide; the method of the present invention improves the preparation and purification efficiency of graphene oxide, and realizes concentrated sulfuric acid Solution recovery and continuous utilization.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a continuous preparation and purification device and method for graphene oxide. Background technique [0002] Graphene is a two-dimensional crystal composed of carbon atoms with a single atomic layer thickness exfoliated from graphite. At present, there are many methods for preparing graphene, among which the chemical redox method can realize the small batch preparation of graphene and graphene oxide powder, and the redox method is the development direction of industrial preparation of graphene / graphene oxide. [0003] In the preparation process of redox method, graphite starts to oxidize under the action of strong oxidant, and at the same time, sulfate radical is inserted into the graphite layer, destroying the conjugated Π bond of graphite, and the interlayer distance of graphite increases from 0.34nm to 0.9nm~ 1nm, after further thermal expansion,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/198
CPCC01B2204/02C01B2204/04C01B32/198
Inventor 金利华白利锋冯建情李成山刘国庆张平祥
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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