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A method and device for producing kilogram-scale large-diameter graphite oxide/graphene oxide

A kilogram-level, large-scale technology, which is applied in the field of large-diameter graphene oxide preparation, can solve the problems of long reaction time, product repeatability and large-scale production, and many human-operated procedures, so as to reduce the reaction time cycle and strengthen intercalation. Oxidation ability, effect of improving repeat stability

Active Publication Date: 2017-12-22
SPECIAL EQUIP SAFETY SUPERVISION INSPECTION INST OF JIANGSU PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two patent reports provide good technical ideas, but the reaction time is still long, and there are many manual operations, which have a certain impact on the repeatability and large-scale production of products

Method used

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  • A method and device for producing kilogram-scale large-diameter graphite oxide/graphene oxide
  • A method and device for producing kilogram-scale large-diameter graphite oxide/graphene oxide
  • A method and device for producing kilogram-scale large-diameter graphite oxide/graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 0.5kg of 250-mesh natural flake graphite, 2.5kg of potassium permanganate and 25L of concentrated sulfuric acid fully cooled at 2°C are placed in layers in the closed reaction vessel inner wall 8 sprayed with an acid-resistant and anti-corrosion layer 14 in sequence, and fixed The bolt 3 fixes the upper cover 5 of the airtight reaction vessel and the outer wall 6 of the airtight reaction vessel to play a role of airtightness; when the constant temperature control tank 1 is opened, the temperature of the circulating temperature control medium layer 7 is regulated at 3 through the liquid inlet 15 and the liquid outlet 9. °C and maintain the reaction for 2 hours.

[0041] Subsequently, increase the temperature of the constant temperature control tank 1 to 80°C, and after maintaining it for 2 hours, stop heating, cool naturally or cool the reaction vessel to room temperature through the constant temperature control tank 1, and open the safety pressure burst valve 4 to make t...

Embodiment 2

[0044] According to the basic process described in Example 1, 1 kg of 50-mesh expandable graphite, 5 kg of potassium permanganate and 60 L of concentrated sulfuric acid fully cooled at 0 ° C were placed in the reaction vessel in order to maintain it at 1 ° C. React for 2 hours; then, increase the temperature to 70°C for 2 hours, cool and pump it into the liquid storage tank for multiple times of standing, washing, and standing, and obtain graphene oxide slurry through ultrasonic treatment. Gained graphene oxide slurry atomic mechanical microscope analysis picture is as follows image 3 As shown, it is shown that the products are all sheet-like structures with a thickness of 0.95 nm and a sheet diameter of more than 150 μm.

Embodiment 3

[0046] According to the basic process described in Example 1, 0.5kg of 200-mesh expanded graphite, 2kg of potassium permanganate and 40L of concentrated sulfuric acid fully cooled at 2°C were layered in the reaction vessel in order to maintain it at 5°C. React for 2 hours; then, increase the temperature to 60°C and maintain for 1.5 hours, cool and pump into the liquid storage tank for multiple times of standing, washing, and standing, and obtain graphene oxide slurry through ultrasonic treatment. Gained graphene oxide slurry atomic mechanical microscope analysis picture is as follows Figure 4 As shown, it is shown that the products are all sheet-like structures with a thickness of 1.1 nm and a sheet diameter of more than 70 μm.

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Abstract

The invention provides a method and device for producing kilogram-level large-flake-diameter graphite oxide / graphene oxide. The device comprises a closable flat-bottom reaction vessel, a temperature control tank, a liquid storage tank and the like, wherein the inner wall surface of the flat-bottom reaction vessel is sprayed with an anti-acid anticorrosive coating, and a circulating temperature control dielectric layer is arranged between the anti-acid anticorrosive coating and the outer wall of the vessel; the circulating temperature control dielectric layer controls the temperature through a circulating constant-temperature temperature control tank outside the vessel; a discharge port on the bottom of the vessel is connected with the external liquid storage tank; the reaction material in the vessel can be sent into the liquid storage tank through a pump; a stirrer is installed above the liquid storage tank, and both sides of the inside of the liquid storage tank are provided with ultrasonic boards; and the middle and lower parts of the liquid storage tank are respectively provided with an upper waste liquid outlet and a material discharge port. The complete device is convenient to operate, has the advantages of fewer artificial intervention factors, and high repetitiveness and stable performance of the product, and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a large-diameter graphene oxide preparation technology and a device, in particular to a method and a device for producing kilogram-scale large-diameter graphite oxide / graphene oxide. Background technique [0002] Graphene oxide is an important derivative of graphene with a large number of hydroxyl groups, carboxyl groups, epoxy groups and other groups on the edge and surface of graphene. In addition to preparing graphene through various reduction methods, it is also because of the two-dimensional The properties of nanomaterials and the chemical activity brought by the rich oxygen-containing functional groups on the surface have unique and huge application value in the fields of composite materials and biomedicine. [0003] At present, most of the preparation methods of graphene oxide need to go through the low-temperature reaction process of graphite and strong acid, the medium-temperature reaction process of adding oxidant, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/198C01B32/23C01B32/184
CPCC01B2204/04C01P2004/04C01P2004/20
Inventor 杨永强王勤生刘峥邓宏康程小豹金玲朱志鑫文煜
Owner SPECIAL EQUIP SAFETY SUPERVISION INSPECTION INST OF JIANGSU PROVINCE
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