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A method for efficient separation and purification of graphite oxide

A technology for separation and purification of graphite, applied in the direction of graphite, etc., can solve the problem of low efficiency of solid-liquid separation, achieve the effect of improving long settling time, simple and easy method, and high separation efficiency

Active Publication Date: 2016-04-20
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Patent CN102626591A provides a method of using different single organic solvents as purifying agents to wash graphite oxide. This method solves the swelling problem of graphite oxide in aqueous solution to a large extent, and improves the solid-liquid concentration of graphite oxide suspension to a certain extent. Separation efficiency, but its solid-liquid separation efficiency is still low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Centrifuge 5L of the synthesized graphite oxide stock solution to remove the supernatant, and collect the graphite oxide solid material.

[0022] 2. Add 5 L of mixed organic solvent to the collected graphite oxide solid material to prepare a dispersion with a concentration of 10 mg / mL, and remove the clear liquid from the uniform dispersion by centrifugation to collect the solid material. The volume ratio of the mixed organic solvent used is 50% methanol, 5% ethanol, 40% acetone, and 5% dimethylformamide.

[0023] 3. Repeat step 2 6 times until the pH of the supernatant reaches 5.6.

[0024] 4. Remove the mixed organic solvent in the finally collected solid slurry by vacuum distillation or freeze-drying to obtain graphite oxide with a purity of 99.45%.

Embodiment 2

[0026] 1. Remove the supernatant liquid from 5L of the synthesized graphite oxide stock solution by filtration, and collect the graphite oxide solid material.

[0027] 2. Add 2.5 L of mixed organic solvent to the collected graphite oxide solid material to prepare a dispersion with a concentration of 20 g / L, and remove the clear liquid from the uniform dispersion by centrifugation to collect the solid material. The volume ratio of the mixed organic solvent used is 5% methanol, 94% ethanol, 0.5% acetone, and 0.5% dimethylformamide.

[0028] 3. Repeat step 2 8 times until the pH of the supernatant reaches 5.5.

[0029] 4. Remove the mixed organic solvent in the finally collected solid slurry by vacuum distillation or freeze-drying to obtain a graphite oxide with a purity of 99.37%.

Embodiment 3

[0031] 1. Centrifuge 5L of the synthesized graphite oxide stock solution to remove the supernatant, and collect the graphite oxide solid material.

[0032] 2. Add 3L of mixed organic solvent to the collected graphite oxide solid material to prepare a dispersion with a concentration of 16.7g / L, and remove the clear liquid from the uniform dispersion by centrifugation to collect the solid material. The volume ratio of the mixed organic solvent used is 0.5% of methanol, 10% of ethanol, 4.5% of acetone, and 85% of dimethylformamide.

[0033] 3. Repeat step 2 7 times until the pH of the supernatant reaches 5.7.

[0034] 4. Remove the mixed organic solvent in the finally collected solid slurry by vacuum distillation or freeze-drying to obtain a graphite oxide with a purity of 99.52%.

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PUM

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Abstract

The invention discloses a method for efficient separation and purification of a graphite oxide. The method comprises the following steps: removing clear liquid from the synthesized graphite oxide stock solution by separation, and collecting solid material; adding a mixed organic solvent to the solid material to prepare graphite oxide dispersion; separating the graphite oxide dispersion and collecting the solid material; removing the mixed organic solvent out of the finally collected solid slurry by using a vacuum distillation or frozen drying method, so as to obtain the high-purity graphite oxide. The method is high in separation efficiency, low in energy consumption, simple and feasible.

Description

technical field [0001] The invention relates to a method for highly efficient separation and purification of graphite oxide. Background technique [0002] Graphene has excellent mechanical, thermal, optical, and electrical properties, and has broad application prospects in many fields such as lithium-ion batteries, supercapacitors, catalysis, and coatings. The large-scale controllable preparation of graphene is the premise and foundation of its commercial application. At present, the preparation of graphene by chemical exfoliation has the advantages of easy availability of raw materials, low cost, and mature technology, and has been used as one of the main technical routes for mass production of graphene. [0003] For the process route of preparing graphene by oxidation intercalation and exfoliation, the purification of intermediate graphite oxide is the speed-limiting link of the process, which directly affects the production efficiency and product purity of graphene indus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/23
Inventor 陈成猛贾蓉蓉王大力孔庆强蔡榕王炜苏小威李元智
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI