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Method for circularly preparing graphene oxide from waste acid resources

A technology for cyclic preparation and graphene is applied in the field of graphene to achieve the effects of saving water resources, realizing zero discharge of waste acid, and improving crystallization yield

Active Publication Date: 2018-11-20
新疆烯金石墨烯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to propose a method for the recycling of waste acid resources to prepare graphene oxide, which solves the problem of recycling waste acid in the process of preparing graphene oxide by chemical methods, and further reduces the energy consumption and cost of recycling

Method used

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Experimental program
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Effect test

Embodiment 1

[0049] The specific operation steps are as follows:

[0050] (1) prepare graphene oxide slurry:

[0051] Put 2L of sulfuric acid and phosphoric acid recovered concentrated acid, that is, mix concentrated acid into a 10L glass reactor with an oil bath jacket, slowly add 300mL of 85% concentrated phosphoric acid and 2.7L of 93% concentrated sulfuric acid, and set the temperature to 0 during stirring ℃, stirring evenly; wherein, the mass ratio of concentrated sulfuric acid to concentrated phosphoric acid is 15:1;

[0052] Slowly add 266g of potassium permanganate into the reaction kettle. During the stirring process, the temperature is controlled below 10°C and mixed evenly; the mass ratio of concentrated sulfuric acid to potassium permanganate is 30:1;

[0053] Continue to add 60g of flake graphite to the reactor, then raise the temperature of the reactor to 60°C and stir for 15h;

[0054] After the liquid was left at room temperature, 25 L of cold water at 5°C was added to di...

Embodiment 2

[0071] The specific operation steps are as follows:

[0072] (1) prepare graphene oxide slurry:

[0073] Put 3L of sulfuric acid and phosphoric acid recovered concentrated acid, that is, mix concentrated acid into a 10L glass reactor with an oil bath jacket, slowly add 200mL of 85% concentrated phosphoric acid and 1.8L of 93% concentrated sulfuric acid, and set the temperature to 0 during stirring ℃, stir evenly; the mass ratio of concentrated sulfuric acid to concentrated phosphoric acid is 10:1;

[0074] Slowly add 320g of potassium permanganate into the reaction kettle, control the temperature below 10°C during the stirring process, and mix well; the mass ratio of concentrated sulfuric acid to potassium permanganate is 25:1;

[0075] Continue to add 104 g of flake graphite to the reactor, then raise the temperature of the reactor to 55°C, and stir for 20 hours;

[0076] After placing the liquid at room temperature, add 10 L of cold water at 5°C to dilute it under agitatio...

Embodiment 3

[0091] The specific operation steps are as follows:

[0092] (1) prepare graphene oxide slurry:

[0093] Put 2.5L of sulfuric acid and phosphoric acid recovered concentrated acid, that is, mix concentrated acid into a 10L glass reactor with an oil bath jacket, slowly add 250mL of 85% concentrated phosphoric acid and 2.25L of 93% concentrated sulfuric acid, and set the temperature during stirring 0°C, stir evenly; wherein, after mixing evenly, the mass ratio of concentrated sulfuric acid to concentrated phosphoric acid is 12:1;

[0094] Slowly add 300g of potassium permanganate into the reaction kettle, control the temperature below 10°C during the stirring process, and mix well; wherein, the mass ratio of concentrated sulfuric acid to potassium permanganate is 27:1;

[0095] Continue to add 150 g of flake graphite to the reactor, then raise the temperature of the reactor to 30°C, and stir for 18 hours;

[0096] After placing the liquid at room temperature, add 5 L of cold wa...

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Abstract

The invention relates to a method for circularly preparing graphene oxide from waste acid resources. The method for circularly preparing graphene oxide from waste acid resources comprises the following steps: (1) preparing graphene oxide slurry; (2) concentrating the slurry through a ceramic filtering membrane to obtain waste acid liquid 1 and graphene concentrated slurry 1, and washing graphene concentrated slurry 1 with water through ceramic filtering equipment to obtain waste acid liquid 2 and graphene concentrated slurry 2; (3) carrying out spray drying on the graphene concentrated slurry2 to obtain graphene oxide powder; (4) distilling, concentrating and crystallizing the waste acid liquid; (5) after detecting the mass ratio of sulfuric acid and phosphoric acid in the mixed concentrated acid, adding new concentrated sulfuric acid and concentrated phosphoric acid to adjust the mass ratio, and mixing the materials uniformly for step (1). According to the method for circularly preparing graphene oxide from waste acid resources provided in the invention, the waste acid generated in the process of preparing graphene oxide is recycled according to a graded decompression distillation concentration and crystallization method to obtain mixed concentrated acid, and graphene oxide is circularly prepared by using the mixed concentrated acid as a raw material.

Description

technical field [0001] The invention belongs to the field of graphene, and in particular relates to a method for preparing graphene oxide by recycling waste acid resources. Background technique [0002] Graphene is made of sp 2 A two-dimensional material with a single atomic layer formed by the arrangement of hybridized carbon atoms. This almost completely transparent, light and flexible material is not only the thinnest and hardest nanomaterial known so far, but also has many excellent properties. For example, the thermal conductivity of graphene is about 5300W / m K, which is higher than that of natural stone. Materials such as ink, carbon nanotubes and diamond; the electron mobility of graphene at room temperature is greater than 15000cm 2 / V s, which is higher than that of carbon nanotubes and silicon crystals; the conductivity of graphene is as high as 10 -6 S / m, lower than copper or silver, is currently the material with the highest electrical conductivity and so on. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198C01D5/02C01G45/10C05D11/00
CPCC01D5/02C01G45/10C05D1/02C01B32/198C05D9/02
Inventor 杨新伟曾艳鲁娜杨子虎
Owner 新疆烯金石墨烯科技有限公司
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