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Green production method of carboxylated graphene

A carboxylated graphene, green production technology, applied in the direction of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of insufficient environmental protection of the production method, high cost of raw materials, poor modification effect, etc., and achieve mechanical property modification Good effect, simple preparation method, good modification effect

Pending Publication Date: 2021-11-23
CHANGZHOU HIGHBERY NEW NANO MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of low amount of carboxyl groups on the surface of carboxylated graphene, high cost of raw materials and poor modification effect in the prior art, the purpose of the present invention is to provide a green production method of carboxylated graphene to solve the production method of the prior art The problem of not being environmentally friendly

Method used

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  • Green production method of carboxylated graphene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Step 1, the embodiment 25kg graphene oxide by high shear emulsifying machine and a ultrasonic dispersing device running simultaneously dispersed in 600kg water to obtain a graphene oxide dispersion.

[0034] Step 2, the graphene oxide dispersion obtained in the above step after homogenization conveyed to the reaction kettle was heated to 60 ℃, 9kg of citric acid was added, 25g of concentrated sulfuric acid and polyphosphoric acid 2kg, 10H reaction, to obtain a reaction product.

[0035] Step 3, after the reaction the reaction product was added to water, subjected to suction filtration, washed, filtered to obtain the product.

[0036] Step 4, by sonication, shear, emulsification product was filtered composite dispersion manner dispersed in deionized water to give a slurry graphene carboxy, and finally freeze-dried to obtain the carboxylated graphene powder.

Embodiment 2

[0038] Step 1, the graphene oxide 25kg by sonication, shear, emulsifying compound dispersed in a distributed manner 500kg of water to obtain a graphene oxide dispersion.

[0039] Step 2, the graphene oxide dispersion obtained in the above step after homogenization conveyed to the reaction kettle was heated to 80 ℃, citric acid was added 10kg, 20g 2.5kg of concentrated sulfuric acid and polyphosphoric acid, the reaction 4h, to obtain a reaction product.

[0040] Step 3, after the reaction the reaction product was added to water, subjected to suction filtration, washed, filtered to obtain the product.

[0041] Step 4, by sonication, shear, emulsification product was filtered composite dispersion manner dispersed in deionized water to give a slurry graphene carboxy, and finally freeze-dried to obtain the carboxylated graphene powder.

[0042] like figure 1 Shows an atomic force microscope photograph carboxyl graphene prepared in Example 2, can be seen from the photograph, particle di...

Embodiment 3

[0044] Step 1, the graphene oxide 25kg by sonication, shear, emulsifying compound dispersed in a distributed manner 600kg of ethylene glycol, to obtain graphene oxide dispersion.

[0045] Step 2, the graphene oxide dispersion obtained in the above step after homogenization conveyed to the reaction kettle was heated to 80 ℃, 9.6kg of citric acid was added, 25g of concentrated sulfuric acid and polyphosphoric acid 1kg, reaction 5h, to obtain a reaction product.

[0046] Step 3, after the reaction was added to the reaction product of ethylene glycol, subjected to suction filtration, washed, filtered to obtain the product.

[0047] Step 4, by sonication, shear, emulsification product was filtered composite dispersion manner dispersed in ethylene glycol, to obtain graphene carboxy slurry, and finally freeze-dried to obtain the carboxylated graphene powder.

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Abstract

The invention discloses a green production method of carboxylated graphene, and belongs to the technical field of preparation of graphene. The preparation method comprises the following steps: dispersing graphene oxide into a solvent to obtain graphene oxide dispersion liquid; adding the graphene oxide dispersion liquid into a reaction kettle, adding citric acid, an esterifying agent and a dehydration condensation agent at the temperature of 20-160 DEG C, and reacting for 1-10 hours to obtain a reaction product; adding a solvent into the reaction product, carrying out suction filtration, and washing to obtain a suction filtration product; and re-dispersing the suction filtration product in the solvent, and drying to obtain the carboxylated graphene powder. The prepared carboxyl graphene is excellent in dispersing performance, the selected carboxylation reagent citric acid is low in price and environmentally friendly, the preparation process is simple and easy to implement, and the preparation method is suitable for large-scale industrial production.

Description

Technical field [0001] The present invention belongs to the technical field of the preparation of graphene, in particular, it relates to a method of producing a green carboxylated graphene. Background technique [0002] Graphene is a carbon atom sp 2 Hybrid orbitals are formed as a planar film of a hexagonal honeycomb lattice, a thickness of a carbon layer thickness (0.35nm), the thinnest material currently found. Graphene has unique physical and chemical properties, is the highest known material hardness, Young's modulus of more than 1000 GPa, while having good toughness; thermal conductivity of 3000W / m K; charge transport speed of 2 × 10 5 cm 2 / Vs; the specific surface area of ​​up to 2600m 2 / g. [0003] Graphene oxide (GO) is introduced into the functional groups on the graphene sheet, so as to have a function of some of the new features of graphene, comprising functional groups located on the surface of the graphene oxide carboxyl and hydroxyl groups and a hydroxyl grou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198C01B32/184B82Y30/00B82Y40/00
CPCC01B32/198C01B32/184B82Y30/00B82Y40/00C01B2204/32
Inventor 宋春丽蒋炎张荣耀邵筱珏马宏明陈润
Owner CHANGZHOU HIGHBERY NEW NANO MATERIALS TECH CO LTD
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