Method for preparing graphene solution based on supercritical carbon dioxide and pyrenyl polymers

A graphene solution, carbon dioxide technology, applied in the production of graphene, nano-carbon, bulk chemicals, etc., can solve problems such as graphene, and achieve the effect of good application prospects

Inactive Publication Date: 2012-06-20
ZHENGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, there is no literature report on the integration of graphene preparation and functionalization using supercritical carbon dioxide and pyrene-based polymer properties.

Method used

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  • Method for preparing graphene solution based on supercritical carbon dioxide and pyrenyl polymers
  • Method for preparing graphene solution based on supercritical carbon dioxide and pyrenyl polymers
  • Method for preparing graphene solution based on supercritical carbon dioxide and pyrenyl polymers

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Embodiment 1

[0021] Pyrene-based polyethylene glycol (pyrene-PEG 2000 and pyrene-PEG 5000 ) preparation: raw materials: 1-pyrenylbutyric acid (purity ≥ 97%) and polyethylene glycol monomethyl ether (m PEG, Mn=2,000 and 5,000). First, polyethylene glycol monomethyl ether was vacuum-dried at 35°C for 24 hours, and then passed through polyethylene glycol monomethyl ether according to the method reported in the literature (Lim, E.-K. et al. Biomaterials, 2010, 31, 9310). The esterification reaction of the hydroxyl group of ether and the carboxyl group of 1-pyrenylbutyric acid prepares pyrene-based polyethylene glycol (pyrene-PEG 2000 and pyrene-PEG 5000 ). Pyrene-PEG 2000 and pyrene-PEG 5000 The molecular structural formula is as follows:

[0022] .

Embodiment 2

[0024] Pyrene-based polycaprolactone (pyrene-PCL 19 and pyrene-PCL 48 ) preparation: raw materials: 1-pyrenylmethanol (purity 98%) and ε-caprolactone (ε-CL, the repeating unit number of monomer caprolactone CL is 19 or 48). Firstly, ε-CL was purified by calcium hydride vacuum distillation, and then according to the method reported in the literature (Li, J. B. 2010, Polymer 51, 1301), 1-pyrenylmethanol (1.314 mmol) was used as the initiator, and ε-CL (26.28 mmol ) ring-opening polymerization to prepare pyrene-based polycaprolactone (pyrene-PCL 19 and pyrene-PCL 48 ), the polymerization reaction temperature was 115°C, and the reaction was stirred for 24h under the protection of nitrogen. Pyrene-PCL 19 and pyrene-PCL 48 The molecular structural formula is as follows:

[0025] .

Embodiment 3

[0027] Based on supercritical carbon dioxide and pyrene-PEG 2000 Preparation of graphene: 20 mg of graphite and 30.8 mg of pyrene-based polyethylene glycol 2000 (pyrene-PEG 2000) was added to 10 ml of dimethyl sulfoxide, ultrasonicated with a low-frequency ultrasonic cleaner (40 kHz, 120W) for 3 h, and the temperature was controlled at about 40 °C to obtain an off-white graphite suspension. The suspension was quickly transferred to a supercritical carbon dioxide reaction device (50 ml stainless steel autoclave) and stirred with a magnet, and carbon dioxide was injected until the pressure was 16 MPa, the temperature was 40 °C, and the pressure holding time was 6 h. Then slowly deflate and release the pressure to take out the sample and continue to sonicate with a low-frequency ultrasonic cleaner (40 kHz, 120W) for 2 h to obtain a dark gray uniform solution (with a part of the precipitate visible to the naked eye). After standing overnight, centrifuge with a centrifuge (9,000 ...

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Abstract

The invention belongs to the technical field of graphene preparation, and discloses a method for preparing graphene solution based on supercritical carbon dioxide and pyrenyl polymers. Graphites of 10 to 20 mg and the pyrenyl polymers of 15.4 to 30.8 mg are dispersed in dimethyl sulfoxide of 5 to 10 ml; then obtained suspending liquid containing the graphites and the pyrenyl polymers is put in a supercritical carbon dioxide reaction device, is stirred and reacts for 3 to 6 hours under the temperature ranging from 40 to 45 DEG C and the pressure ranging from 12 to 16 MPa, and then is processedthrough pressure relief; obtained liquid reactant is separated to remove supernatant; sediments are repeatedly washed through solvent so as to remove unreacted pyrenyl polymers, and then are dispersed in the same type of solvent renewedly; and finally, the graphites that are not exfoliated are removed, and then graphene solution is obtained. The method solves the problem that high-concentration uniform graphene solution is difficult to prepare at present, can achieve the high-yield and high-quality preparation and the functionalization of graphene in one step, can enable the output of non-defective graphene layers to be high to 51.8 wt percent, and is a simple and effective method for preparing graphene solution.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a method for preparing a graphene solution based on supercritical carbon dioxide and pyrene-based polymers. Background technique [0002] Graphene is another new nano-carbon material after fullerene and carbon nanotube, and is currently the most ideal two-dimensional nano-material. Graphene's special structure makes it have excellent performance in mechanics, electricity, optics and heat, and has great application prospects in the fields of electronics, information, energy, materials and biomedicine. However, large-scale preparation of graphene must be achieved in order to prepare useful graphene-based materials. In recent years, people have made some progress in the preparation of graphene, developed mechanical exfoliation (Novoselov, K. S. et al. Science 2004, 306, 666), crystal epitaxial growth (Berger, C. et al. J Phys Chem B 2004, 108, 19912), chemical oxidati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
CPCY02P20/54
Inventor 许群郑晓莉
Owner ZHENGZHOU UNIV
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