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Nano graphene material and preparation method and application thereof

A nano-graphene, inert gas technology, applied in nanotechnology, chemical instruments and methods, other chemical processes, etc., can solve the problems of long reaction route, difficult to obtain raw materials, harsh conditions, etc., to achieve strong green light absorption ability, good Thermal and chemical stability, mild effects

Active Publication Date: 2019-03-29
SHAANXI SCI TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The classic synthetic method has a long reaction route, the raw materials are not easy to obtain, and the conditions are relatively harsh

Method used

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  • Nano graphene material and preparation method and application thereof
  • Nano graphene material and preparation method and application thereof
  • Nano graphene material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 12 mmol of 2-phenylphenylboronic acid, 5 mmol of 1,4-dibromonaphthalene, 24 mmol of potassium carbonate, 15 mL of ethanol, and 15 mL of deionized water into the sealed tube in sequence, and inert gas (argon) for 10 min Then add 0.3 g of palladium catalyst (tetrakis(triphenylphosphine) palladium, 10%), and after passing inert gas for 5 min, seal the sealed tube and place it in an oil bath at 80-90 °C for 45-50 h.

[0039] The reaction product was extracted with ethyl acetate as the extractant, the organic layer was dried, and petroleum ether (60-90 °C) was used as the eluent to separate white solid intermediate 1 by silica gel column chromatography with a yield of 90 %; Structural characterization of Intermediate 1: Melting range 141-143 ℃; HRMS (ESI) m / z: theoretical (C 34 h 24 +H) 433.1956, Literature (C 34 h 24 +H) 433.1951.

Embodiment 2

[0041] Add 10 mmol of 2-phenylphenylboronic acid, 6 mmol of 1,4-dibromonaphthalene, 48 mmol of potassium carbonate, 30 mL of organic solvent xylene, and 30 mL of deionized water into the sealed tube in sequence, and inert gas (argon ) 10 min later, 0.3 g of palladium catalyst (palladium chloride, 10%) was added, and after passing inert gas for 5 min, the sealed tube was sealed and placed in an oil bath at 80-90 °C for 45-50 h.

[0042] The reaction product was extracted with ethyl acetate as the extractant, the organic layer was dried, and petroleum ether (60-90 °C) was used as the eluent to separate white solid intermediate 2 by silica gel column chromatography with a yield of 89 %; Structural characterization of Intermediate 2: Melting range 141-143 ℃; HRMS (ESI) m / z: theoretical (C 34 h 24 +H) 433.1956, Literature (C 34 h 24 +H) 433.1951.

Embodiment 3

[0044]11 mmol 2-phenylphenylboronic acid, 5.5 mmol 1,4-dibromonaphthalene, 30 mmol potassium carbonate, 20 mL organic solvent (a mixed solvent of tetrahydrofuran and water at a volume ratio of 4:1), and 20 mL deionized water were sequentially Put it into a sealed tube, add 0.3 g palladium catalyst (palladium acetate, 10%) after passing inert gas (argon) for 10 min, seal the sealed tube and place it at 80~90 °C after passing inert gas for 5 min React in an oil bath environment for 45-50 h.

[0045] The reaction product was extracted with ethyl acetate as the extractant, the organic layer was dried, and petroleum ether (60-90 °C) was used as the eluent to separate white solid intermediate 3 by silica gel column chromatography with a yield of 92 %; Structural characterization of intermediate 1: its melting range is measured at 141-143°C; HRMS (ESI) m / z: theoretical (C 34 h 24 +H) 433.1956, Literature (C 34 h 24 +H) 433.1951.

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Abstract

The invention discloses a nano graphene material and a preparation method and application thereof. The preparation method comprises the steps: biphenyl-2-boronic acid, 1,4-dibromonaphthalene, potassium carbonate, an organic solvent and deionized water are sequentially added into a sealing pipe, a palladium catalyst is added in an inert gas atmosphere, the inert gas atmosphere in the sealing pipe is maintained, and the sealing pipe is sealed and then placed in an oil bath environment at 80-90 DEG C to react for 45-50 h; a reaction product is extracted, and an organic layer is dried and subjected to silica-gel column chromatography to separate out an intermediate; and under the inert gas atmosphere and room temperature environment, the intermediate is added into the CH2Cl2 treated by calciumhydroxide to obtain a reaction solution, FeCl3 is dissolved in CH3NO2 and then slowly added into the reaction solution to be stirred for 2 h, then methanol and water are sequentially added into the reaction solution to extract an organic phase, and the organic phase is dried, concentrated and subjected to silica-gel column chromatography to separate out the nano graphene material. The preparationmethod is easy to operate, mild in condition and high in yield, and the prepared nano graphene materials can be applied to the aspects of green light absorption materials and semiconductor films.

Description

technical field [0001] The invention belongs to the research field of polycyclic aromatic hydrocarbons, and in particular relates to a novel nano-graphene material and its preparation method and application. Background technique [0002] In recent years, organic light emitting diodes (OLEDs) have gradually become the focus of development in the field of flat panel display research. This kind of multilayer device injects holes and electrons by applying an electric field to the anode and cathode at both ends of the device, and meets and recombines excitons in the organic light-emitting layer, and finally releases energy from the excitons to emit visible light. Compared with traditional liquid crystal displays (LCDs), organic light-emitting diodes (OLEDs) have the advantages of self-luminescence without background light source, simple process and low cost, no viewing angle problem, and flexible screen display. The most important organic light-emitting layer in OLED devices is ...

Claims

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Application Information

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IPC IPC(8): C07C15/20C07C1/26B82Y40/00C09K3/00
CPCC09K3/00B82Y40/00C07C1/26C07C15/20C07C2603/54
Inventor 张强
Owner SHAANXI SCI TECH UNIV
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