Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of organic graphene nano-tubes with titanium dioxide modified on the surface

A titanium dioxide, surface modification technology, applied in nanotechnology, chemical instruments and methods, nanotechnology and other directions for materials and surface science, to achieve the effect of strong stability and enhanced energy transmission efficiency

Active Publication Date: 2018-01-19
DONGHUA UNIV
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These research results provide a theoretical basis and synthesis ideas for the functionalization and application of graphene nanotubes, but so far the research is mainly on the introduction of organic functional groups, and there are few reports on the development of inorganic-graphene tube composites

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of organic graphene nano-tubes with titanium dioxide modified on the surface
  • Preparation method of organic graphene nano-tubes with titanium dioxide modified on the surface
  • Preparation method of organic graphene nano-tubes with titanium dioxide modified on the surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of compound 2

[0042] Add triethylene glycol (2g, 13.3mmol, 1eq) into a 250mL two-necked flask, dissolve it in 20mL THF, pump for ventilation, protect with Ar, and slowly add 1.5mL of pyridine dropwise at 0°C. TsCl (3.01g, 15.84mmol, 1.3eq) was dissolved in 50mLTHF, and the reaction solution was slowly added dropwise, and stirred overnight. After acidification, the reaction solution was extracted with DCM, then washed with saturated NaCl, and most of the solvent was evaporated by rotary evaporation, and an appropriate amount of silica gel was added for dry column chromatography and eluent (EA) to obtain 4 g of white liquid, namely compound 2, the yield 98%.

[0043] 1 H NMR (400MHz, CDCl 3 )δ7.78(d,J=8.3Hz,2H),7.33(d,J=8.1Hz,2H),4.17–4.12(m,2H),3.68(dt,J=4.6,3.8Hz,4H), 3.60–3.52(m,6H),2.60(s,1H),2.43(s,3H).

[0044] MS-EI (C 13 h 20 o 6 S) Theoretical value [M] + : m / z 304.10. Measured value: 304.6.

Embodiment 2

[0046] Preparation of compound 3

[0047] Compound 2 (800mg, 2.63mmol, 1eq), p-bromobiphenol (1.63g, 6.58mmol, 2.5eq), K 2 CO 3 (3.63g, 26.3mmol, 10eq), 25mL of dimethylformamide, and gas exchange three times under the protection of Ar. After reacting at 100°C for 24 hours, add p-bromobiphenol, dimethylformamide and a small amount of 18-crown ether, and react for another 24 hours. Spin to dry, extract with dichloromethane, wash with water three times, dry over anhydrous magnesium sulfate, and elute with dichloromethane and ethanol sequentially after column chromatography to obtain 600 mg of white solid, namely compound 3, with a yield of 65%.

[0048] 1 H NMR (400MHz, CDCl 3 )δ7.52(d, J=8.0Hz, 2H), 7.47(d, J=8.2Hz, 2H), 7.40(d, J=8.0Hz, 2H), 6.98(d, J=8.2Hz, 2H) ,4.18(t,J=4.6Hz,2H),3.89(t,J=4.6Hz,2H),3.77–3.69(m,6H),3.65–3.59(m,2H).

[0049] MS-EI (C 18 h 21 BrO 4 ) theoretical value [M] + : m / z 380.06. Measured value: 381.2.

Embodiment 3

[0051] Preparation of Compound 4

[0052] After adding compound 3 (600mg, 1.58mmol, 1eq) and acetic anhydride (217mg, 2.25mmol, 1.5eq) into a 50mL two-neck flask, dichloromethane was added to dissolve it, and the gas was exchanged three times under the protection of Ar. Pyridine (0.2mL, 1.5eq) was added at 0°C, and after 20min, it was moved to room temperature and reacted overnight. After raising the temperature to 60°C and refluxing for 3 hours, it was washed three times with saturated ammonium chloride aqueous solution, dried over anhydrous magnesium sulfate, and spin-dried. After column chromatography, dichloromethane was eluted to obtain 530 mg of white solid, that is, compound 4, and the yield was 80%.

[0053] 1 H NMR (400MHz, CDCl 3 )δ7.52(d, J=8.0Hz, 2H), 7.47(d, J=8.2Hz, 2H), 7.40(d, J=8.0Hz, 2H), 6.98(d, J=8.2Hz, 2H) ,4.18(t,J=4.6Hz,2H),3.89(t,J=4.6Hz,2H),3.77–3.69(m,6H),3.65–3.59(m,2H).

[0054] MS-EI (C 20 h 23 BrO 5 ) theoretical value [M] + : m / z 423.30....

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of organic graphene nano-tubes with titanium dioxide modified on the surface. The preparation method comprises: preparing a hexabenzocoronene compound with introduced carboxyl by using triglycol as a raw material, ultrasonically dissolving the obtained compound in a solvent, forming a nano-tubular structure A-GNT through self-assembly, hydrolyzing theester groups on the inner surface and the outer surface of the nano-tubes into the hydroxyl groups, adding Ti(OiPr)4, and carrying out a transesterification reaction on the hydroxyl groups on the surface and the titanate to obtain the organic graphene nano-tubes A-GNT-TiO2 with titanium dioxide modified on the surface. According to the present invention, the organic graphene nano-tubes A-GNT-TiO2with titanium dioxide modified on the surface can be used as the functional graphene material so as to perform photocatalytic reactions in photoelectric materials and solar cell materials; and the preparation method can provide the scientific basis for the improvement of the self-assembly theory.

Description

technical field [0001] The invention belongs to the field of nano-supramolecular materials, in particular to a method for preparing organic graphene nanotubes whose surface is modified with titanium dioxide. Background technique [0002] As a new type of two-dimensional planar nanomaterial, graphene has become a research frontier and hotspot that has attracted much attention since its discovery in 2004. However, since graphene does not contain any unstable bonds, its chemical stability is very high, the surface is in an inert state, and there is a strong van der Waals force between the sheets, which is easy to aggregate. Moreover, the interaction between graphene and other solvents and other media is weak, and it is difficult to dissolve in water and commonly used organic solvents. These problems greatly limit the further research and application of graphene. At this stage, the research on its functionalization has just begun, and the surface functionalization of graphene i...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B82Y30/00B82Y40/00
Inventor 李贤英金武松张灯青李荣胡捷娜张权
Owner DONGHUA UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com