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Water-soluble nano graphene surfactant, and synthesis method and application thereof

A surfactant and nano-graphene technology, applied in carboxylate preparation, organic chemistry, etc., can solve the problems of low economic efficiency and poor product quality, and achieve the effects of safe and convenient operation, simple synthesis method and high efficiency

Inactive Publication Date: 2016-04-20
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem solved by the present invention is to overcome the problems of low economic efficiency and poor product quality in the preparation of existing graphene, and provide a water-soluble nano-graphene surfactant that can be used to efficiently peel off graphite to prepare graphene, and the Preparation method and application of surfactant

Method used

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  • Water-soluble nano graphene surfactant, and synthesis method and application thereof
  • Water-soluble nano graphene surfactant, and synthesis method and application thereof
  • Water-soluble nano graphene surfactant, and synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Taking the water-soluble nano-graphene surfactant with the following structural formula as an example, the specific synthesis method is:

[0036]

[0037] 1. Ring closing reaction

[0038] Add 1.22g (1.56mmol) 1,3,5-tris((3,4-dibutoxy)phenylmethyl)benzene, 1.60g (5.15mmol) 3,4-di( Ethoxycarbonylmethoxy) benzaldehyde, 3.00mL (31.70mmol) acetic anhydride, 0.10g (0.62mmol) ferric chloride and 150mL dry dichloromethane, stirred at room temperature for 24 hours, in an ice-water bath, under the protection of argon , add dropwise 20mL of nitromethane solution having 4.02g (24.96mmol) of ferric trichloride dissolved therein, continue to stir and react at room temperature for 6 hours after the dropwise addition, add methanol to quench the reaction, and the reaction solution is successively washed with saturated sodium chloride aqueous solution, removed Washed with ionic water for 3 times, then dried over anhydrous sodium sulfate, filtered, and rotary evaporated to remove dic...

Embodiment 2

[0052] Taking the water-soluble nano-graphene surfactant with the following structural formula as an example, the specific synthesis method is:

[0053]

[0054] In step 3 of Example 1, add 0.50g (0.34mmol) hexabenzophenone derivative hexacarboxylic acid, 30mL aqueous solution containing 0.12g (2.04mmol) potassium hydroxide in a 50mL single-necked flask, stir at room temperature for 30 minutes, Other steps are identical with embodiment 1, obtain water-soluble nano-graphene surfactant.

[0055] The resulting product is characterized by Maxis high-resolution mass spectrometer (Germany, Bruker company), and the characterization data are as follows:

[0056] UHRMS-ESI: m / z (C 84 h 78 K 6 o 24 ) theoretical value 1704.2705, measured value 813.1725 ([M-2K] 2- ), 529.1274 ([M-3K] 3- ), 387.1042 ([M-4K] 4- ), 542.0336 ([2M-5K] 5- ).

Embodiment 3

[0058] Taking the hexabenzoquinone derivative hexacarboxylic acid sodium salt of the following synthetic structural formula as an example, the specific synthesis method is:

[0059]

[0060] 1. Ring closing reaction

[0061] In step 1 in Example 1, the 1,3,5-tris((3,4-diethoxy)phenylmethyl)benzene used was 1,3,5-tris(( 3,4-dimethoxy) phenylmethyl) benzene replacement, other steps are identical with embodiment 1, obtain the yellow solid 2,3,10,11,18,19-hexa(ethoxycarbonylmethoxy) of following structural formula base)-6,7,14,15,22,23-hexamethoxyhexabenzo[a,d,g,j,m,p]conone with a yield of 81%.

[0062]

[0063] The resulting product was characterized with an Avance type superconducting Fourier digital nuclear magnetic resonance spectrometer (Switzerland, Bruker company) and a MALDI-TOF mass spectrometer (Germany, BurkerDaltonics), and the characterization data were as follows:

[0064] 1 HNMR (400MHz, CDCl 3 +TMS)δ(ppm): 8.72(s, 2H), 8.60(s, 2H), 5.01-4.91(s, 4H), 4.37...

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Abstract

The invention discloses a water-soluble nano graphene surfactant, and a synthesis method and application thereof. The structural formula of the surfactant is disclosed in the specification, wherein M<+> represents Li<+>, Na<+>, K<+>, NH4<+>, N(CH3)4<+> or N(C2H5)4<+>, and R represents C1-C12 alkyl group. The synthesis method of the surfactant comprises the following steps: by using 3,4-di(ethoxycarbonylmethoxy)benzaldehyde and 1,3,5-tri((3,4-dialkoxy)phenylmethyl)benzene as raw materials, carrying out Friedel-Craft reaction and cyclization oxydehydrogenation reaction by using an Ac2O / FeCl3 / CH3NO2 system by a one-pot process, and carrying out hydrolysis and acid-base neutralization. The method has the advantages of cheap and accessible raw materials, mild reaction conditions and higher product yield. The water-soluble nano graphene surfactant can be used for stripping graphite to prepare single-layer fewer-layer graphene with favorable surface topography; and the stripped graphene dispersion solution has high concentration, and provides a feasible large-scale preparation method for graphene with excellent properties.

Description

technical field [0001] The invention belongs to the technical field of carbon material preparation, and in particular relates to a water-soluble nano-graphene surfactant and a synthesis method thereof, and the application of the surfactant in efficiently exfoliating graphite to prepare graphene. Background technique [0002] Graphene has a special two-dimensional structure, which is composed of planar carbon atoms arranged in a honeycomb order. Graphene has excellent electronic, thermal and mechanical properties due to its special structure and high specific surface area, and is expected to be widely used in the fields of electronic devices, energy, machinery, chemicals, special materials and medical treatment. Therefore, large-scale, efficient and economical preparation of graphene has become one of the research hotspots of scientists. [0003] At present, the preparation methods of graphene mainly include mechanical exfoliation method, epitaxial growth method, chemical va...

Claims

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Application Information

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IPC IPC(8): C07C59/66C07C51/41C01B31/04
CPCC01P2002/72C01P2004/03C01P2004/04C01P2004/61C01P2004/62C07C59/66
Inventor 魏俊发施东辉彭汗青李靖杨明瑜石先莹刘波杨奕辉程昆木鲁瑶刘恒
Owner SHAANXI NORMAL UNIV