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Graphite with surface modified by azido groups and preparation method thereof

A surface modification and azide-based technology, applied in the field of material chemistry, can solve the problems of poor selectivity and expensive iodine monochloride reagent, and achieve the effects of low cost, high selectivity and simple preparation method

Inactive Publication Date: 2015-05-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The disadvantages of the above method are: (1) a certain amount of iodine is also modified on the graphite surface in the form of a covalent bond while the azide group is connected, and the selectivity is poor; (2) the iodine monochloride reagent is expensive; (3) It is necessary to use an organic solvent under cooling conditions to prepare the intermediate iodine azide; (4) Two-step reaction is required

Method used

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  • Graphite with surface modified by azido groups and preparation method thereof
  • Graphite with surface modified by azido groups and preparation method thereof
  • Graphite with surface modified by azido groups and preparation method thereof

Examples

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Embodiment 1

[0025] A method for preparing a surface-modified azide-based graphite, the method comprising the following steps:

[0026] Step 1. In a 1mol / L sodium azide solution, use a three-electrode system, with graphite sheet as anode, platinum sheet electrode as cathode, and saturated calomel electrode as reference electrode, and use an electrochemical workstation to test the graphite sheet. The electrode was treated with 20mA constant current for 30min;

[0027] Step 2: Soak the graphite sheet electrode treated in Step 1 in methanol and then dry it at room temperature (25° C.) to obtain surface-modified azide-based graphite.

[0028] figure 1 with figure 2 Respectively, the X-photoelectron energy spectrum full image scan and the fine scan of N1s of the surface-modified azide-based graphite sheet prepared by the method of Example 1; it can be seen from the figure that the azide group center nitrogen atom can be seen from the figure The signal of about 404eV and the signal of the ot...

Embodiment 2

[0032] The preparation method of this embodiment is as follows:

[0033] Step 1. In a 2mol / L potassium azide solution, use a three-electrode system, with graphite sheets as anodes, platinum sheets as cathodes, and saturated calomel electrodes as reference electrodes, and use an electrochemical workstation to test the graphite sheets. Apply 0.6V constant potential to the electrode for 60min;

[0034] Step 2: Soak the graphite sheet electrode treated in Step 1 in methanol and then dry it at room temperature to obtain surface-modified azide-based graphite.

[0035] For the surface-modified azide-based graphite sheet prepared in this example, XPS characterization shows that the relative content of N elements on the surface is 1.2%.

Embodiment 3

[0037] The preparation method of this embodiment is as follows:

[0038] Step 1. In a 1.5mol / L lithium azide solution, use a three-electrode system, with graphite sheet as anode, platinum sheet electrode as cathode, and saturated calomel electrode as reference electrode, and use an electrochemical workstation to test graphite Apply a 10mA constant current to the sheet electrode for 60min;

[0039] Step 2: Soak the graphite sheet electrode treated in Step 1 in methanol and then dry it at room temperature to obtain surface-modified azide-based graphite.

[0040] XPS characterization of the surface-modified azide-based graphite sheet prepared in this example shows that the relative content of N elements on the surface is 1.5%.

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Abstract

The invention discloses graphite with the surface modified by azido groups and a preparation method thereof. The method comprises the steps: in an electrolyte solution with the azide ion concentration of 1 mol / L to 2 mol / L, employing a three-electrode system, with a graphite sheet as an anode, a platinum sheet electrode as a cathode and a saturated calomel electrode as a reference electrode, and applying a constant electric potential of 0.5-2 V or a constant current of 10-60 mA to treat the graphite sheet electrode for 10-60 min; soaking the treated graphite sheet electrode in methanol, and then drying at the room temperature to obtain the graphite sheet with the surface modified by the azido groups. The method of the invention has high selectivity, does not introduce other groups or atoms to the surface of graphite, allows the reaction to be carried out without cooling conditions, has low-price raw materials, does not employ organic solvents, and only needs one step reaction.

Description

technical field [0001] The invention belongs to the field of material chemistry, and relates to a method for modifying azide groups on the surface of graphite by an electrochemical method and the surface-modified azide group graphite prepared by the method. Background technique [0002] Compared with other electrode materials, graphite is cheaper and easier to process. It has been widely used in electroanalysis, electrolytic preparation and other research directions. As the cheapest carbon electrode material, functionalized graphite has always been a research hotspot in the field of materials. In order to expand its application range, the modification of functional molecules with excellent electrochemical properties on the surface of graphite has become a hot spot that has attracted extensive attention in recent years. For example, Anando Devadoss et al. (J.Am.Chem.Soc., 2007,129,5370-5371) disclose a method for directly modifying the graphite surface with an azido group, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/21
Inventor 纪晓唐葛忠学汪伟李陶琦毕福强刘庆黄小梧徐敏李晓宇许诚刘愆苏海鹏丁可伟肖啸卜建华郝晓春
Owner XIAN MODERN CHEM RES INST