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Method for preparing boron carbon nitride nanotube with high oxygen reduction catalytic activity

A catalytic activity, boron carbon nitrogen technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problem of no oxygen reduction catalytic activity, etc., and achieve excellent oxygen reduction catalytic activity, operation Simple process and good tube shape

Active Publication Date: 2014-06-11
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Reported in "Journal of American Chemical Society" (J.Am.Chem.Soc.2000,122(49):12383-12384) and "Inorganic Chemistry" (Inorg.Chem.2004,43(2):822-829) Liao Qian et al. and Xie et al. successfully prepared carbon nanotubes and boron nitride nanotubes by solvothermal synthesis at a temperature of 350-400°C; in "Canadian Chemistry" (Can.J.Chem.2010,88(12) :1256-1261) reported that Sun et al. synthesized carbon-boron nitride-carbon sandwich nanotubes by solvothermal method, but the synthesized tubes were disordered nanotubes and did not have oxygen reduction catalysis. active

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  • Method for preparing boron carbon nitride nanotube with high oxygen reduction catalytic activity
  • Method for preparing boron carbon nitride nanotube with high oxygen reduction catalytic activity
  • Method for preparing boron carbon nitride nanotube with high oxygen reduction catalytic activity

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Embodiment 1

[0023] Distill the analytically pure acetonitrile solvent at 65°C to obtain pure anhydrous acetonitrile, which is sealed and ready for use; in a nitrogen-protected glove box, 2.5 grams of analytically pure NaN 3 , 2.5 grams of analytically pure NH 4 BF 4 , 0.42 g of CTAC and 13 ml of the above-mentioned pure anhydrous acetonitrile were added successively to 16 ml of benzene, stirred for 15 minutes, and the mixture was put into a stainless steel reactor with a volume of 40 ml and sealed; Under heating for 8 hours, then the reaction kettle was naturally cooled to room temperature, and the mixture was taken out. The above mixture was washed four times with absolute ethanol, dilute hydrochloric acid and distilled water successively, filtered, and then vacuum-dried at 100° C. for 6 hours to obtain directional grown boron carbon nitrogen nanotubes with high catalytic activity for oxygen reduction.

[0024] like figure 1 As shown, all nanotubes grow in the same direction, and the ...

Embodiment 2

[0028] Distill the analytically pure acetonitrile solvent at 70°C to obtain pure anhydrous acetonitrile, which is sealed and ready for use; in a nitrogen-protected glove box, 1.8 grams of analytically pure NaN 3 , 2.1 grams of analytically pure NH 4 BF 4 , 1.0 gram of CTAB and 1ml of the above-mentioned pure anhydrous acetonitrile were added successively in 8ml of benzene, stirred for 25 minutes, the mixture was put into a stainless steel reaction kettle with a volume of 15ml, and sealed; Under heating for 36 hours, then the reaction kettle was naturally cooled to room temperature, and the mixture was taken out. The above mixture was washed three times successively with absolute ethanol, dilute hydrochloric acid and distilled water, filtered, and then vacuum-dried at 60° C. for 10 hours to obtain directional grown boron carbon nitrogen nanotubes with high catalytic activity for oxygen reduction.

[0029] like Figure 4 As shown, all the nanotubes grow in the same direction,...

Embodiment 3

[0034] Distill the analytically pure acetonitrile solvent at 75°C to obtain pure anhydrous acetonitrile, which is sealed and ready for use; in a nitrogen-protected glove box, 3.0 grams of analytically pure NaN 3, 4.5 grams of analytically pure NH 4 BF 4 , 0.5 gram of CTAC and 4ml of the above-mentioned pure anhydrous acetonitrile were added successively in 24ml of benzene, stirred for 30 minutes, the mixture was put into a stainless steel reaction kettle with a volume of 40ml, and sealed; Under heating for 24 hours, then the reaction kettle was naturally cooled to room temperature, and the mixture was taken out. The above mixture was washed 5 times with absolute ethanol, dilute hydrochloric acid and distilled water successively, filtered, and then vacuum-dried at 80° C. for 8 hours to obtain directional grown boron carbon nitrogen nanotubes with high catalytic activity for oxygen reduction.

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Abstract

The invention discloses a method for preparing a boron carbon nitride nanotube with high oxygen reduction catalytic activity. The method mainly comprises the following steps of: sequentially adding 6-18 weight percent of analytically pure NaN3, 6-21 weight percent of analytically pure NH4BF4, 1-10 weight percent of analytically pure surfactant and 8-25 weight percent of analytically pure purely anhydrous acetonitrile into benzene under nitrogen protection, and stirring for 15 to 30 minutes; adding the mixture into a stainless steel reaction kettle for sealing, putting the reaction kettle in a crucible furnace, heating at the temperature of 300-600 DEG C for 8-36 hours, naturally cooling the reaction kettle to room temperature, and taking out the mixture; and sequentially washing the mixture for 3-5 times by using absolute ethyl alcohol, diluted hydrochloric acid and distilled water, filtering, and performing vacuum drying on the powder in a vacuum drying box at the temperature of 60-100 DEG C for 6-10 hours. The method is simple in process, moderate in reaction conditions and low in cost, a metal catalyst is not required, the prepared boron carbon nitride nanotube has excellent oxygen reduction catalytic activity, and large-scale production can be realized.

Description

technical field [0001] The invention belongs to the field of fuel cell oxygen reduction catalysts, in particular to a preparation method of boron carbon nitrogen nanotubes. Background technique [0002] Fuel cell is one of the key development directions in the field of new energy. It is a power generation device that directly converts chemical energy into electrical energy. It has the advantages of high energy density, high energy conversion efficiency, and no pollution. The oxidant used in fuel cells is generally oxygen, so the oxygen reduction reaction constitutes an important reaction in the operation of fuel cells. The metal with excellent electrocatalytic activity for oxygen reduction reaction is metal platinum (Pt), but platinum is an expensive metal, and it also has CH 3 The disadvantages of OH / CO tolerance and poor long-term operation stability greatly limit its practical application in fuel cells. Therefore, the research and development of low-noble metal and non-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 高发明周军双李娜徐子明侯莉
Owner YANSHAN UNIV
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