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Nitrogen-doped carbonized bacterial cellulose loaded nano-platinum electrode material and preparation method thereof

A technology of bacterial cellulose and bacterial cellulose membrane is applied in the field of preparation of nitrogen-doped carbonized bacterial cellulose-loaded nano-platinum electrode materials, which can solve the problems of complex preparation process, volatile, expensive equipment, etc., and increase the number of active sites. , the effect of increasing the electrical conductivity and improving the utilization rate

Active Publication Date: 2017-01-04
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[Adv.Funct.Mater.2014,24,5104-5111] reported a method of mixing carbon source and phosphate followed by carbonization to prepare heteroelement-doped carbon fibers. This method has the advantages of mild synthesis conditions and low energy consumption. , but due to the collapse and stacking of a large number of voids due to the doping of nitrogen elements, the specific surface area and pore volume of the material are small, which is not conducive to further application
[NanoEnergy 2015,11,366-376] reported a 3 A method for carbonizing bacterial cellulose at high temperature in an air atmosphere, the prepared material has a super high specific surface area (916m 2 g -1 ), but its operation process is complex, the raw material conditions are harsh, volatile and have a pungent smell, and it is difficult to produce on a large scale
Most of the current methods for preparing nitrogen-doped carbon materials involve complex preparation processes, expensive equipment, or harsh conditions such as dangerous chemical reagents (concentrated sulfuric acid, etc.), which are difficult to mass-produce

Method used

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  • Nitrogen-doped carbonized bacterial cellulose loaded nano-platinum electrode material and preparation method thereof
  • Nitrogen-doped carbonized bacterial cellulose loaded nano-platinum electrode material and preparation method thereof
  • Nitrogen-doped carbonized bacterial cellulose loaded nano-platinum electrode material and preparation method thereof

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preparation example Construction

[0026] A kind of preparation method of nitrogen-doped carbonized bacterial cellulose supported nano-platinum electrode material of the present invention, the preparation flow chart is as follows figure 1 shown, including the following steps:

[0027] In the first step, the bacterial cellulose fermented by Acetobacter xylinum is pretreated to obtain a clean bacterial cellulose film, and the bacterial cellulose aerogel is obtained after freeze-drying;

[0028] The second step is to divide the airgel, soak it in urea solution, ultrasonically make the nitrogen source urea fully adsorbed into the bacterial cellulose, and let it stand for 20-24 hours; take out the urea / bacterial cellulose gel and freeze-dry it;

[0029] The third step is to heat the freeze-dried urea / bacterial cellulose gel to 600°C-1000°C for 2 hours, and obtain nitrogen-doped carbonized bacterial cellulose nanofibers after high-temperature carbonization;

[0030] The fourth step is to disperse the obtained nitrog...

Embodiment 1

[0032] Heat the bacterial cellulose film obtained by the static fermentation of Acetobacter xylinum with 0.3% NaOH at 80°C for 3 hours, wash it with tap water until it becomes neutral; cut it into small pieces with a regular size of 2cm×2cm with scissors, place them in a freeze dryer and dry them for 24 hours. Take out and soak in 2.5% urea solution, ultrasonic for 30 minutes, then stand for 24 hours, and freeze-dry for 12 hours to obtain urea / bacterial cellulose airgel. Place in a tubular muffle furnace, raise the temperature to 800°C at a heating rate of 2°C / min, and keep the temperature for 2 hours to obtain nitrogen-doped carbonized bacterial cellulose. Take 20 mg of the product, disperse it in 80 mL of ethylene glycol solution, ultrasonicate for 30 min, then add 540 μL of chloroplatinic acid aqueous solution to adjust the pH to 9, transfer the sample to a three-neck flask, heat to 90°C and reflux for 3 h. Centrifuge the reaction product at a speed of 10000r / min for 15min,...

Embodiment 2

[0035]Heat the bacterial cellulose film obtained by the static fermentation of Acetobacter xylinum with 0.2% NaOH at 80°C for 3 hours, wash it with tap water until it becomes neutral; cut it into small pieces with a regular size of 2cm×2cm with scissors, place it in a freeze dryer and dry it for 24 hours, Take it out and soak it in 2.0% urea solution, sonicate for 30 minutes, then let it stand for 24 hours, and freeze-dry for 12 hours to obtain a white airgel. Place in a tubular muffle furnace, raise the temperature to 800°C at a heating rate of 2°C / min, and keep the temperature for 2 hours to obtain nitrogen-doped carbonized bacterial cellulose. Take 20 mg of the product, disperse it in 80 mL of ethylene glycol solution, ultrasonicate for 30 min, then add 540 μL of chloroplatinic acid aqueous solution to adjust the pH to 9, transfer the sample to a three-neck flask, heat to 90°C and reflux for 3 h. Centrifuge the reaction product at a speed of 10000r / min for 15min, pour off t...

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Abstract

The invention discloses a preparation method of a nitrogen-doped carbonized bacterial cellulose loaded nano-platinum electrode material. The material is obtained through the following steps: taking bacterial cellulose as a carbon source, soaking in a urea solution, and preparing nitrogen-doped carbide bacterial cellulose after freeze drying and carbonization. In-situ reduced and loaded nano-platinum particles on fiber are extremely high in methanol oxidation activity. According to the nitrogen-doped carbonized bacterial cellulose prepared by using a soaking-freeze-drying-carbonization technology, the method is mild, the material sources are abundant, the cost is low, and the controllability is high; meanwhile, the content and variety of doped nitrogen can be further regulated and controlled by changing the carbonization temperature; for the nano-scale carbonized bacterial cellulose fiber obtained after carbonization, the original three-dimensional network structure characteristics of the bacterial cellulose can be maintained, the bacterial cellulose is large in specific surface area and is a carbon carrier material with excellent performance, the nano-platinum particles are loaded by using the bacterial cellulose, the dimensions of the nano-platinum particles in an obtained compound are only 2.0 nm, the distribution is uniform, and the utilization rate of metallic platinum can be improved to a great extent.

Description

technical field [0001] The invention belongs to the field of nanomaterials, and in particular relates to a preparation method of nitrogen-doped carbonized bacterial cellulose-loaded nano-platinum electrode material. Background technique [0002] Bacterial cellulose has a wide range of sources, is cheap and easy to obtain, and has a uniform and controllable shape. It is a renewable and environmentally friendly biomass material. Carbonized bacterial cellulose is a carbonized material processed by high-temperature annealing of bacterial cellulose under an inert atmosphere. In recent years, carbonized bacterial cellulose has attracted extensive attention, especially in the field of energy storage materials, because it can retain the three-dimensional network nanofibers, excellent electrical conductivity and chemical stability of its precursor bacterial cellulose. However, the carbonized materials prepared by high-temperature annealing have fewer oxygen-containing functional gro...

Claims

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Application Information

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IPC IPC(8): H01M4/88H01M4/92B82Y30/00
CPCB82Y30/00H01M4/8825H01M4/926Y02E60/50
Inventor 孙东平袁凡舒黄洋陈春涛范孟孟张衡杨加志
Owner NANJING UNIV OF SCI & TECH
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