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Method of large quantity preparing hollow carbon nano-cage

A carbon nanocage and hollow carbon technology, which is applied in the field of preparation of nanomaterials technology, can solve the problems of difficult fluidization, abnormal operation, and low specific surface area in the production process, and achieve the goals of reducing energy consumption, easy operation, and simplified process Effect

Inactive Publication Date: 2008-07-02
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Activated carbon has a high specific surface area (>1000m 2 g -1 ), but its amorphousness determines that it is not conducive to conduction; multi-walled carbon nanotubes have a high degree of graphitization, so they have good electrical conductivity, but their specific surface area is usually low (100-200m 2 g -1 ), both of which restrict its application
Traditionally speaking, the chemical vapor deposition method is a method suitable for continuous production, but the traditional gas-solid fluidized bed can only be used for the fluidized preparation process of non-carbon particles with a diameter greater than 30 microns. For catalytic cracking In the process of preparing nanocomposite particles, due to the appearance of one-dimensional nanomaterials and easy bonding, it is very easy to cause fluidization difficulties in the production process and cannot be operated normally

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Preparation of solid carbon nanocage:

[0016] Mix the carbonyl nickel and ethanol in a volume ratio of 1:5 to obtain the reaction solution and place it in a volumetric flask; raise the temperature of the main reactor to 800°C, and blow in nitrogen, and the nitrogen flow rate is 120 liters·hour -1 ; The reaction solution is sprayed from the internal ejector of the main reactor through the electronic peristaltic pump, and the spraying speed is 100 ml·hour -1 . A solid carbon nanocage wrapped with metal particles is obtained in the product collector at the tail of the main reactor.

[0017] (2) Preparation of hollow carbon nanocage:

[0018] ① Perform air oxidation of the solid carbon nanocage obtained in step (1) at 400°C for 0.5 hours;

[0019] ②Put the mixture treated in step ① into a pure hydrochloric acid solution and vibrate ultrasonically for 1 hour;

[0020] ③The mixture obtained in the above steps is rinsed and filtered with deionized water until the solution is ...

Embodiment 2

[0023] (1) Preparation of solid carbon nanocage:

[0024] The reaction solution was uniformly proportioned by volume ratio of cobalt carbonyl and ethanol 1:10 and placed in a volumetric flask; the temperature of the main reactor was raised to 900°C, and nitrogen was introduced, and the nitrogen flow rate was 40 liters·hour -1 ; Spray the reaction solution from the internal ejector of the main reactor via the electronic peristaltic pump, and the injection speed is 50 ml·hour -1 . A solid carbon nanocage wrapped with metal particles is obtained in the product collector at the tail of the main reactor.

[0025] (2) Preparation of hollow carbon nanocage:

[0026] ① The solid carbon nanocage obtained in step (1) is subjected to air oxidation at 350°C for 1 hour;

[0027] ②Put the mixture treated in step ① into a pure hydrochloric acid solution and vibrate ultrasonically for 1.5 hours;

[0028] ③The mixture obtained in the above steps is rinsed and filtered with deionized water until th...

Embodiment 3

[0031] (1) Preparation of solid carbon nanocage:

[0032] The reaction solution was uniformly proportioned by carbonyl iron and ethanol at a volume ratio of 1:30 and placed in a volumetric flask; the temperature of the main reactor was raised to 750°C, and nitrogen was introduced, and the nitrogen flow rate was 80 liters·hour -1 ; Spray the reaction solution from the internal ejector of the main reactor via the electronic peristaltic pump, and the injection speed is 50 ml·hour -1 . A solid carbon nanocage wrapped with metal particles is obtained in the product collector at the tail of the main reactor.

[0033] (2) Preparation of hollow carbon nanocage:

[0034] ① Perform air oxidation of the solid carbon nanocage obtained in step (1) at 300°C for 2 hours;

[0035] ②Put the mixture treated in step ① into a mixed solution of pure hydrochloric acid and distilled water (V 酸 / V 水 =1:1), in the solution, ultrasonic vibration for 1.5 hours;

[0036] ③The mixture obtained in the above st...

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Abstract

The method for massively preparing hollow carbon nano cage includes the following steps: firstly, preparing solid carbon nano cage: uniformly mixing metal carbonyls liquid and low-carbons organic liquid according to a certain mixing ratio to obtain reaction solution and placing it into a volumetric flask; heating main reactor, introducing inert gas, then making the reaction solution be passed through an electronic peristaltic pump and injected into the volumetric flask by means of injector positioned in the end portion of main reactor so as to obtain solid carbon nano cage wrapped with metal particles from tail portion product collector of main reactor; then preparing hollow carbon nano cage: making the obtained solid carbon nano cage undergo the process of air oxidation treatment, then placing it in pure hydrochloric acid or pure hydrochloric acid and distilled water mixed solution and making ultrasonic oscillation, flushing the mixture obtained after ultrasonic oscillation with deionized water, filtering until the solution is neutrality or approaching to neutrality, standing still to make the solid matter be deposited and removing upper portion liquid, drying so as to obtain the invented hollow carbon nano cage.

Description

Technical field [0001] The invention relates to a preparation method in the technical field of nanomaterials, specifically, a method for preparing a large amount of hollow carbon nano cages. Background technique [0002] In recent years, more and more attention has been paid to the practical application value of carbon nanomaterials and their specific performance in applications. The hollow carbon nanocage has unique physical and chemical properties, such as forming a carbon layer on the surface of metal nanoparticles to protect the metal particles; Depositing different metal elements in the cavity to produce nano-scale electronic components has broad application prospects, which determines that the preparation can meet the requirements of continuity and transformation to meet this demand. The preparation method of hollow carbon nanocage draws on the preparation method of nano-metal composite particles, and there are two main categories: physical preparation method and chemical s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02
Inventor 王健农余帆盛赵旻
Owner SHANGHAI JIAOTONG UNIV