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Preparation method for biomass-based hollow carbon microtube/Ni-Co metal sulfide composite electrode material

A technology of metal sulfide and carbon microtubes, which is applied in the manufacture of hybrid capacitor electrodes, hybrid/electric double layer capacitors, etc., to achieve high price advantages, excellent electrochemical performance, and solve the effects of large-scale application difficulties

Active Publication Date: 2016-05-25
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method for biomass-based hollow carbon microtube/Ni-Co metal sulfide composite electrode material
  • Preparation method for biomass-based hollow carbon microtube/Ni-Co metal sulfide composite electrode material
  • Preparation method for biomass-based hollow carbon microtube/Ni-Co metal sulfide composite electrode material

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Embodiment 1

[0033] (1) Put 5g of biomass catkins in a tubular carbonization furnace, feed Ar as a protective gas, and control the gas flow rate at 5mlmin -1 g -1 , at 5°C min -1 The heating rate was increased to 1000°C, the temperature was kept constant for 2 hours, and the hollow carbon microtube was obtained by natural cooling to room temperature.

[0034] (2) Weigh the raw material nickel acetate Ni(CH 3 COO) 2 4H 2 O (1.2mmol), cobalt acetate Co (CH 3 COO) 2 4H 2 O (0.6mmol), thiourea (3.6mmol) is dissolved in 60ml dehydrated alcohol, makes mixed solution, then adds the mesoporous carbon microtube that 150mg above-mentioned step (1) makes in mixed solution, magnetically stirs 2h, well mixed.

[0035] (3) Transfer the above mixture to a polytetrafluoroethylene hydrothermal kettle with a volume of 100ml. The hydrothermal reaction kettle is placed in a blast oven, kept at a constant temperature of 180°C for 8h, then cooled to room temperature, and centrifuged at a speed of 9000rp...

Embodiment 2

[0037] (1) Put 5g of biomass catkins in a tubular carbonization furnace, feed Ar as a protective gas, and control the gas flow rate at 7mlmin -1 g -1 , at 7°C min -1 The heating rate was increased to 700°C, the temperature was kept constant for 1.5h, and then cooled to room temperature naturally to obtain hollow carbon microtubes.

[0038] (2) Weigh the raw material nickel acetate Ni(CH 3 COO) 2 4H 2 O (0.9mmol), cobalt acetate Co (CH 3 COO) 2 4H 2 O (0.9mmol), thiourea (4.5mmol) is dissolved in 80ml dehydrated alcohol, makes mixed solution, then adds the mesoporous carbon microtube that 200mg above-mentioned step (1) makes in mixed solution, magnetic stirring 3h, well mixed.

[0039] (3) Transfer the above mixture to a 100ml polytetrafluoroethylene hydrothermal kettle, place the hydrothermal reaction kettle in a blast oven, keep the temperature at 170°C for 10h, then cool to room temperature, centrifuge at 8000rpm for 20min, and then use Fully washed with water ethan...

Embodiment 3

[0041] (1) Put 8g of biomass catkins in a tubular carbonization furnace, 2 As a protective gas, the gas flow rate is controlled at 8mlmin -1 g -1 , at 10°C min -1 The heating rate was increased to 1000°C, the temperature was kept constant for 3 hours, and then cooled to room temperature naturally to obtain hollow carbon microtubes.

[0042] (2) Weigh the raw material nickel acetate Ni(CH 3 COO) 2 4H 2 O (0.6mmol), cobalt acetate Co (CH 3 COO) 2 4H 2 O (1.2mmol), thiourea (5.4mmol) is dissolved in 80ml ethylene glycol, makes mixed solution, then adds the mesoporous carbon microtube that 300mg above-mentioned step (1) makes in mixed solution, magnetic stirring 3h, well mixed.

[0043] (3) Transfer the above mixture to a 100ml polytetrafluoroethylene hydrothermal kettle, place the hydrothermal reaction kettle in a blast oven, keep the temperature at 200°C for 5h, then cool to room temperature, centrifuge at 7000rpm for 30min, and then use anhydrous Fully wash with ethan...

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Abstract

A preparation method for a biomass-based hollow carbon microtube / Ni-Co metal sulfide composite electrode material comprises the following steps of selecting clean and dried biomass catkins; placing the biomass catkins in a tubular carbonization stove; introducing inert gas as protective gas; carrying out high-temperature processing to prepare hollow carbon microtubes; selecting and dissolving nickel acetate, cobaltous acetate and thiourea in an organic solvent to prepare a mixed solution; adding the hollow carbon microtubes into the mixed solution, fully stirring and uniformly mixing the solution; carrying out hydrothermal reaction; naturally cooling the solution to room temperature after the reaction; and carrying out centrifuging, filtering, washing and drying to prepare the hollow carbon microtube / Ni-Co metal sulfide composite electrode material. The preparation method has the advantages of high specific capacity and excellent rate characteristic.

Description

technical field [0001] The invention belongs to a method for preparing a capacitor electrode material, in particular to a method for preparing a biomass-based hollow carbon microtube / nickel-cobalt metal sulfide composite electrode material Background technique [0002] Biomass catkins are a common environmental pollutant, especially in late spring and early summer, causing serious pollution to the natural environment, bringing a lot of inconvenience to people's travel, and causing problems such as respiratory diseases and skin allergies. However, as a natural, recyclable, and cheap biomass waste, catkins have a microstructure of biomass fibers with high and high hollowness. Utilizing the unique microstructural properties of the biomass, subjecting it to high-temperature heat treatment under inert atmosphere conditions, hollow carbon microtubes with a hollowness of more than 80% can be prepared. Useful ways. [0003] Metal sulfides such as cobalt sulfide, nickel sulfide, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/30H01G11/32H01G11/86
CPCY02E60/13H01G11/86H01G11/30H01G11/32
Inventor 宋燕王凯
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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