Method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate

A technology of ferric oxide and ferrous sulfate, applied in ferrous oxide, iron oxide/iron hydroxide, nanotechnology, etc., can solve the problem of high cost of ferric oxide particles, and achieve battery and capacitor capacity Obvious, the battery and capacitor capacity increase, the effect of the synthesis method is stable

Inactive Publication Date: 2020-01-14
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the deficiencies in the prior art and solve the technical problem of the high cost of mesoporous nano-ferric oxide particles for synthesizing electrodes, the present invention provides a titanium dioxide by-product, ferrous sulfate, which can be reused as a resource in iron-nickel batteries and supercapacitors. The method of utilization, the method is simple in process, realizes the reuse of ferrous sulfate by-product of titanium dioxide, reduces the cost of iron-nickel batteries and supercapacitors while increasing their capacity

Method used

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  • Method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate
  • Method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate
  • Method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate

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Effect test

Embodiment 1

[0034] (1) Dissolve the refined ferrous sulfate in deionized water according to the molar ratio of 0.2, and dissolve urea in deionized water according to the molar ratio of 0.2, then pour the two solutions into a beaker, stir and mix the reaction evenly, and the volume of the mixed solution 30% of the volume of the beaker;

[0035] (2) Seal the beaker containing the mixed liquid, leaving only one air outlet and one air inlet, and at the air inlet, inject oxygen at a flow rate of 80mL / min for 30 minutes;

[0036] (3) Seal the air inlet and outlet;

[0037] (4) Heat the sealed beaker containing the mixed solution to 85°C for 5 hours. After the reaction, the solid product is filtered out, washed 3 times, and vacuum-dried at 60°C to obtain high-crystallinity mesoporous nano-Fe 3 o 4 particles.

[0038] From figure 1 According to the X-ray diffraction spectrum, we can confirm that the obtained mesoporous nano-Fe3O4 particles belong to spinel (JCPDS: 19-0629), with high crystall...

Embodiment 2

[0045] (1) Dissolve the refined ferrous sulfate in deionized water according to the molar ratio of 0.1, and dissolve the ammonium bicarbonate in deionized water according to the molar ratio of 0.08, then pour the two solutions into a beaker, stir and mix the reaction evenly, and mix The liquid volume accounts for 45% of the volume of the beaker;

[0046] (2) Seal the beaker containing the mixed liquid, leaving only one air outlet and one air inlet, and at the air inlet, flow oxygen at a flow rate of 20mL / min for 30 minutes;

[0047] (3) Seal the air inlet and outlet;

[0048] (4) Heat the sealed beaker containing the mixed solution to 30°C for 5 hours to react. After the reaction, the solid product is filtered out, washed 3 times, and vacuum-dried at 60°C to obtain low-crystallinity mesoporous nano-Fe3O4 particles.

[0049] From figure 2 X-ray diffraction spectrum, we can determine the mesoporous nano-Fe 3 o 4 The particles belong to the spinel type (JCPDS: 19-0629), the ...

Embodiment 3

[0054] (1) Dissolve 0.3 mole of refined ferrous sulfate in deionized water, dissolve sodium bicarbonate in deionized water according to the molar ratio of 0.3, then pour the two solutions into a beaker, stir and mix the reaction evenly, and the volume of the mixed solution accounts for 50% of the volume of the beaker;

[0055] (2) Seal the beaker containing the mixed liquid, leaving only one air outlet and one air inlet, and at the air inlet, inject oxygen at a flow rate of 80mL / min for 30 minutes;

[0056] (3) Seal the air inlet and outlet;

[0057] (4) Heat the sealed beaker containing the mixed solution to 65°C for 15 hours. After the reaction, the solid product is filtered out, washed 3 times, and vacuum-dried at 60°C to obtain high-crystallinity mesoporous nano-Fe 3 o 4 particles.

[0058] From the X-ray diffraction spectrum, we can determine that the obtained mesoporous nano-Fe 3 o 4 The particles belong to the spinel type (JCPDS: 19-0629), with a pure phase and a h...

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Abstract

The invention relates to a method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate, and belongs to the technical field of inorganic functionalmaterial and electrochemical energy. The method is capable of solving a problem that synthesis cost of electrode mesoporous nano ferroferric oxide particles is high. The method comprises following steps: firstly, respectively dissolving a ferric salt and an alkaline carbon-containing compound in deionized water, uniformly mixing two obtained solutions, pouring an obtained mixed solution into a beaker, blowing oxygen into the beaker, and sealing; and at last, carrying out low-temperature heating reaction. The key points are that in the ferroferric oxide nucleation-crystallization process, CO2generated by a carbon-containing compound is used as a template to form ferroferric oxide nanoparticles with large specific surface area and adjustable size. According to the method, the cheap titanium dioxide byproduct ferrous sulfate is utilized, the use of various expensive additives is avoided, the method is suitable for large-scale production, and when the obtained Fe3O4 nanoparticle materialwith the large specific surface area is used for iron-nickel batteries and super capacitors, the capacity is remarkably improved, and the method has great economic benefits.

Description

technical field [0001] The invention belongs to the technical field of inorganic functional materials and electrochemical energy, and in particular relates to a method for preparing iron-nickel batteries and mesoporous nanometer ferric oxide particles for supercapacitors by using ferrous sulfate, a by-product of titanium dioxide. Background technique [0002] In recent years, the deepening of the energy crisis and the growing environmental problems have led to the rapid development of water-based supercapacitors and iron-nickel batteries with high safety performance and environmental friendliness. Ferroferric oxide is widely used in supercapacitors and iron-nickel batteries due to its high theoretical capacity, good electrical conductivity, and moderate volume expansion during electrochemical processes. However, commercial ferroferric oxide is generally produced by carbothermal reduction method, which has high cost and large particle size, which leads to unsatisfactory price...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08H01M4/525H01M10/30B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G49/08C01P2002/72C01P2004/04C01P2004/64H01M4/525H01M10/30Y02E60/10
Inventor 丁瑞敏吕宝亮王会香王连成
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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