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Preparation method and application of three-dimensional multistage flower-like cobalt-titanium spinel nano material

A nano-material and spinel technology, which is applied in the field of preparation of three-dimensional multi-level flower-shaped cobalt-titanium spinel nano-materials, can solve the problems of irregular shape and structure, accompanied by impurities, small specific surface area, etc., to achieve Well-developed pore structure, low cost, and large specific surface area

Inactive Publication Date: 2020-09-04
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cobalt titanium spinel (Co 2 TiO 4 ) has a stable crystal structure and is widely used in the pigment industry. It is a potential high-efficiency cobalt-based advanced oxidation catalyst. At present, there have been no research reports on this material in the field of advanced oxidation, and the existing synthesis methods are not only harsh, but also The prepared materials are often irregular in morphology, accompanied by impurity substances, and have a small specific surface area.

Method used

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  • Preparation method and application of three-dimensional multistage flower-like cobalt-titanium spinel nano material
  • Preparation method and application of three-dimensional multistage flower-like cobalt-titanium spinel nano material
  • Preparation method and application of three-dimensional multistage flower-like cobalt-titanium spinel nano material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1.25mmolCoCl·6H 2 O is dissolved in 8mL (15.625mol / L) ethylenediamine solution and makes cobalt-ethylenediamine precursor; 1.25mmol tetraisopropyl titanate is dissolved in the aqueous solution of glycerol (the use volume of glycerol is 32mL , the concentration of glycerol is 15.625mol / L, and the use volume of water is 20mL) to prepare the titanium-glycerol precursor; pour the above-mentioned cobalt-ethylenediamine precursor and titanium-glycerol precursor into 16mL In a NaOH solution with a concentration of 4mol / L, and encapsulated in a polytetrafluoroethylene reactor liner equipped with a stainless steel shell, react at 200°C for 24h, then centrifuge at 8000rpm for 3min, wash at 60°C After drying for 12 h, the three-dimensional hierarchical flower-like cobalt-titanium spinel nanomaterial Co 2 TiO 4 .

[0029] The process flow chart of above-mentioned preparation process sees figure 1 .

[0030] For the three-dimensional multi-level flower-like cobalt-titanium spin...

Embodiment 2

[0039] 1.25mmolCoC 2 o 4 4H 2 O is dissolved in 8mL (15.625mol / L) ethylenediamine solution and makes cobalt-ethylenediamine precursor; 1mmol tetraisopropyl titanate is dissolved in the aqueous solution of glycerol (the use volume of glycerol is 25.6mL , the concentration of glycerol is 15.625mol / L, and the use volume of water is 20mL) to prepare the titanium-glycerol precursor; pour the above-mentioned cobalt-ethylenediamine precursor and titanium-glycerol precursor into 20mL In a NaOH solution with a concentration of 4mol / L, and encapsulated in a polytetrafluoroethylene reactor liner equipped with a stainless steel shell, react at 185°C for 24h, then centrifuge at 4000rpm for 3min, wash at 60°C After drying for 12 h, the three-dimensional hierarchical flower-like cobalt-titanium spinel nanomaterial Co 2 TiO 4 .

Embodiment 3

[0041] 1.25mmolCo(NO 3 ) 2 ·6H 2 O was dissolved in 8mL (15.625mol / L) ethylenediamine solution to prepare cobalt-ethylenediamine precursor; 2mmol tetrabutyl titanate was dissolved in glycerol aqueous solution (the use volume of glycerol was 51.2mL, The concentration of glycerol is 15.625mol / L, and the use volume of water is 40mL) to make titanium-glycerol precursor; Pour the above-mentioned cobalt-ethylenediamine precursor and titanium-glycerol precursor 4mol / L NaOH solution, and encapsulated in a polytetrafluoroethylene reactor liner equipped with a stainless steel shell, reacted at 210°C for 24h, then centrifuged at 6000rpm for 3min, washed, and at 60°C After drying for 12 h, the three-dimensional hierarchical flower-like cobalt-titanium spinel nanomaterial Co 2 TiO 4 .

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Abstract

The invention provides a preparation method of a three-dimensional multistage flower-like cobalt-titanium spinel nano material, which comprises the following steps: dissolving a cobalt source in an ethylenediamine solution to obtain a cobalt source-ethylenediamine precursor; dissolving a titanium source in an aqueous solution of glycerol to obtain a titanium source-glycerol precursor; adding the cobalt source-ethylenediamine precursor and the titanium source-glycerol precursor into an alkaline solution, uniformly mixing, reacting at 180-220 DEG C for 12-48 hours, and carrying out centrifuging,washing and drying after the reaction is finished, thereby obtaining the three-dimensional multi-stage flower-like cobalt-titanium spinel nano material. The cobalt-titanium spinel nano material prepared by the method has a spherical flower-like microstructure, and has the characteristics of monodispersity, pure phase crystal form, developed pore structure (about 10.8nm), large specific surface area (113.6m<2>.G<-1>) and the like. The preparation method disclosed by the invention has the advantages of simple process, low cost, convenience and quickness, high yield and easiness in large-scale production.

Description

technical field [0001] The invention relates to the technical field of heterogeneous catalysis, in particular to a preparation method and application of a three-dimensional multilevel flower-like cobalt-titanium spinel nanomaterial. Background technique [0002] In recent years, due to the indiscriminate discharge of industrial wastewater and production sewage, a large number of organic pollutants have invaded the water environment, causing serious water pollution problems. Advanced oxidation technology, characterized by the generation of strong oxidizing active free radicals, has shown excellent performance and good application prospects in the treatment of organic wastewater. Among them, sulfate radicals (SO 4 – ·) has the advantages of long half-life (30-40μs) and high redox potential (2.5-3.1 V), and has attracted the attention of many researchers. Currently, cobalt-based catalysts have been shown to be the first choice for activating persulfates to generate sulfate ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00B82Y40/00B01J23/75B01J35/08B01J35/10B01J37/10C02F1/72C02F101/34C02F101/36C02F101/38
CPCC01G51/00B82Y40/00B01J23/75B01J23/005B01J37/10C02F1/725C02F1/722C01P2002/32C01P2004/32C01P2006/16C01P2006/12C02F2101/34C02F2101/36C02F2101/38B01J35/50B01J35/60B01J35/51B01J35/615
Inventor 高强李海涛王官帅
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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