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Method for preparing graphene-loaded flower-like titanium dioxide composites by hydrothermal method

A titanium dioxide and composite material technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as complex processes, and achieve the effects of simple process, easy mass production, and mild reaction conditions

Inactive Publication Date: 2017-05-03
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process also requires more than two steps, and the process is complicated.

Method used

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  • Method for preparing graphene-loaded flower-like titanium dioxide composites by hydrothermal method
  • Method for preparing graphene-loaded flower-like titanium dioxide composites by hydrothermal method
  • Method for preparing graphene-loaded flower-like titanium dioxide composites by hydrothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Preparation of graphite oxide: Weigh 1.5g flake graphite and mix with 4.5g potassium permanganate, add 180mL to the mixed acid solution of sulfuric acid and phosphoric acid (volume ratio 9:1), stir and react at 30~40℃ for 1h Afterwards, the temperature was raised to 50° C. to continue the reaction for 12 h. Cool to room temperature after the reaction, slowly pour the reaction product into ice water containing 10mL hydrogen peroxide, let it stand, pour off the supernatant, filter with suction, and wash the filter cake with 5% hydrochloric acid until there is no SO in the filtrate. 42- , followed by alternating washing with deionized water and ethanol to neutrality, and vacuum drying at 50°C for 12-24 hours to obtain the required graphite oxide.

[0035] (2) Preparation of graphene / flower-like titanium dioxide composite material: Weigh 8 mg of graphite oxide and add it to a mixed solution of 20 ml of ethylene glycol and 20 ml of water, and sonicate for 10-24 hours; S...

Embodiment 2

[0037] (1) The preparation of graphite oxide is the same as in Example 1.

[0038] (2) Preparation of graphene / flower-like titanium dioxide composite material: Weigh 12 mg of graphite oxide and add it to a mixed solution of 30 ml of propanol and 10 ml of water, and sonicate for 10-24 hours. After the graphite oxide is homogenized by ultrasonication, 5 ml of an aqueous solution of polyvinylpyrrolidone with a concentration of 8 mg / ml is added thereto, and stirred for 1 h. Measure 0.5ml of titanium isopropoxide and add dropwise to 5ml of concentrated hydrochloric acid, stir and mix evenly, then add dropwise to the above graphite oxide solution, and continue to stir for 2h. Then the solution was added to a 100ml polytetrafluoroethylene reactor, reacted at 150°C for 24h, cooled to room temperature, filtered, washed, and dried to obtain a graphene-loaded flower-shaped titanium dioxide composite material. The graphene in the product is flat, and the size distribution of the flower-l...

Embodiment 3

[0040] (1) The preparation of graphite oxide is the same as in Example 1.

[0041] (2) Preparation of graphene / flower-like titanium dioxide composite material: Weigh 8 mg of graphite oxide and add it to a mixed solution of 20 ml of ethylene glycol and 20 ml of water, and sonicate for 10-24 hours; 8mg / ml cetyltrimethylammonium bromide aqueous solution, stir for 1h; measure 0.5ml titanium isopropoxide and add dropwise to 5ml concentrated hydrochloric acid, stir and mix evenly, then add dropwise to the alcoholic aqueous solution of graphite oxide , continue to stir for 2h, then add it into a 100ml polytetrafluoroethylene reactor, react at 180°C for 20h, cool to room temperature, filter, wash, and dry to obtain a graphene-loaded flower-shaped titanium dioxide composite material. Characterization found that the flower-shaped titanium dioxide in the composite material with a diameter of about 3-4um is composed of nanorods with a diameter of 35nm and a length of about 680nm, which ar...

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Abstract

The invention discloses a method for hydrothermal method preparation of a graphene-loaded flower-type titanium dioxide composite material and belongs to the technical field of composite materials. The method utilizes graphite oxide and a titanium salt as precursors, a low carbon alcohol-water mixed solvent as a medium and a surfactant as a soft template and comprises carrying out functionalization modification on the graphite oxide, adding an acid solution of the titanium salt into the modified graphite oxide, carrying out stirring so that the titanium ions are combined to the functionalized graphite oxide, adding the functionalized graphite oxide into a reactor, and carrying out a hydro-thermal reaction process so that the graphene-loaded flower-type titanium dioxide composite material is prepared by one step. The graphene-loaded flower-type titanium dioxide composite material comprises a rutile phase titanium dioxide nanometer rod-assembled flower-type structure with nanometer rod diameters of 15-35nm on the graphene surface, and through graphene connection, the structure has high specific surface area and can promote electron transmission on the material. Therefore, the graphene-loaded flower-type titanium dioxide composite material has good application prospects in the fields of photocatalysis, solar cells and gas-sensitive sensors.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and relates to a preparation method of a graphene / flower-shaped titanium dioxide composite material, in particular to a method for preparing a graphene-loaded flower-shaped titanium dioxide composite material through a hydrothermal method using graphite oxide and titanium salt as precursors . Background technique [0002] It is well known that the properties of materials are closely related to some geometric factors such as shape, size, crystal structure and so on. Therefore, the controlled synthesis of inorganic materials with well-defined morphology has become a research hotspot in the field of materials chemistry today. Among them, the microstructure composed of nanostructure units, such as the multi-level nano / microstructure assembled by nanorods, nanosheets or nanowires, has the advantages of nanomaterials—surface effect and quantum size effect while avoiding The shortcomings o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18
Inventor 莫尊理王雅雯郭瑞斌缑浩张平胡惹惹魏晓娇陈芳
Owner NORTHWEST NORMAL UNIVERSITY
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