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A core-shell structure titanium dioxide mesoporous material with cavity and preparation method thereof

A technology of core-shell structure and mesoporous materials, applied in the direction of titanium dioxide, chemical instruments and methods, titanium oxide/hydroxide, etc., can solve the difficulty of increasing the production cost of the calcination process and the control difficulty of structure repeatability, and the bonding strength of the titanium dioxide shell Insufficient, unstable and easy hydrolysis of titanium alkoxide, etc., to achieve good anti-toxin performance, good recycling, avoiding the effect of increasing production costs and environmental costs

Active Publication Date: 2019-04-30
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Soft templates usually use surfactants to form micelles or vesicles, etc., and obtain composite materials with hollow or core-shell structures after roasting, which affects many parameters and is not conducive to industrialization; hard templates mostly use organic polymer microspheres, dioxide Silicon microspheres, carbon spheres, etc. are used as carriers, and the nano-titanium dioxide is evenly distributed on the surface of the carrier in the form of a shell, but the bonding strength of the loaded titanium dioxide shell is insufficient, and the loading capacity is not high
It is also reported that a titanium dioxide material with a core-shell structure is prepared by hydrothermal method using titanium alkoxide as a titanium source, but the titanium alkoxide is unstable and easily hydrolyzed, and the reaction rate is difficult to control; Chinese patent CN201010201801.6 discloses a titanium dioxide material with a core-shell structure A method for preparing nanomaterials, which uses trivalent titanium salt and glucose as initial raw materials, and obtains titanium dioxide nanomaterials with a core-shell structure by solvothermal and calcination
This method needs to comprehensively consider the degree of removal of residual carbon in the precursor and the overall degree of damage to the core-shell structure by sintering, which increases the production cost of the calcination process and the difficulty of controlling the structure repeatability

Method used

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  • A core-shell structure titanium dioxide mesoporous material with cavity and preparation method thereof
  • A core-shell structure titanium dioxide mesoporous material with cavity and preparation method thereof
  • A core-shell structure titanium dioxide mesoporous material with cavity and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Mix ethanol and water in a ratio of 1:1 by volume to obtain an ethanol aqueous solution;

[0031] Add 2g of titanium sulfate to the ethanol aqueous solution and stir evenly to form a titanium sulfate ethanol aqueous solution; wherein the molar ratio of titanium sulfate to ethanol is 1:50;

[0032] Add ammonium chloride powder to the ethanol aqueous solution of titanium sulfate and stir to make a colorless and transparent mixed solution; wherein the molar ratio of titanium sulfate to ammonium chloride is 1:1;

[0033] Put the mixed solution into the reaction kettle, react at 150°C for 10 hours, cool to room temperature naturally, and then separate the solid phase as the precursor;

[0034] The precursor is washed with deionized water to remove acid radical ions, then dried at 100±3°C for 2 hours, and finally calcined at 500°C for 7 hours to prepare a hollow core-shell structured titanium dioxide mesoporous material;

[0035] XRD analysis of phase composition such as figure 1 As sh...

Embodiment 2

[0038] The method is the same as in Example 1, the difference is:

[0039] (1) The volume ratio of ethanol and water is 1:2;

[0040] (2) The molar ratio of titanium sulfate to ethanol is 1:60;

[0041] (3) The molar ratio of titanium sulfate to ammonium chloride is 1:2;

[0042] (4) Put the mixed solution into the reactor and react at 170°C for 5 hours;

[0043] (5) The drying time is 3 hours, the roasting temperature is 450°C, and the time is 8 hours;

[0044] The BJH adsorption pore size distribution curve and adsorption / desorption isotherm are as image 3 As shown, the specific surface area calculated by BET is 125m 2 / g; It can be seen from the figure that the most probable pore size on the BJH adsorption pore size distribution curve is in the range of 10-20nm, indicating that the product is a mesoporous material; the adsorption / desorption isotherm is a typical type IV and has a H1 type hysteresis loop It further shows that the product has a cylindrical uniform mesoporous structur...

Embodiment 3

[0046] The method is the same as in Example 1, the difference is:

[0047] (1) The volume ratio of ethanol and water is 1:3;

[0048] (2) The molar ratio of titanium sulfate to ethanol is 1:70;

[0049] (3) The molar ratio of titanium sulfate to ammonium chloride is 1:2;

[0050] (4) Put the mixed solution into the reactor and react at 180°C for 3 hours;

[0051] (5) Drying time is 2 hours, roasting temperature is 520℃, time is 6 hours;

[0052] The specific surface area of ​​the hollow core-shell structured titanium dioxide mesoporous material is 112m 2 / g, the crystal form is anatase nanocrystalline.

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Abstract

A core-shell structure titanium dioxide mesoporous material with a cavity and a preparation method thereof, belonging to the field of material technology, the grain size of the material is 10-30nm, stacked to form a core-shell structure with mesoporous structures, including a shell structure and a core structure; method It is: (1) mix ethanol and water into ethanol aqueous solution; (2) add titanium sulfate; (3) add ammonium chloride powder and stir to form a colorless and transparent mixed solution; (4) put it into the reaction kettle, React at 220°C for 1 to 10 hours, cool naturally, and separate the solid phase as a precursor; (5) Wash and dry the precursor and then roast to prepare a core-shell structure titanium dioxide mesoporous material with a cavity. The product of the present invention has the advantages of large specific surface area, strong adsorption capacity, easy diffusion and transportation of reactants / products, good anti-poison performance and recyclability; the method is simple to operate and avoids the problems of increased production costs and environmental costs.

Description

Technical field [0001] The invention belongs to the technical field of metal oxide materials, and particularly relates to a core-shell structured titanium dioxide mesoporous material with a cavity and a preparation method thereof. Background technique [0002] Increasing water pollution has promoted the research of photocatalytic degradation materials, nanocrystalline TiO 2 It has the characteristics of high catalytic activity, good chemical stability, low energy consumption, non-toxicity and safety, and low price. It is an ideal semiconductor photocatalytic degradation material. The main problem hindering its application and promotion is that the absorption efficiency of visible light is not high, and its catalytic stability and recycling capacity need to be further improved; TiO 2 The mesoporous material has high porosity, large specific surface area and activity, can absorb more organic pollutants, and can use the multiple reflection between the grains in the pores to enhance i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/08C01G23/053B01J20/06B01J20/30B82Y40/00
CPCB01J20/06B82Y40/00C01G23/0532C01G23/08C01P2002/72C01P2004/03C01P2004/30C01P2004/61C01P2006/12C01P2006/16C01P2006/17
Inventor 李明春杨浩刘俊相红钰
Owner SHENYANG POLYTECHNIC UNIV