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Method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by fast sol-gel method

A nano-titanium dioxide, sol-gel technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, nanotechnology, etc., can solve the problem of reducing the recombination rate of photogenerated electron-hole pairs, and achieve iron-nitrogen co-doped mesoporous The effect of nano-titanium dioxide with obvious red shift of ultraviolet-visible light absorption edge, large specific surface area, and reduced electron-hole recombination rate

Inactive Publication Date: 2014-07-02
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Another important problem to be solved is to reduce the recombination rate of photogenerated electron-hole pairs, that is, to increase the survival time of photogenerated holes.

Method used

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  • Method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by fast sol-gel method
  • Method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by fast sol-gel method
  • Method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by fast sol-gel method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) At room temperature, add 280mL of absolute ethanol, 10mL of deionized water, 1.5g of urea, and 0.12g of ferric nitrate nonahydrate into a beaker, then adjust the pH to 3 to 4 with 5wt% dilute nitric acid, stir, and record as A;

[0028] (2) Take a small beaker, add 20mL absolute ethanol and 10mL butyl titanate respectively, mix well, record as B;

[0029] (3) Take 0.1g polyacrylamide (molecular weight: 3 million) and add it into 100g deionized water to prepare a solution with a mass concentration of about 0.1wt%, denoted as C;

[0030] (4) Slowly drop A into B, and keep stirring. After the addition, continue to stir for 10-15 minutes, and then add 20mL of C solution dropwise. Continue to stir for 1 hour after the addition to obtain a wet gel;

[0031] (5) Put the wet gel in an oven and dry it at 80°C to remove the solvent and moisture to obtain the wet gel;

[0032] (6) Grind the xerogel in a mortar for 10 minutes, take it out and put it into a crucible, calcinat...

Embodiment 2

[0034] (1) At room temperature, add 200 mL of absolute ethanol, 10 mL of deionized water, 1.0 g of urea, and 0.05 g of ferric nitrate nonahydrate into a beaker, and then use 5 wt% dilute nitric acid to adjust the pH to 3-4, which is designated as A, stir;

[0035] (2) Take a small beaker, add 20mL absolute ethanol and 10mL butyl titanate respectively, mix well, record as B;

[0036] (3) Get 15g polyethylene glycol (molecular weight is 20,000) and add 100g deionized water, the preparation mass concentration is about the polyethylene glycol solution of 15wt%, denoted as C;

[0037] (4) Slowly drop A into B, and keep stirring, continue to stir for 10 minutes after the addition, and then slowly add 20mL of C solution dropwise. Continue to stir for 2h after adding until gelling;

[0038] (5) Put the wet gel in an oven and dry it at 90°C to remove the solvent and moisture to obtain a dry gel;

[0039] (6) Grinding the xerogel in a mortar for 15 minutes, taking it out and putting ...

Embodiment 3

[0041] This embodiment is specifically carried out according to the following steps:

[0042]1) At room temperature, first use dilute nitric acid or dilute hydrochloric acid to adjust the mixed solution of absolute ethanol, deionized water, nitrogen source, and iron source to a pH value of 3 to 4, wherein the volume ratio of absolute ethanol to water is 20:1 , then drop the absolute ethanol solution of butyl titanate at a volume ratio of 1:1, and then add an aqueous solution of polyacrylamide with a mass fraction of 0.1%, and stir for 0.1 h to obtain a gel; wherein the nitrogen source is urea, The molar ratio of titanium source to urea is 0.90:1; the iron source is ferric nitrate nonahydrate, and the molar ratio of titanium source to iron source is 1:0.001;

[0043] 2) Dry the gel in an oven at 80°C for 4 hours to remove the solvent and water to obtain a xerogel; grind the xerogel in a mortar, put it in a crucible, and calcinate and remove the template agent at a low temperatu...

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Abstract

The invention discloses a method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by a fast sol-gel method. In the method, a polymer with a molecular weight of 2*10<4>-3*10<6> is used as a template agent, and simultaneously, the template agent reacts with titanium-source hydrolysate to form a hydrogen bond so as to be fast gelated; and simultaneously, an iron source and a nitrogen source are uniformly dispersed in a uniform gel system, and then codoped mesoporous titanium dioxide is obtained by calcination. In the method, the iron element and nitrogen source are codoped and enter crystal lattices of nano titanium dioxide, wherein Fe<3+> becomes a center of capturing photoelectrons, thereby prolonging the survival time of photoholes; nitrogen atoms substitute partial oxygen atoms, so that the forbidden band width of titanium dioxide is reduced, the photoresponse range is enlarged, and titanium dioxide has a certain absorption in a visible light range; and simultaneously, on the basis of the traditional sol-gel method, the defect of long preparation period is overcome by using the method disclosed by the invention. A sample prepared by using high polymers such as polyacrylamide and the like as the template agent has mesopore duct and large specific surface area, and the photocatalysis efficiency is improved.

Description

technical field [0001] The invention belongs to the field of preparation technology of inorganic materials and photocatalytic semiconductor materials, and relates to a method for iron-nitrogen co-doped mesoporous nano-titanium dioxide, in particular to a rapid sol-gel preparation of iron-nitrogen co-doped mesoporous nano-titanium dioxide Methods. Background technique [0002] Titanium dioxide is one of the most commonly used photocatalysts. Due to its good thermal and chemical stability, it is widely used in the fields of environmental protection, photocatalytic hydrogen production, and self-cleaning materials. However, due to the good photocatalytic performance of anatase TiO 2 The forbidden band width of solar energy is 3.2eV, and only about 5% of ultraviolet rays in sunlight can be used, so the utilization rate of solar energy is low. Asahi et al. proposed for the first time to replace part of the lattice oxygen in the titanium dioxide lattice with nitrogen doping, whic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047B82Y30/00B82Y40/00
Inventor 王向东秦雷郭晓玲刘二强
Owner XI AN JIAOTONG UNIV
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