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Preparation method of ferro-doped TiO2/SiO2 aerogel microball

A technology of airgel and microspheres, which is applied in the fields of chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., which can solve the constraints of use efficiency and application range, low utilization rate of visible light, uneven filling, etc. problem, to achieve the effect of easy filling, low price, uniform and controllable shape

Inactive Publication Date: 2007-05-23
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as "a kind of TiO 2 / SiO 2 Airgel preparation method" (Chinese invention patent application number: 200310109507.2, publication number: CN1546226), however prepared TiO 2 / SiO 2 Aerogels are mostly irregular massive solid materials, which makes TiO 2 / SiO 2 In practical applications, airgel has disadvantages such as uneven filling and difficult recycling, which restrict its use efficiency and application range.
"A TiO 2 / SiO 2 Airgel pellets and their preparation method" (Chinese invention patent application number: 200310109498.7, publication number: CN1546225) will TiO 2 / SiO 2 Airgel made of millimeter-scale TiO with regular shape and controllable particle size 2 / SiO 2 Airgel beads greatly expand the application range of this nanoporous material in the fields of heat insulation, chromatographic separation and catalysis, but its excessive particle size restricts its application
Moreover, the existing conventional TiO 2 material or TiO 2 / SiO 2 The material can only be photocatalyzed under ultraviolet light, and the ultraviolet light in sunlight is less than 5%, so the utilization rate of visible light is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 16g of 98% TiOSO 4 with 0.84g FeCl 3 Add to 500ml deionized water, stir to dissolve completely, and obtain 0.2mol L -1 Fe-doped TiOSO 4 Solution, at 600r·min -1 Stir at a stirring rate of 5%, dropwise add ammonia water with a mass fraction of 5%, until the pH value of the solution is 7-9, fully wash the obtained precipitate with deionized water, until there is no SO in the washing liquid 4 2- until the ion is detected. Add 70mL of deionized water to the washed precipitate to disperse, then add 31mL of 1.6mol·L -1 Nitric acid, stirred at 50°C for 5 hours to get iron-doped titanium sol.

[0022] Take 10mL of silica sol (25%, w / w), add 1mL of nitric acid with a mass fraction of 5%, and add 5mL of absolute ethanol under stirring conditions to obtain SiO 2 Alcohol sol.

[0023] Mix the iron-doped titanium sol and silica sol prepared above in a ratio of 1:5, add an appropriate amount of formamide, and the amount of formamide is TiO 2 and SiO 2 25% of the total...

Embodiment 2

[0028] Weigh 16 g of 98% TiOSO 4 with 8.4g FeCl 3 Add to 500mL deionized water, stir to dissolve completely. at 1200r min -1 Aqueous ammonia with a mass fraction of 20% was added dropwise under stirring at a stirring rate of 20% until the pH value of the solution was 7-9. Wash the resulting precipitate thoroughly with deionized water until there is no SO in the wash 4 2- until the ion is detected. Add 70mL of deionized water to the washed precipitate to disperse, then add 31mL of 1.6mol·L -1 nitric acid, stirred at 90°C for 20 hours to obtain iron-doped titanium sol.

[0029] Take 10 mL of silica sol (25%, w / w), add 40 mL of 5% nitric acid, and add 50 mL of absolute ethanol under stirring. The above prepared iron-doped titanium sol and silica sol are TiO in molar ratio 2 : SiO 2 = 1:8 ratio mixed evenly, the added mass is TiO 2 and SiO 2 40% of the total amount of formamide at 1200r min -1 Stirring at a stirring rate of 1000 to obtain TiO with uniformly dispersed p...

Embodiment 3

[0032] Weigh 16 g of 98% TiOSO 4 with 5.6g FeCl 3 Add to 500mL deionized water, stir to dissolve completely. At 1000r·min -1 Aqueous ammonia with a mass fraction of 10% was added dropwise under stirring at a stirring rate of 100% until the pH value of the solution was 7-9. Wash the resulting precipitate thoroughly with deionized water until there is no SO in the wash 4 2- until the ion is detected. Add 70mL of deionized water to the washed precipitate to disperse, then add 31mL of 1.6mol·L -1 nitric acid, stirred at 60°C for 10 hours to obtain iron-doped titanium sol.

[0033] Take 10 mL of silica sol (25%, w / w), add 25 mL of 5% nitric acid, and add 19 mL of absolute ethanol under stirring. The iron-doped titanium sol and silica sol prepared above were pressed by n(TiO 2 ):n(SiO 2 )=1:4 ratio and mix evenly, the amount of addition is TiO 2 and SiO 2 20% formamide of the total mass, at 1000r·min -1 Stirring at a stirring rate of 1000 to obtain iron-doped TiO with un...

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Abstract

The invention relates to a method for preparing TiO2 / SiO2 aerogel micro ball doping with iron, wherein it dissolves TiOSO4 and FeCl3 into deionized water, adjusts pH value to 7-8, to obtain deposits; washes deposits, adds nitric acid solution, mixes at 50-90Deg. C to obtain TiO2 sol doping with iron; adds nitric acid into silicasol and absolute ethyl alcohol to prepare SiO2 alcohol sol; then mixes titanium sol with SiO2 alcohol sol at 1:3-8 volume ratio, adds formamide, mixes to obtain TiO2 / SiO2 composite sol; mixes skellysolve C / skellysolve B, siban 80, tuwen 85, butanol / hexanol at 1000:1-10:0.1-1:25-100, to obtain the oil phase; then adds TiO2 / SiO2 composite sol into oil phase, to make pH at 7-10, to obtain the TiO2 / SiO2 gel micro ball; washes with acetone and dries, to obtain the TiO2 / SiO2 aerogel micro ball at 10-200micrometer diameter. The invention has simple process and low cost.

Description

technical field [0001] An iron-doped TiO 2 / SiO 2 Preparation method of airgel microspheres, involving a micron-sized TiO with visible light photocatalytic properties 2 / SiO 2 Preparation technology of airgel microspheres. Background technique [0002] TiO 2 Due to the high specific surface area, airgel has strong adsorption, and TiO 2 Films have higher photocatalytic activity than powders. while TiO 2 / SiO 2 When airgel is used as a photocatalyst due to the introduction of SiO 2 The colloidal particles have significantly improved the specific surface area, transparency, thermal stability, and skeleton strength. Its activity in the photocatalytic treatment of cyanide, pyridine, and phenolic pollutants in the liquid phase is significantly better than that of Ordinary TiO 2 airgel. Such as "a kind of TiO 2 / SiO 2 Airgel preparation method" (Chinese invention patent application number: 200310109507.2, publication number: CN1546226), however ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J21/08B01J23/74B01J35/08
Inventor 甘礼华田辞刘明贤庞颖聪陈龙武
Owner TONGJI UNIV
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