CN1327878A - Process for preparing visual light reaction type nm TiO2-base optical catalyst - Google Patents
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Abstract
A process for preparing visual light reaction type nanometer-level TiO2-base photo-catalyst, which can decompose he harmful gas in room, the polluing gas in atmosphere and organic pollutant in water under the radiation of 400-700 nm visual light, features that the improved cosolvent doping method and high-temp calcination are used, polyethanediol is added, and the preparing time is shortened to prevent growth of particles. Said photo-catalyst features 10-20 nm of grain size, high photo-catalysis activity and energy conversion efficiency, and low cost.
Description
The present invention relates to a kind of photochemical catalyst, particularly a kind of preparation method of metal-doped visual light reaction type nm TiO 2-base optical catalyst.
Under the ultraviolet ray irradiation, titanium dioxide (TiO
2But) organic pollution in photochemical catalyst catalytic decomposition indoor harmful gas, atmosphere pollution gas and the water, but this titanium dioxide optical catalyst can only be by wavelength less than 400nm (~387.5nm) ultraviolet ray excited, and this part ultraviolet light only accounts for 4-6% in the solar radiation total amount that arrives ground, and change in time obviously, as artificial ultraviolet light sources such as applying high voltage mercury lamps, energy consumption is too big.If can be with TiO
2The spectrum of photochemical catalyst utilizes range expansion to arrive visible region, then can make full use of solar source, if with excitation wavelength from the 387.5nm red shift to~443nm, then the sunshine utilization rate can be increased to tens percent by a few percent, can reduce equipment investment and operating cost significantly, apply for large-scale industrialization and lay scientific basic.On the other hand, since nano material exclusive quantum size effect and skin effect, nano titanium dioxide photocatalyst has higher photocatalysis efficiency than conventional titanium dioxide optical catalyst, therefore, can be by the titanium dioxide optical catalyst of the crystallite dimension of excited by visible light in nanometer scale, to be a kind of desirable photochemical catalyst, also be the problem that is worth research.
At present relevant document proposes to adopt the semiconductor surface modification technology to utilize scope to expand to visible region the spectrum of titanium dioxide optical catalyst, for example: (1) semiconductor surface noble metal loading, adopt deposition process such as immersion reduction method and photoreduction met hod, can improve photocatalytic activity, and make the absorbing wavelength expanded range of photochemical catalyst; (2) semi-conductive metal ion mixing adopts dipping back high-temperature roasting, light assistant depositing, is total to solute doping method etc., not only can strengthen semi-conductive photocatalysis, also may make semi-conductive absorbing wavelength range expansion to the visible region; (3) semi-conductive photoactivate, with Photoactive compounds with physics and chemisorbed in semiconductor surface.Photosensitizers such as the phthalein mountain valley with clumps of trees and bamboo, Porphyrins have bigger motivating factor under visible light, might make its excitation electron inject (conveying) to semi-conductive conduction band, thereby enlarge the semiconductor excitation wavelength range, make its reaction wavelength extend to the visible region; (4) composite semiconductor is prepared binary and polynary composite semiconductor with infusion process and mixed sols method, and its photocatalysis property is higher than single semiconductor ... or the like.But above-mentioned report not mentioned all the time in whole visible wavelength range 400-700nm light absorption and the effect of photoresponse.The Chinese patent literature application number is that " photochemical catalyst and utilization thereof with visible light activity " disclosed technology of 97181439.2 is by in plasma, gaseous mixture with methane and hydrogen carries out CVD processing acquisition to titanium dioxide, provide the photochemical catalyst that can utilize visible light, but can its prepared photochemical catalyst there be all the effect of visible light activity not to be reported in whole visible wavelength range 400-700nm.
The object of the present invention is to provide a kind of preparation method that the visual light reaction type nm TiO 2-base optical catalyst of stronger light absorption and photoresponse is all arranged in whole visible wavelength range 400-700nm.
According to the foregoing invention purpose, preparation method of the present invention: the preparation method of visual light reaction type nm TiO 2-base optical catalyst is characterized in that:
A. the pure salt with titanium adds in the proper amount of solvent alcohols, adds a certain amount of acid again and stirs;
The soluble-salt of metallic element that b. will be to be mixed dissolves in the appropriate amount of deionized water;
C. press doping ratio and in stirring, an amount of b is added among a, obtain oolemma look solution, add an amount of polyethylene glycol again and stir;
D. moisture is removed in above-mentioned mixed solution heating and obtained the solid drying thing;
E. dry thing is calcined in 500-600 ℃ of air atmosphere and promptly obtained metal-doped visual light reaction type nm TiO 2-base optical catalyst in 2-4 hour.
The present invention is owing to adding an amount of polyethylene glycol in preparation process and stirring, it is a kind of modified solute doping method altogether, prevented in the dry run that particle grows up and whole preparation time is shortened greatly, the average grain size of photochemical catalyst is about 10-20nm, has very strong photocatalytic activity, in whole visible wavelength range 400-700nm, stronger light absorption and photoresponse are arranged all, can make full use of visible light sources such as sunshine and indoor incandescent lamp, its energy conversion efficiency improves greatly, low cost of manufacture, cycle is short, can reduce equipment investment and operating cost significantly, applies for large-scale industrialization and lays scientific basic.
As can be seen from Figure 1, in whole visible wavelength range 400-700nm, the absorbance A of 1% bronze medal that mixes is much higher than plain, improves 4-6 doubly than unadulterated nano titanium dioxide photocatalyst.
Below will further understand preparation method of the present invention by embodiment.
Embodiment 1:
A. with the 10mL tetra-n-butyl titanate, add in the 10mL ethanol, add a certain amount of concentrated hydrochloric acid again and stir about 5min till evenly;
B. with 50mg copper chloride (CuCl
2) dissolve in the 20mL deionized water;
C. b is added among a in stirring by doping ratio, stir and take 5min, obtain the oolemma green solution, add an amount of polyethylene glycol again and stir;
D. the direct heating evaporation of above-mentioned mixed solution is removed moisture and obtain the solid drying thing;
E. dry thing is calcined the visual light reaction type nm TiO 2-base optical catalyst of 1% metallic copper that promptly obtained in 2 hours mixing in 550 ℃ of air atmosphere.
Embodiment 2:
A. with the 10mL tetra-n-butyl titanate, add in the 10mL ethanol, add a certain amount of concentrated hydrochloric acid again and stir about 5min till evenly;
B. with 119.1mg iron chloride (Fecl
3) dissolve in the 20mL deionized water;
C. b is added among a in stirring by doping ratio, stir and take 5min, obtain the oolemma yellow solution, add an amount of polyethylene glycol again and stir;
D. the direct heating evaporation of above-mentioned mixed solution is removed moisture and obtain the solid drying thing;
E. dry thing is calcined the visual light reaction type nm TiO 2-base optical catalyst of 1.5% metallic iron that promptly obtained in 2-4 hour mixing in 550 ℃ of air atmosphere.
Embodiment 3:
A. with the 100L tetra-n-butyl titanate, add in the 50L ethanol, add a certain amount of concentrated hydrochloric acid again and stir about 5min till evenly;
B. with 1kg copper chloride (CuCl
2) dissolve in the 50L deionized water;
C. b is added among a in stirring by doping ratio, stir and take 15min, obtain the oolemma green solution, add an amount of polyethylene glycol again and stir;
D. with above-mentioned mixed solution spray drying process drying;
E. with dry thing in 550 ℃ of air atmosphere in pushed bat kiln calcining promptly obtained in 4 hours the mixing visual light reaction type nm TiO 2-base optical catalyst of 2% metallic copper.
Claims (7)
1. the preparation method of a visual light reaction type nm TiO 2-base optical catalyst is characterized in that:
A. the pure salt with titanium adds in the proper amount of solvent alcohols, adds a certain amount of acid again and stirs;
The soluble-salt of metallic element that b. will be to be mixed dissolves in the appropriate amount of deionized water;
C. press doping ratio and in stirring, an amount of b is added among a, obtain oolemma look solution, add an amount of polyethylene glycol again and stir;
D. moisture is removed in above-mentioned mixed solution heating and obtained the solid drying thing;
E. dry thing is calcined in 500-600 ℃ of air atmosphere and promptly obtained metal-doped visual light reaction type nm TiO 2-base optical catalyst in 2-4 hour.
2. the preparation method of visual light reaction type nm TiO 2-base optical catalyst according to claim 1 is characterized in that the pure salt of described titanium includes metatitanic acid four positive fourth fat, metatitanic acid second fat, metatitanic acid isopropyl ester.
3. the preparation method of visual light reaction type nm TiO 2-base optical catalyst according to claim 1 is characterized in that described solvent alcohols includes ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol.
4. the preparation method of visual light reaction type nm TiO 2-base optical catalyst according to claim 1 is characterized in that described acid includes hydrochloric acid, acetic acid, nitric acid, sulfuric acid.
5. the preparation method of visual light reaction type nm TiO 2-base optical catalyst according to claim 1 is characterized in that described metallic element includes copper, iron, vanadium, nickel, strontium, cadmium.
6. the preparation method of visual light reaction type nm TiO 2-base optical catalyst according to claim 1 is characterized in that described soluble-salt includes villaumite, acetate, nitrate, sulfate.
7. the preparation method of visual light reaction type nm TiO 2-base optical catalyst according to claim 1 is characterized in that described mixed solution heats anhydrate branch directly heating evaporation or spray drying process.
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CN1327953C (en) * | 2004-08-30 | 2007-07-25 | 中国科学院上海硅酸盐研究所 | Photocatalyst of nano titanium oxide modifed by cadmium selenide and preparation method |
CN1331592C (en) * | 2002-09-18 | 2007-08-15 | 东芝陶瓷株式会社 | Titanium dioxide particle and its preparing method and optical catalyst preparing method |
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2001
- 2001-05-31 CN CN 01113065 patent/CN1116927C/en not_active Expired - Fee Related
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CN101347732B (en) * | 2008-09-04 | 2010-06-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing porous iron-doped titanic oxide photocatalyst |
CN101774635A (en) * | 2010-03-15 | 2010-07-14 | 彩虹集团公司 | Method for preparing titanium dioxide microballoon sphere modified with noble metals |
CN102631949A (en) * | 2011-02-12 | 2012-08-15 | 首都师范大学 | Modified visible-light responsive titania doped photocatalyst and production method and uses thereof |
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