CN102059110A - Preparation method of double-rare earth co-doped nanometer titanium dioxide photocatalyst - Google Patents
Preparation method of double-rare earth co-doped nanometer titanium dioxide photocatalyst Download PDFInfo
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Abstract
The invention relates to a preparation method of a double-rare earth co-doped nanometer titanium dioxide photocatalyst, which is a titanium dioxide photocatalyst prepared from co-doping two rare earth ions. Compared with the single-doped rare earth titanium dioxide, the invention has higher photocatalysis activity and can quickly degrade pollutants in dye waste water. The invention has high activity of the prepared catalyst and high degradation of the pollutants and provides a foundation for industrial application.
Description
Technical field
The present invention relates to a kind of preparation method of nano titanic oxide catalyst, particularly relate to a kind of pair of rare earth coblended nano TiO 2 Preparation of catalysts method.
Background technology
Photocatalysis technology is one of most active research field of international academic community in recent years.Titanium dioxide (TiO
2) received the increasingly extensive concern of people as photochemical catalyst.Titanium dioxide (TiO
2) as a kind of semiconductor functional material, its photocatalytic activity is mainly by self crystal structure decision, but also very responsive to small amount of impurities.Can improve the spectral response range and the catalytic efficiency of photochemical catalyst by doping vario-property.
At present to the research of single doping vario-property of titanium dioxide comparative maturity, by the doping of some metallic elements and nonmetalloid, the photocatalysis performance of titanium dioxide significantly improves.Discover, choose suitable element and carry out codope that the photochemical catalyst that obtains has than the single-element higher photocatalysis performance that mixes recent years, wherein studying more is bimetal element and the codope of two nonmetalloids.The codope of two nonmetalloids generally all shows as at visible region and produces absorption, is to realize titanium dioxide (TiO
2) effective means of photochemical catalyst excited by visible light, have excellent research and be worth.
Rare earth element is because special level structure and spectral characteristic can effectively improve nano-TiO by mixing
2Photocatalysis efficiency.If two kinds of different rare earth elements are doped in the titanium dioxide simultaneously, when suitable and both concentration proportioning is best when selected rare earth ion, produce synergy, improve the photocatalytic activity of titanium dioxide jointly.
The invention provides a kind of titanic oxide composite photochemical catalyst material of double rare-earth elements codope,, have higher photocatalytic activity, fast the pollutant in the degradation of dye waste water compared to the nano titanium oxide of single rare earth element doping.
Summary of the invention
One of purpose of the present invention is to provide a kind of pair of rare earth coblended nano TiO 2 catalyst, it is the nano titanium dioxide photocatalyst by two kinds of rare earth ion codopes, make it have higher photocatalytic activity, fast the organic pollution in the degradation of dye waste water.
Two of purpose of the present invention is to provide the preparation method of this titanium deoxide catalyst.
The invention provides the preparation method of a kind of pair of rare earth coblended nano TiO 2 light catalyst, it is characterized in that, comprise the steps:
(1) tetrabutyl titanate is added in the absolute ethyl alcohol and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 2-3, drip the back and continue to stir 0.5-2 hour, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) two kinds of different nitrate of rare earth element aqueous solution, absolute ethyl alcohol and small amount of deionized water are fully mixed, stir about 10-30 minute, obtain B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, continues to stir 2 hours, obtain the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, 50-80 ℃ of oven dry obtains xerogel;
(5) xerogel is pulverized last, place Muffle furnace to heat, heating rate 5-10 ℃/min,, obtain two rare earth coblended nano TiO 2 light catalysts in 500 ℃ of sintering.
Described rare earth element is gadolinium and lanthanum or gadolinium and yttrium or lanthanum and cerium or gadolinium and europium.
The molar percentage of described rare earth element and titanium dioxide is 0.2-5%.
Described butyl titanate: the volume ratio of absolute ethyl alcohol is 1: 4.
Described butyl titanate: the mol ratio of deionized water (containing the deionized water that dissolves nitrate) is 4: 1.
The present invention adopts the two rear-earth-doped nanometer titanic oxide materials of sol-gel technique preparation, and the catalytic activity height has the catalytic activity higher than the titanium dioxide of single doped with rare-earth elements, the organic pollution in the industrial wastewater of degrading fast and effectively.Two rear-earth-doped preparation process are simple, can realize industrial production.
The specific embodiment
The several embodiment of various details, but content of the present invention is not limited to this fully.
Embodiment 1:
(1) 10 milliliters of tetrabutyl titanates are added in 25 milliliters of absolute ethyl alcohols and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 3, drip the back and continue to stir 2 hours, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) a small amount of gadolinium nitrate aqueous solution, lanthanum nitrate aqueous solution and small amount of deionized water are fully mixed with 15 milliliters of absolute ethyl alcohols, stir about 10 minutes obtains B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, after continuing to stir 2 hours, obtains the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, dried 12 hours, and obtained xerogel for 50 ℃;
(5) xerogel is pulverized last, place Muffle furnace to heat, heating rate 5/min in 500 ℃ of sintering 2 hours, obtains two rare earth ion gadoliniums and lanthanum co-doped nano titanium dioxide photocatalyst.
Embodiment 2:
(1) 30 milliliters of tetrabutyl titanates are added in 105 milliliters of absolute ethyl alcohols and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 2, drip the back and continue to stir 1 hour, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) a small amount of gadolinium nitrate aqueous solution, yttrium nitrate aqueous solution and small amount of deionized water are fully mixed with 15 milliliters of absolute ethyl alcohols, stir about 30 minutes obtains B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, after continuing to stir 2 hours, obtains the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, dried 12 hours, and obtained xerogel for 80 ℃;
(5) xerogel is pulverized last, place Muffle furnace to heat, 5 ℃/min of heating rate in 500 ℃ of sintering 2 hours, obtains two rare earth ion gadoliniums and yttrium coblended nano TiO 2 light catalyst.
Embodiment 3:
(1) 10 milliliters of tetrabutyl titanates are added in 25 milliliters of absolute ethyl alcohols and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 3, drip the back and continue to stir 0.5 hour, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) a small amount of lanthanum nitrate aqueous solution, the cerous nitrate aqueous solution and small amount of deionized water are fully mixed with 15 milliliters of absolute ethyl alcohols, stir about 15 minutes obtains B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, after continuing to stir 2 hours, obtains the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, 50 ℃ of oven dry obtain xerogel;
(5) xerogel is pulverized last, place Muffle furnace to heat, 10 ℃/min of heating rate in 500 ℃ of sintering 2 hours, obtains two rare earth ion lanthanums and cerium coblended nano TiO 2 light catalyst.
Embodiment 4:
(1) 10 milliliters of tetrabutyl titanates are added in 25 milliliters of absolute ethyl alcohols and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 2, drip the back and continue to stir 2 hours, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) a small amount of dysprosium nitrate aqueous solution, the cerous nitrate aqueous solution and small amount of deionized water are fully mixed with 15 milliliters of absolute ethyl alcohols, stir about 15 minutes obtains B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, after continuing to stir 2 hours, obtains the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, dried 12 hours, and obtained xerogel for 50 ℃;
(5) xerogel is pulverized last, place Muffle furnace to heat, 10 ℃/min of heating rate in 500 ℃ of sintering 2 hours, obtains two rare earth ion dysprosiums and cerium coblended nano TiO 2 light catalyst.
Embodiment 4:
(1) 10 milliliters of tetrabutyl titanates are added in 25 milliliters of absolute ethyl alcohols and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 2, drip the back and continue to stir 2 hours, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) a small amount of gadolinium nitrate aqueous solution, the europium nitrate aqueous solution and small amount of deionized water are fully mixed with 15 milliliters of absolute ethyl alcohols, stir about 30 minutes obtains B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, after continuing to stir 2 hours, obtains the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, dried 12 hours, and obtained xerogel for 50 ℃;
(5) xerogel is pulverized last, place Muffle furnace to heat, 15 ℃/min of heating rate in 500 ℃ of sintering 2 hours, obtains two rare earth ion gadoliniums and europium-doped nano titanium dioxide photocatalyst.
Claims (5)
1. the preparation method of two rare earth coblended nano TiO 2 light catalysts is characterized in that, comprises the steps:
(1) tetrabutyl titanate is added in the absolute ethyl alcohol and continuous the stirring until dropwising, obtain the yellow solution of homogeneous transparent, be added dropwise to a small amount of red fuming nitric acid (RFNA) again, regulating the pH value is 2-3, drip the back and continue to stir 0.5-2 hour, the yellow solution that obtains homogeneous transparent is an A liquid;
(2) two kinds of different nitrate of rare earth element aqueous solution, absolute ethyl alcohol and small amount of deionized water are fully mixed, stir about 10-30 minute, obtain B liquid;
(3) under stirring and room temperature condition, B liquid slowly is added drop-wise in the A liquid, continues to stir 2 hours, obtain the colloidal sol of homogeneous transparent, ageing to colloidal sol loses flowability and obtains gel;
(4) gel is placed thermostatic drying chamber, 50-80 ℃ of oven dry obtains xerogel;
(5) xerogel is pulverized last, place Muffle furnace to heat, heating rate 5-10 ℃/min,, obtain two rare earth coblended nano TiO 2 light catalysts in 500 ℃ of sintering.
2. the preparation method of according to claim 1 pair of rare earth coblended nano TiO 2 light catalyst is characterized in that, described rare earth element is gadolinium and lanthanum or gadolinium and yttrium or lanthanum and cerium or gadolinium and europium.
3. the preparation method of according to claim 1 pair of rare earth coblended nano TiO 2 light catalyst is characterized in that, the molar percentage of described rare earth element and titanium dioxide is 0.2-5%.
4. the preparation method of according to claim 1 pair of rare earth coblended nano TiO 2 light catalyst is characterized in that, described butyl titanate: the volume ratio of absolute ethyl alcohol is 1: 4.
5. the preparation method of according to claim 1 pair of rare earth coblended nano TiO 2 light catalyst is characterized in that, described butyl titanate: the mol ratio of deionized water (containing the deionized water that dissolves nitrate) is 4: 1.
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Application publication date: 20110518 |