CN1506154A - Prepn of nitrogen-doped titania powder - Google Patents
Prepn of nitrogen-doped titania powder Download PDFInfo
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- CN1506154A CN1506154A CNA021552010A CN02155201A CN1506154A CN 1506154 A CN1506154 A CN 1506154A CN A021552010 A CNA021552010 A CN A021552010A CN 02155201 A CN02155201 A CN 02155201A CN 1506154 A CN1506154 A CN 1506154A
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Abstract
The present invention belongs to the field of titania catalysis technology, and is especially the preparation of nitrogen-doped titania powder with visible light catalysis performance. Ammonia water of 15-45 wt% concentration is added into titanium compound solution of 25-50 wt% concentration via stirring to form precipitate, with the volume ratio between the ammonia water and the titanium compound solution being 0.5-3.0. Through filtering, washing, drying and calcination at 350-700 deg.c of the precipitate, nitrogen-doped titania powder of average size 100 nm is prepared. The liquid phase nitrogen doping process has homogeneous nitrogen doping, no environmental pollution and low cost, and the prepared nitrogen-doped titania powder has excellent absorption in visible light region.
Description
Technical field
The invention belongs to the optically catalytic TiO 2 technical field, particularly have the preparation method of the nitrogen-doped titanium dioxide powder of visible light catalytic performance.
Background technology
Nitrogen-doped titanium dioxide makes it have the effect of the traditional titanium dioxide of a series of replacements owing at visible light strong sink effect is arranged.There is good application prospects aspects such as multiple pollutant, automatically cleaning technology, anti-biotic material, antifogging coating and solar energy conversion in degradation of sewage and air.Therefore caused people's very big interest.But the preparation method's of relevant nitrogen-doped titanium dioxide powder report is also few, in a spot of report, point out as " science " (Science Vol 293 2001 p.269-27)-Wen, because nitrogen doping process time is long or operation requires high, cause the cost height, it is inhomogeneous to mix simultaneously, and environment is affected.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with nitrogen-doped titanium dioxide powder of visible light catalytic performance.
The present invention is a raw material with the compound and the ammoniacal liquor of titanium, adopts liquid-phase precipitation method to prepare.To precipitate oven dry,, prepare the nitrogen yellow titanium dioxide powder that mixes then in uniform temperature calcining.
Preparation method with nitrogen-doped titanium dioxide powder of visible light catalytic performance of the present invention:
With concentration is that the ammoniacal liquor of 15~45wt% slowly joins in the compound solution of titanium that concentration is 25~50wt%, and strong agitation forms precipitation, and wherein the volume ratio of the compound solution of ammoniacal liquor and titanium is 0.5~3.0; Filter, sediment is calcined under 350-700 degree atmosphere after washing, drying, makes the nitrogen-doped titanium dioxide powder; The average grain diameter of titanium dioxide powder is 100nm.
The compound of described titanium can be isopropyl titanate, butyl titanate, titanium sulfate, titanium trichloride, Titanium Nitrate or titanium tetrachloride etc.Nitrogen content can be regulated by the consumption of ammoniacal liquor.The particle diameter of powder and crystalline form are subjected to heat treated temperature effect in the step, and temperature is high more, and particle diameter is big more.Along with the rising of temperature, crystalline form by amorphous to Detitanium-ore-type to the rutile ore type.
The present invention carries out nitrogen with the liquid phase conventional method to mix, and can make the nitrogen uniform doping, the preparation process non-environmental-pollution, and cost is low.
The titanium dioxide powder that the nitrogen of the present invention's preparation mixes is compared with traditional titanium dioxide powder, at visible region excellent absorption is arranged.
Description of drawings
Fig. 1. the embodiment of the invention 1,2 and 3 ultraviolet-visible absorption spectroscopy figure.
Fig. 2. the X-ray diffractogram of the embodiment of the invention 1.
Fig. 3. the X-ray diffractogram of the embodiment of the invention 2.
Fig. 4. the X-ray diffractogram of the embodiment of the invention 3.
Fig. 5. the catalytic efficiency figure of the titanium dioxide of the embodiment of the invention 1,2,3 and the nitrogen of not mixing.
The specific embodiment
Further set forth the present invention below in conjunction with preferred embodiment of the present invention, but these embodiment limit to technical scheme of the present invention.
Embodiment 1
Adding concentration in the conical flask of 100ml is the 20ml butyl titanate solution of 25wt%, by being the 20ml ammoniacal liquor of 25wt% near the adding concentration of overflowing, produce white precipitate, stirred 3 hours, heavyization of precipitation 24 hours, precipitation is dried in 80-120 degree baking oven through the washing back, calcines under the nitrogen atmosphere of 500 degree then, obtains the nitrogen-doped titanium dioxide powder of little Huang.The average grain diameter of titanium dioxide powder is 100nm.Powder property sees Table-1
Its ultraviolet-visible absorption spectroscopy is seen accompanying drawing 1-A.X-ray diffractogram is seen accompanying drawing 2
Embodiment 2
Adding concentration in the conical flask of 100ml is the 20ml titanium sulfate solution of 25wt%, by being the 20ml ammoniacal liquor of 25wt% near the adding concentration of overflowing, produce white precipitate, stirred 3 hours, heavyization of precipitation 24 hours, precipitation is dried in 80-120 degree baking oven through the washing back, calcines under the nitrogen atmosphere of 500 degree then, obtains the nitrogen-doped titanium dioxide powder of little Huang.The average grain diameter of titanium dioxide powder is 100nm.Powder property sees Table-2.
Its ultraviolet-visible absorption spectroscopy is seen accompanying drawing 1-B.X-ray diffractogram is seen accompanying drawing 3.
Embodiment 3
Adding concentration in the conical flask of 100ml is the 20ml titanium trichloride solution of 50wt%, by being the 20ml ammoniacal liquor of 25wt% near the adding concentration of overflowing, produce white precipitate, stirred 3 hours, heavyization of precipitation 24 hours, precipitation is dried in 80-120 degree baking oven through the washing back, calcines under the nitrogen atmosphere of 500 degree then, obtains the nitrogen-doped titanium dioxide powder of little Huang.The average grain diameter of titanium dioxide powder is 100nm.Powder property sees Table-3.
Its ultraviolet-visible absorption spectroscopy is seen accompanying drawing 1-C.X-ray diffractogram is seen accompanying drawing 4.
Comparative Examples 1.1
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 5ml ammoniacal liquor is precipitating reagent.Powder property sees Table-1.
Comparative Examples 1.2
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 10ml ammoniacal liquor is precipitating reagent.Powder property sees Table-1.
Comparative Examples 1.3
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 15ml ammoniacal liquor is precipitating reagent.Powder property sees Table-1.
Comparative Examples 1.4
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 25ml ammoniacal liquor is precipitating reagent.Powder property sees Table-1.
Comparative Examples 1.5
According to embodiment 1 in the identical method described obtain the nitrogen-doped titanium dioxide powder.Just having used 30ml ammoniacal liquor is precipitating reagent.Powder property sees Table-1.
Comparative Examples 1.6
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 350 degree atmosphere, calcine.Powder property sees Table-4.
Comparative Examples 1.7
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 400 degree atmosphere, calcine.Powder property sees Table-4.
Comparative Examples 1.8
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 550 degree atmosphere, calcine.Powder property sees Table-4.
Comparative Examples 1.9
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 600 degree atmosphere, calcine.Powder property sees Table-4.
Comparative Examples 1.10
According to embodiment 1 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 700 degree atmosphere, calcine.Powder property sees Table-4.
Comparative Examples 2.1
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 5ml ammoniacal liquor is precipitating reagent.Powder property sees Table-2.
Comparative Examples 2.2
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 10ml ammoniacal liquor is precipitating reagent.Powder property sees Table-2.
Comparative Examples 2.3
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 15ml ammoniacal liquor is precipitating reagent.Powder property sees Table-2.
Comparative Examples 2.4
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 25ml ammoniacal liquor is precipitating reagent.Powder property sees Table-2.
Comparative Examples 2.5
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 30ml ammoniacal liquor is precipitating reagent.Powder property sees Table-2.
Comparative Examples 2.6
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 350 degree atmosphere, calcine.Powder property sees Table-5.
Comparative Examples 2.7
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 400 degree atmosphere, calcine.Powder property sees Table-5.
Comparative Examples 2.8
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 550 degree atmosphere, calcine.Powder property sees Table-5.
Comparative Examples 2.9
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 600 degree atmosphere, calcine.Powder property sees Table-5.
Comparative Examples 2.10
According to embodiment 2 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 700 degree atmosphere, calcine.Powder property sees Table-5.
Comparative Examples 3.1
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 5ml ammoniacal liquor is precipitating reagent.Powder property sees Table-3.
Comparative Examples 3.2
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 10ml ammoniacal liquor is precipitating reagent.Powder property sees Table-3.
Comparative Examples 3.3
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 15ml ammoniacal liquor is precipitating reagent.Powder property sees Table-3.
Comparative Examples 3.4
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 25ml ammoniacal liquor is precipitating reagent.Powder property sees Table-3.
Comparative Examples 3.5
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just having used 30ml ammoniacal liquor is precipitating reagent.Powder property sees Table-3
Comparative Examples 3.6
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 350 degree atmosphere, calcine.Powder property sees Table-6
Comparative Examples 3.7
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 400 degree atmosphere, calcine.Powder property sees Table-6.
Comparative Examples 3.8
According to embodiment 3 in the identical method described obtain the nitrogen-doped titanium dioxide powder.Just under 550 degree atmosphere, calcine.Powder property sees Table-6.
Comparative Examples 3.9
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 600 degree atmosphere, calcine.Powder property sees Table-6.
Comparative Examples 3.10
According to embodiment 3 in the method described obtain the nitrogen-doped titanium dioxide powder.Just under 700 degree atmosphere, calcine.Powder property sees Table-6.
Table-1
Embodiment 1 | Comparative Examples 1.1 | Comparative Examples 1.2 | Comparative Examples 1.3 | Comparative Examples 1.4 | Comparative Examples 1.5 | |
Color | Little Huang | Little Huang | Little Huang | Little Huang | Little Huang | Little Huang |
Crystalline form | Anatase | Anatase | Anatase | Anatase | Anatase | Anatase |
N content % (at) | ???0.85 | ??0.69 | ???0.79 | ?0.83 | ???0.86 | ???0.86 |
Table-2
Embodiment 2 | Comparative Examples 2.1 | Comparative Examples 2.2 | Comparative Examples 2.3 | Comparative Examples 2.4 | Comparative Examples 2.5 | |
Color | Little Huang | Little Huang | Little Huang | Little Huang | Little Huang | Little Huang |
Crystalline form | Anatase | Anatase | Anatase | Anatase | Anatase | Anatase |
N content % (at) | ??0.78 | ???0.61 | ???0.76 | ???0.77 | ???0.79 | ???0.79 |
Table-3
Embodiment 3 | Comparative Examples 3.1 | Comparative Examples 3.2 | Comparative Examples 3.3 | Comparative Examples 3.4 | Comparative Examples 3.5 | |
Color | Little Huang | Little Huang | Little Huang | Little Huang | Little Huang | Little Huang |
Crystalline form | Anatase | Anatase | Anatase | Anatase | Anatase | Anatase |
N content % (at) | ???0.83 | ????0.66 | ???0.71 | ????0.79 | ????0.83 | ????0.83 |
Table-4
Embodiment 1 | Comparative Examples 1.6 | Comparative Examples 1.7 | Comparative Examples 1.8 | Comparative Examples 1.9 | Comparative Examples 1.10 | |
Color | Little Huang | White | Little Huang | Little Huang | Little Huang | Little Huang |
Crystalline form | Anatase | Amorphous | Anatase | Anatase | Rutile | Rutile |
Table-5
Embodiment 2 | Comparative Examples 2.6 | Comparative Examples 2.7 | Comparative Examples 2.8 | Comparative Examples 2.9 | Comparative Examples 2.10 | |
Color | Little Huang | White | Little Huang | Little Huang | Little Huang | Little Huang |
Crystalline form | Anatase | Amorphous | Anatase | Anatase | Rutile | Rutile |
Table-6
Embodiment 3 | Comparative Examples 3.6 | Comparative Examples 3.7 | Comparative Examples 3.8 | Comparative Examples 3.9 | Comparative Examples 3.10 | |
Color | Little Huang | White | Little Huang | Little Huang | Little Huang | Little Huang |
Crystalline form | Anatase | Amorphous | Anatase | Anatase | Rutile | Rutile |
1 ,-1 as can be known, the content that the volume ratio of the consumption of ammoniacal liquor and precipitation presoma is about 1: 1 o'clock nitrogen is the highest, and the consumption that improves ammoniacal liquor does not again have very big influence to the content of nitrogen by table.
2 ,-2 as can be known, the content that the volume ratio of the consumption of ammoniacal liquor and precipitation presoma is about 1: 1 o'clock nitrogen is the highest, and the consumption that improves ammoniacal liquor does not again have very big influence to the content of nitrogen by table.
3 ,-3 as can be known, the content that the volume ratio of the consumption of ammoniacal liquor and precipitation presoma is about 1: 1 o'clock nitrogen is the highest, and the consumption that improves ammoniacal liquor does not again have very big influence to the content of nitrogen by table.
4, as can be known, the analysis through Comparative Examples 1.6~1.10 has only obtained good X-ray diffraction image in embodiment 1 by table-4.By figure-2 as can be known, under 500 degree temperature, can access good anatase crystalline substance.
5, as can be known, the analysis through Comparative Examples 2.6~2.10 has only obtained good X-ray diffraction image in embodiment 2 by table-5.By figure-3 as can be known, under 500 degree temperature, can access good anatase crystalline substance.
6, as can be known, the analysis through Comparative Examples 3.6~3.10 has only obtained good X-ray diffraction image in embodiment 3 by table-6.By figure-4 as can be known, under 500 degree temperature, can access good anatase crystalline substance.
7, as can be known, according to the method for embodiment 1~3, can obtain at the very strong nitrogen-doped titanium dioxide powder of visual field absorption by figure-1.
The measurement of photocatalysis performance:
Contrast commercial available photochemical catalyst commonly used, measurement by embodiment 1~3 obtain the photocatalysis performance of nitrogen-doped titanium dioxide powder, the PC-25 that produces with Germany is as catalyst A, the nitrogen-doped titanium dioxide powder is a catalyst B among the embodiment 1, the nitrogen-doped titanium dioxide powder is catalyst C among the embodiment 2, and the nitrogen-doped titanium dioxide powder is catalyst D among the embodiment 3.
The detection principle is: because the absorbing wavelength of methyl orchid is 620nm, so penetrate above the catalyst that load has the methyl orchid with the detection illumination of 620nm, during beginning, the methyl orchid is made as 100% to the absorption of surveying light, and through after the visible light radiation, methyl is blue to be decomposed, concentration reduces, the absorption of surveying light is reduced, and initial relatively being absorbed as is negative, can represent the amount of the decomposition of methyl orchid in the test interval with △ ABS.The catalytic performance of representing catalyst by △ ABS/MIN.
For tested material in the experiment is the blue solution of methyl of 1.0mM/L, the use of catalyst is: mix mutually with the Ludox of 10ml and the catalyst of 1g, after fully stirring, put into wherein with the ito glass of 2cm * 2cm, take out after 2 minutes, drying at room temperature, the blue drips of solution of methyl of using 0.6ml is on the ito glass of dried supported catalyst, put into the dark place drying at room temperature, standby.
It is that the visible light of 440nm is used as detection light source that experimentation is used after filter plate filters wavelength, and its energy is: 0.6mW/cm
2, its catalytic efficiency is as figure-5.
Shown in figure-5, the catalytic effect of catalyst B~D is quite similar, and at visible region good catalytic effect is arranged with respect to commerce catalyst A: PC-25.
Compound and ammoniacal liquor according to the present invention with titanium are raw material, and the nitrogen-doped titanium dioxide powder that adopts liquid-phase precipitation method to prepare has good absorption and catalytic effect in the visible region.
Although the present invention has been carried out clear and definite explanation with reference to its specific embodiment, but scientific and technical personnel to this area, under the situation that does not break away from the spirit and scope of the present invention defined in the appended claims, can make multiple change to form of the present invention and content.
Claims (4)
1. the preparation method of a nitrogen-doped titanium dioxide powder is characterized in that:
With concentration is that the ammoniacal liquor of 15~45wt% slowly joins in the compound solution of titanium that concentration is 25~50wt%, and strong agitation forms precipitation, and wherein the volume ratio of the compound solution of ammoniacal liquor and titanium is 0.5~3.0; Filter, sediment is calcined under 350-700 degree atmosphere after washing, drying, makes the nitrogen-doped titanium dioxide powder.
2. the method for claim 1, it is characterized in that: the compound of described titanium is isopropyl titanate, butyl titanate, titanium sulfate, titanium trichloride, Titanium Nitrate or titanium tetrachloride.
3. the method for claim 1 is characterized in that: the crystalline form of described titanium dioxide powder is amorphous, Detitanium-ore-type or rutile ore type.
4. as claim 1 or 3 described methods, it is characterized in that: the average grain diameter of described titanium dioxide powder is 100nm.
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CN1305560C (en) * | 2004-11-06 | 2007-03-21 | 重庆工学院 | Process for preparing highly efficient titania photocatalyst |
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CN1321738C (en) * | 2005-04-29 | 2007-06-20 | 北京科技大学 | Production of nitrogen-doped anatase-type nanometer titanium dioxide |
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CN102817021A (en) * | 2012-08-28 | 2012-12-12 | 南昌大学 | Method for preparing novel visible light-responded N-TiO2/SiO2 composite file on surface of fluorine-carbon aluminum single sheet |
CN102976401A (en) * | 2012-10-22 | 2013-03-20 | 山东轻工业学院 | Ultrasonic chemical preparation method for nitrogen-doped nano-titanium dioxide crystal |
CN104248967A (en) * | 2014-06-17 | 2014-12-31 | 扬州大学 | Vapor phase method for preparation of porous carrier supported nitrogen doped titanium dioxide |
CN107662942A (en) * | 2017-10-30 | 2018-02-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Nano-TiO2Preparation method |
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CN111634943A (en) * | 2020-06-15 | 2020-09-08 | 上海工程技术大学 | Crystalline phase regulation and control method of titanium dioxide nano material |
CN111634943B (en) * | 2020-06-15 | 2022-08-23 | 上海工程技术大学 | Crystalline phase regulation and control method of titanium dioxide nano material |
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