CN104437449A - Preparation method of black titanium dioxide visible light photocatalyst - Google Patents
Preparation method of black titanium dioxide visible light photocatalyst Download PDFInfo
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- CN104437449A CN104437449A CN201410752139.1A CN201410752139A CN104437449A CN 104437449 A CN104437449 A CN 104437449A CN 201410752139 A CN201410752139 A CN 201410752139A CN 104437449 A CN104437449 A CN 104437449A
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Abstract
The invention discloses a preparation method of a black titanium dioxide visible light photocatalyst, relating to a preparation method of a visible light photocatalyst and aiming at solving the technical problems that titanium dioxide prepared by adopting the existing method is low in the utilization ratio of sunshine and the crystallization degree of the titanium dioxide is low as a catalyst. The method comprises the following steps: I, mixing reagents; II, performing oil bath; III, drying; IV, performing thermal treatment; V, carrying out ball-grinding; VI, calcining; and VII, Washing and drying. According to the prepared black titanium dioxide visible light photocatalyst, organic pollutants can be effectively removed, the removal rate can achieve 100%, and the mineralization degree can achieve 100%. Compared with the similar black titanium dioxide processes, the preparation method disclosed by the invention has no severe reaction conditions, and the reaction efficiency is improved by three times. The preparation method of the black titanium dioxide visible light photocatalyst belongs to the field of preparation of the photocatalyst.
Description
Technical field
The present invention relates to a kind of preparation method of visible-light photocatalyst.
Background technology
Environmental pollution has badly influenced the productive life of the mankind, especially to the pollution of water body, has caused hydrobiological mortality, and carry out enrichment in biological chain.Therefore, environment and the energy become the focus that people pay close attention to.Conductor photocatalysis is a kind of advanced oxidation processes, has unique advantage, thus receive in recent years and especially pay close attention in the field of disposing of sewage.Titanium dioxide extensive use because of inexpensive, nontoxic and excellent optical, electrical performance.But traditional nano titanium oxide is because of its lower specific area and photogenerated charge recombination rate and limit the raising of its performance faster.In addition, anatase titania has wider band gap (3.2eV) width, can only absorb ultraviolet light, and ultraviolet light only accounts for about 5% of solar energy gross energy, therefore, lower to the utilization rate of sunshine.People adopt the means such as doping, compound to expand the photoresponse scope of titanium dioxide, improve the absorbability to visible ray, but effect not obvious.The titanium dioxide of black can strengthen the absorption to visible ray and infrared light greatly.A large amount of lattice disorders will produce the intermediate state being different from single imperfect crystal, these intermediate state energy continuous distributed are also overlapping with conduction band limit, therefore they are often called as magnetic tape trailer state (band tail states), magnetic tape trailer state is dissolved into valence band by a large amount of lattice disorders, and what these extended can be with the energy level combining doping generation to become optical excitation center.
Summary of the invention
The present invention will solve the low and titanium dioxide of the utilization rate of titanium dioxide to sunshine prepared by existing method as the low technical problem of the degree of crystallization of catalyst, provides a kind of preparation method of black TiO 2 visible light catalyst.
The preparation method of black TiO 2 visible light catalyst carries out according to following steps:
One, the mixing of reagent:
Joined by anatase titanium dioxide in the aqueous solution of ethylenediamine, wherein the mass ratio of anatase titanium dioxide and ethylenediamine is 1:40-100, stir 10-60min, and adjust ph is 10-12, obtains mixed liquor;
Two, oil bath: by mixed liquor under the condition of 80-120 DEG C of oil bath, condensing reflux 12-48h;
Three, dry: by the solution of step 2 gained, be separated with centrifuge, by sediment deionized water rinsing 2-8 time, then under the condition of 40-80 DEG C, keep 12-36h, obtain powder;
Four, heat treatment: powder mull is even, is warming up to 600 DEG C-1000 DEG C with the speed of 2 DEG C/min-10 DEG C/min and is incubated 2h-6h in air atmosphere, being cooled to room temperature, obtaining powder;
Five, ball milling: the ratio mixed grinding 10-40min by powder and sodium borohydride being 1:3-8 in mass ratio, then put into ball mill ball milling 10-30min;
Six, calcine: the powder after step 5 ball milling is warming up to 150 DEG C-450 DEG C with the speed of 2 DEG C/min-10 DEG C/min and keeps 30-150min under inert gas atmosphere, is cooled to room temperature;
Seven, washing is dry: powder step 6 obtained is respectively with ethanol, deionization washing 4-6 time, and centrifugation, proceeds to drying box by powder, keeps 12-36h, obtain black TiO 2 visible light catalyst at 60-80 DEG C.
Anatase titanium dioxide described in step one is P25 type titanium dioxide, mesoporous TiO 2, spherical tio2 or bar-shaped titanium dioxide.
Inert gas described in step 6 is argon gas, nitrogen or neon.
The black TiO 2 visible light catalyst that the present invention obtains effectively can remove organic pollution, clearance can reach 100%, and salinity reaches 100%, Pyrogentisinic Acid under visible light conditions irradiates, methylene blue, methyl orange, the pollutants removal rates such as rhodamine B can reach more than 98%, and mineralization rate is all more than 97%.And in the process prepared than similar black titanium dioxide, without harsh reaction condition and reaction efficiency improves 2 times.
The black titanium dioxide visible light catalyzer of prepared by the present invention have high degree of crystallization, has high stability good, adsorptivity, photocatalytic activity is high, the advantage of environmental protection, and product can directly be recycled.The inventive method preparation technology is simple, and equipment is simple, and cost is low, high efficiency, is easy to realize commercialization.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the black TiO 2 visible light catalyst that experiment one obtains.
Fig. 2 is the comparison diagram of the UV-vis DRS spectrum of the obtained black TiO 2 visible light catalyst of experiment one and P25 type titanium dioxide, in figure, a represents the UV-vis DRS spectrogram of P25 type titanium dioxide, and b represents the UV-vis DRS spectrogram of the black TiO 2 visible light catalyst that experiment one is obtained.
Fig. 3 is the photo of the black TiO 2 visible light catalyst that experiment one obtains;
Fig. 4 is the photo of P25 type titanium dioxide powder.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: the preparation method of the black TiO 2 visible light catalyst of present embodiment carries out according to following steps:
One, the mixing of reagent:
Joined by anatase titanium dioxide in the aqueous solution of ethylenediamine, wherein the mass ratio of anatase titanium dioxide and ethylenediamine is 1:40-100, stir 10-60min, and adjust ph is 10-12, obtains mixed liquor;
Two, oil bath: by mixed liquor under the condition of 80-120 DEG C of oil bath, condensing reflux 12-48h;
Three, dry: by the solution of step 2 gained, be separated with centrifuge, by sediment deionized water rinsing 2-8 time, then under the condition of 40-80 DEG C, keep 12-36h, obtain powder;
Four, heat treatment: powder mull is even, is warming up to 600 DEG C-1000 DEG C with the speed of 2 DEG C/min-10 DEG C/min and is incubated 2h-6h in air atmosphere, being cooled to room temperature, obtaining powder;
Five, ball milling: the ratio mixed grinding 10-40min by powder and sodium borohydride being 1:3-8 in mass ratio, then put into ball mill ball milling 10-30min;
Six, calcine: the powder after step 5 ball milling is warming up to 150 DEG C-450 DEG C with the speed of 2 DEG C/min-10 DEG C/min and keeps 30-150min under inert gas atmosphere, is cooled to room temperature;
Seven, washing is dry: powder step 6 obtained is respectively with ethanol, deionization washing 4-6 time, and centrifugation, proceeds to drying box by powder, keeps 12-36h, obtain black TiO 2 visible light catalyst at 60-80 DEG C.
Anatase titanium dioxide described in present embodiment joins grinding 10-30min before in the aqueous solution of ethylenediamine.
The device that in present embodiment step 4, heat treatment is used is Muffle furnace, tube furnace, micro-wave oven or electrothermal furnace.
Detailed description of the invention two: present embodiment and detailed description of the invention one are P25 type titanium dioxide, mesoporous TiO 2, spherical tio2 or bar-shaped titanium dioxide unlike described anatase titanium dioxide.Other is identical with detailed description of the invention one.
Mesoporous TiO 2 described in present embodiment is N-TiO
2or S-TiO
2.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one or two are 1:50-80 unlike the mass ratio of anatase titanium dioxide in step one and ethylenediamine.Other is identical with one of detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three are 90-110 DEG C unlike oil bath temperature in step 2, return time 18-30h.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four are unlike being keep 18-30 hour under the condition of 50-70 DEG C in temperature in step 3.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five are unlike being warming up to 700 DEG C-900 DEG C with the speed of 6 DEG C/min in air atmosphere in step 4 and being incubated 2h-6h.Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six unlike the ratio mixed grinding 15-25min in step 5 by powder and sodium borohydride being 1:3-5 in mass ratio, then put into ball mill ball milling 15-25min.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven are argon gas, nitrogen or neon unlike the inert gas described in step 6.Other is identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to eight, unlike the powder after step 5 ball milling being warming up to 300-450 DEG C under inert gas atmosphere in step 6 and keeping 60-120min, are cooled to room temperature.Other is identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention one to nine keep 20h by step 7 at 70 DEG C unlike in step 6.Other is identical with one of detailed description of the invention one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of black TiO 2 visible light catalyst carries out according to following steps:
One, the mixing of reagent:
Join in the aqueous solution of ethylenediamine by after anatase titanium dioxide 15min, wherein the mass ratio of anatase titanium dioxide and ethylenediamine is 1:60, stir 30min, and adjust ph is 11, obtains mixed liquor;
Two, oil bath: by mixed liquor under the condition of 90-100 DEG C of oil bath, condensing reflux 24h;
Three, dry: by the solution of step 2 gained, be separated with centrifuge, by sediment deionized water rinsing 4 times, then under the condition of 60 DEG C, keep 24h, obtain powder;
Four, heat treatment: powder mull is even, is warming up to 800 DEG C with the speed of 5 DEG C/min in air atmosphere and is incubated 2h-6h, being cooled to room temperature, obtaining powder;
Five, ball milling: the ratio mixed grinding 30min by powder and sodium borohydride being 1:5 in mass ratio, then put into ball mill ball milling 30min;
Six, calcine: the powder after step 5 ball milling be warming up to 400 DEG C with the speed of 5 DEG C/min under inert gas atmosphere and keep 90min, being cooled to room temperature;
Seven, washing is dry: powder step 6 obtained washes 4 times with ethanol, deionization respectively, and powder is proceeded to drying box by centrifugation, keeps drying, obtain black TiO 2 visible light catalyst at 60 DEG C.
Fig. 1 is the XRD figure of the obtained black TiO 2 visible light catalyst of experiment one, analysis can find out into after high-temperature calcination the crystallization Cheng Du of material be greatly improved,
Fig. 2 is the comparison diagram of the UV-vis DRS spectrum of the obtained black TiO 2 visible light catalyst of experiment one and P25 type titanium dioxide, pass through atlas analysis, P25 type titanium dioxide does not substantially have photoresponse in visible-range, and black TiO 2 visible light catalyst has extraordinary photoresponse in visible region, be that the visible light-responded material that even exceedes of 600-800nm is from the photophase in ultraviolet light range at wavelength.
Fig. 3 and Fig. 4 is the color contrast figure of the obtained black TiO 2 visible light catalyst of experiment one and P25 type titanium dioxide powder, can find to become black through testing the powder color after a process from white from the contrast of Fig. 3 and Fig. 4, color there occurs significant change.
The black TiO 2 visible light catalyst that this experiment obtains effectively can remove organic pollution, clearance can reach 100%, and salinity reaches 100%, Pyrogentisinic Acid under visible light conditions irradiates, methylene blue, methyl orange, the pollutants removal rates such as rhodamine B can reach more than 98%, and mineralization rate is all more than 97%.
Claims (10)
1. the preparation method of black TiO 2 visible light catalyst, is characterized in that the preparation method of black TiO 2 visible light catalyst carries out according to following steps:
One, the mixing of reagent:
Joined by anatase titanium dioxide in the aqueous solution of ethylenediamine, wherein the mass ratio of anatase titanium dioxide and ethylenediamine is 1:40-100, stir 10-60min, and adjust ph is 10-12, obtains mixed liquor;
Two, oil bath: by mixed liquor under the condition of 80-120 DEG C of oil bath, condensing reflux 12-48h;
Three, dry: by the solution of step 2 gained, be separated with centrifuge, by sediment deionized water rinsing 2-8 time, then under the condition of 40-80 DEG C, keep 12-36h, obtain powder;
Four, heat treatment: powder mull is even, is warming up to 600 DEG C-1000 DEG C with the speed of 2 DEG C/min-10 DEG C/min and is incubated 2h-6h in air atmosphere, being cooled to room temperature, obtaining powder;
Five, ball milling: the ratio mixed grinding 10-40min by powder and sodium borohydride being 1:3-8 in mass ratio, then put into ball mill ball milling 10-30min;
Six, calcine: the powder after step 5 ball milling is warming up to 150 DEG C-450 DEG C with the speed of 2 DEG C/min-10 DEG C/min and keeps 30-150min under inert gas atmosphere, is cooled to room temperature;
Seven, washing is dry: powder step 6 obtained is respectively with ethanol, deionization washing 4-6 time, and centrifugation, proceeds to drying box by powder, keeps 12-36h, obtain black TiO 2 visible light catalyst at 60-80 DEG C.
2. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that the anatase titanium dioxide described in step one is P25 type titanium dioxide, mesoporous TiO 2, spherical tio2 or bar-shaped titanium dioxide.
3. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that the mass ratio of anatase titanium dioxide and ethylenediamine in step one is 1:50-80.
4. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that in step 2, oil bath temperature is 90-110 DEG C, return time 18-30h.
5. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that under temperature is the condition of 50-70 DEG C, keeping 18-30 hour in step 3.
6. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that being warming up to 700 DEG C-900 DEG C with the speed of 6 DEG C/min in air atmosphere in step 4 and being incubated 2h-6h.
7. the preparation method of black TiO 2 visible light catalyst according to claim 1, to is characterized in that powder and sodium borohydride in step 5 being the ratio mixed grinding 15-25min of 1:3-5 in mass ratio, then puts into ball mill ball milling 15-25min.
8. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that the inert gas described in step 6 is argon gas, nitrogen or neon.
9. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that in step 6, the powder after step 5 ball milling being warming up to 300-450 DEG C under inert gas atmosphere and keeping 60-120min, is cooled to room temperature.
10. the preparation method of black TiO 2 visible light catalyst according to claim 1, is characterized in that keeping 20h by step 7 at 70 DEG C in step 6.
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Cited By (8)
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| CN105056925A (en) * | 2015-09-07 | 2015-11-18 | 黑龙江大学 | Preparation method of black titanium dioxide nano rod visible light catalyst |
| CN105195133A (en) * | 2015-09-18 | 2015-12-30 | 黑龙江大学 | Preparation method of molybdenum disulfide-black titanium dioxide composite visible-light-driven photocatalyst for hydrogen production |
| CN105618022A (en) * | 2016-01-12 | 2016-06-01 | 遵义医学院 | Preparation method of high-activity mesoporous hydrated titanium oxide powder |
| CN107640801A (en) * | 2017-10-12 | 2018-01-30 | 黑龙江大学 | A kind of method of photocatalysis coupled filtering integral PROCESS FOR TREATMENT phenol wastewater |
| CN107827152A (en) * | 2017-11-09 | 2018-03-23 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide for carbon dioxide photocatalysis synthesizing methane and preparation method thereof |
| CN113209954A (en) * | 2021-05-12 | 2021-08-06 | 南昌航空大学 | Preparation method of titanium dioxide surface heterojunction hybrid material |
| CN115067359A (en) * | 2022-06-21 | 2022-09-20 | 重庆德强化工有限公司 | Ag ion-loaded black TiO 2 Nano photocatalytic bactericidal material and preparation method thereof |
| CN116375499A (en) * | 2023-01-04 | 2023-07-04 | 盐城工学院 | Black TiO 2 Preparation method of basic photocatalytic concrete ecological brick and application of basic photocatalytic concrete ecological brick in purifying automobile exhaust |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105056925A (en) * | 2015-09-07 | 2015-11-18 | 黑龙江大学 | Preparation method of black titanium dioxide nano rod visible light catalyst |
| CN105195133A (en) * | 2015-09-18 | 2015-12-30 | 黑龙江大学 | Preparation method of molybdenum disulfide-black titanium dioxide composite visible-light-driven photocatalyst for hydrogen production |
| CN105618022A (en) * | 2016-01-12 | 2016-06-01 | 遵义医学院 | Preparation method of high-activity mesoporous hydrated titanium oxide powder |
| CN105618022B (en) * | 2016-01-12 | 2018-09-18 | 遵义医学院 | A kind of mesoporous hydrous titanium oxide raw powder's production technology of high activity |
| CN107640801A (en) * | 2017-10-12 | 2018-01-30 | 黑龙江大学 | A kind of method of photocatalysis coupled filtering integral PROCESS FOR TREATMENT phenol wastewater |
| CN107827152A (en) * | 2017-11-09 | 2018-03-23 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide for carbon dioxide photocatalysis synthesizing methane and preparation method thereof |
| CN107827152B (en) * | 2017-11-09 | 2019-07-16 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide and preparation method thereof for carbon dioxide photocatalysis synthesizing methane |
| CN113209954A (en) * | 2021-05-12 | 2021-08-06 | 南昌航空大学 | Preparation method of titanium dioxide surface heterojunction hybrid material |
| CN115067359A (en) * | 2022-06-21 | 2022-09-20 | 重庆德强化工有限公司 | Ag ion-loaded black TiO 2 Nano photocatalytic bactericidal material and preparation method thereof |
| CN115067359B (en) * | 2022-06-21 | 2024-03-19 | 重庆德强化工有限公司 | Ag ion-loaded black TiO 2 Nanometer photocatalysis sterilization material and preparation method thereof |
| CN116375499A (en) * | 2023-01-04 | 2023-07-04 | 盐城工学院 | Black TiO 2 Preparation method of basic photocatalytic concrete ecological brick and application of basic photocatalytic concrete ecological brick in purifying automobile exhaust |
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Application publication date: 20150325 |