CN104841471A - Method for doping TiO2 and ammonia water modified carrier activated carbon in Fe to prepare Fe-TiO2/N-AC photocatalyst - Google Patents
Method for doping TiO2 and ammonia water modified carrier activated carbon in Fe to prepare Fe-TiO2/N-AC photocatalyst Download PDFInfo
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- CN104841471A CN104841471A CN201510221735.1A CN201510221735A CN104841471A CN 104841471 A CN104841471 A CN 104841471A CN 201510221735 A CN201510221735 A CN 201510221735A CN 104841471 A CN104841471 A CN 104841471A
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Abstract
The invention discloses a method for doping TiO2 and ammonia water modified carrier activated carbon in Fe to prepare Fe-TiO2/N-AC photocatalyst. The method includes the following steps: (1), mixing anhydrous ethanol, deionized water, ferric salt and diluted ammonia water to prepare a mixed solution A; (2), mixing anhydrous ethanol, methyl cellulose and tetrabutyl titanate to prepare a mixed solution B1; (3), mixing activated carbon, the mixed solution A and the mixed solution B1 to prepare a mixed solution C; (4) preparing a mixed solution B2; (5), dropwise adding all of the mixed solution B2 into the mixed solution C; (6), filtering a solution acquired in step (5), and drying, cooling, roasting and cooling a filter cake to acquire the Fe-TiO2/N-AC photocatalyst. The Fe-TiO2/N-AC photocatalyst is prepared by adopting a two-step method, TiO2 serving as an active component is modified through metal Fe, and ammonia water is utilized to perform surface modifying on carrier activated carbon, so that photocatalytic activity of the photocatalyst is improved to greatest extent, and degradation rate of the photocatalyst to printing and dyeing secondary wastewater can reach 70%.
Description
Technical field
The invention belongs to catalysis material preparing technical field, be specifically related to a kind of Fe doped Ti O
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst.
Background technology
Along with the development of economy, environmental problem becomes the outstanding problem that the whole world is paid close attention to day by day, the continuous aggravation of air, water pollution, serious threat is to the survival and development of the mankind, and how effectively degraded and elimination environmental contaminants have become a most active research direction.Because photocatalysis technology can carry out at normal temperatures and pressures, relatively more thorough to organic degraded, and the advantage not having secondary pollution etc. to give prominence to, be the best approach of generally acknowledging at present.The key of photocatalysis technology is the preparation of photochemical catalyst, especially with supported titanium
2most widely used.
At present, the photochemical catalyst of use mainly active carbon (AC) supported titanium
2.TiO
2energy level be discontinuous, under normality, electronics can only move in the energy level track of valence band, and after the light quantum being subject to energy and being greater than energy gap excites, electronics just transits to conduction band, makes valence band produce hole.Therefore, the component of doping is selected to enter into TiO
2lattice structure inner, in its band gap, introduce impurity energy level and defect level, thus make TiO
2band-gap energy diminish, under the irradiation of the lower light of energy, just can produce photo-generate electron-hole pair, thus improve the organic photocatalytic activity of photocatalytic oxidation degradation.The doping component available metal ion doping of modification, nonmetallic ion-doped and codope etc.Gan Lihua etc. will mix iron TiO by infusion process
2colloidal sol loads to preparation on active carbon and mixes iron TiO
2-active carbon photocatalysis composite, as described in Chinese invention patent CN1899686A.In Chinese invention patent 201410028900.7, describe a kind of by nitrogen-doped nanometer titanium dioxide and activated carbon fiber-loaded, prepare the method for nitrogen-doped nanometer titanium dioxide supported active carbon fiber composite.In Chinese invention patent 201110093927.0, describe the preparation method of a kind of platinum, nitrogen codoped active carbon supported titanium dioxide photocatalyst.
The preparation method TiO of traditional photochemical catalyst
2/ AC photocatalysis is TiO
2the result that high light catalytic activity and the strong absorption property of AC have been worked in coordination with, no matter being metal ion-modified, nonmetallic modifying or codoping modified at present, is all for TiO
2modification, only improve TiO
2high light catalytic activity, does not improve the absorption property of AC.
Summary of the invention
The present invention is in order to solve prior art only for TiO
2modification and the improvement that have ignored AC absorption property, a kind of Fe doped Ti O is provided
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, not by means of only metal ion to active component TiO
2carry out modification, and finishing is carried out to carrier active carbon, improve the photocatalytic activity of photochemical catalyst to greatest extent.
For achieving the above object, the technical solution used in the present invention is: a kind of Fe doped Ti O
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, comprises the steps:
(1), after absolute ethyl alcohol and deionized water fully being mixed, vigorous stirring, then adds molysite and weak aqua ammonia, is configured to mixed solution A;
(2) absolute ethyl alcohol is fully mixed with methylcellulose, vigorous stirring, then add tetrabutyl titanate, be configured to mixed solution B1;
(3) active carbon is joined in mixed solution A, after vigorous stirring, add step (2) gained mixed solution B1, and keep constant temperature in dropping process, form mixed solution C;
(4) repeat step (2), prepare mixed solution B2;
(5) under temperature constant state, mixed solution B2 is all added drop-wise in mixed solution C;
(6), after solution step (5) obtained filters, carry out drying to filter cake, taking-up after drying completes also is cooled to room temperature; At 350 DEG C ~ 600 DEG C, after roasting 2 ~ 8h, naturally cool to room temperature, obtain modified Fe-TiO
2/ N-AC photochemical catalyst.
Wherein, in step (1), the volume ratio of described absolute ethyl alcohol and deionized water is 1 ~ 10:1.Molysite is one or more mixing in ferric sulfate, ferric nitrate and ferric carbonate, and molysite preferably sulfuric acid iron, the mass volume ratio of itself and absolute ethyl alcohol and deionized water mixed solution is 0.1 ~ 1g/mL.In described weak aqua ammonia, the mass concentration of ammonia is 1 ~ 5%, and weak aqua ammonia is 1:5 ~ 20 with absolute ethyl alcohol and deionized water mixed liquor volume ratio.
Wherein, in step (2), the mass volume ratio of described methylcellulose and absolute ethyl alcohol is 0.005 ~ 0.02g/mL, and the volume ratio of tetrabutyl titanate and absolute ethyl alcohol is 1:5 ~ 10.
Wherein, in step (3), the particle diameter of described active carbon is 0.1 ~ 2mm, and the mass volume ratio of active carbon and mixed solution A is 0.01 ~ 0.1g/mL.The mixed solution B1 rate of addition be added drop-wise in mixed solution A is 0.5 ~ 5mL/min, and temperature is 15 ~ 40 DEG C.
Wherein, in step (5), mixed solution B2 is added drop-wise to the rate of addition 0.5 ~ 5mL/min in mixed solution C, and temperature is 15 ~ 40 DEG C.
Wherein, in step (6), the baking temperature of described filter cake 100 ~ 120 DEG C, drying time 6 ~ 12h.
Further, above-mentioned Fe-TiO
2when/N-AC photochemical catalyst is for the treatment of dyeing waste water, Fe-TiO
2the mass volume ratio of/N-AC photochemical catalyst and dyeing waste water is 1 ~ 5g/L, and UV power is 100 ~ 500W, processing time 5 ~ 10h, and wastewater degradation rate is 50 ~ 70%.
Because technique scheme is used, the present invention compared with prior art has following advantages:
The present invention prepares photochemical catalyst by two-step method, compared with traditional once through method in Sol Gel process, titanium Ester hydrolysis technique, not only increases the yield of catalyst, and has saved the consumption of solvent-absolute ethyl alcohol.The present invention is not by means of only metal pair active component TiO
2carry out modification, and utilize ammoniacal liquor to carry out finishing to carrier active carbon, improve the photocatalytic activity of photochemical catalyst to greatest extent, be particularly useful for when printing and dyeing secondary waste water is degraded effective, photochemical catalyst is reusable after cleaning, drying.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment one:
After fully being mixed with 10mL deionized water by 10mL absolute ethyl alcohol, vigorous stirring, adds 1g ferric sulfate and 1mL ammonia mass concentration is the weak aqua ammonia of 5%, is configured to mixed solution A;
10mL absolute ethyl alcohol is fully mixed with 0.05g methylcellulose (dispersant), vigorous stirring, add 2mL tetrabutyl titanate, be configured to mixed solution B1;
Taking 0.12g particle diameter is that the active carbon of 2nm joins in mixed solution A, and after vigorous stirring, add step (2) gained mixed solution B1 with the speed of dripping of 1mL/min, in dropping process, control temperature is at 15 DEG C, generates mixed solution C;
10mL absolute ethyl alcohol is fully mixed with 0.05g methylcellulose (dispersant), vigorous stirring, add 2mL tetrabutyl titanate, be configured to mixed solution B2;
Keep 40 DEG C of temperature, mixed solution B2 is joined in mixed solution C with the speed of dripping of 0.5mL/min;
The mixed solution that obtains is filtered, to filter cake at 100 DEG C after dry 12h, is dryly cooled to room temperature; Then roasting 2h at 600 DEG C, naturally cools to room temperature, obtains modified Fe-TiO
2/ N-AC photochemical catalyst.
By the Fe-TiO of preparation
2/ N-AC photochemical catalyst is used for treatment of dyeing wastewater, and the initial COD of dyeing waste water is 200mg/L, Fe-TiO
2the mass volume ratio of/N-AC photochemical catalyst and dyeing waste water is 1g/L, and UV power is 100W, processing time 5h, and wastewater degradation rate is 50%.
Embodiment two:
After fully being mixed with 2mL deionized water by 10mL absolute ethyl alcohol, vigorous stirring, adds 2.4g ferric sulfate and 2.4mL ammonia mass concentration is the weak aqua ammonia of 3%, is configured to mixed solution A;
10mL absolute ethyl alcohol is fully mixed with 0.2g methylcellulose, vigorous stirring, add 1mL tetrabutyl titanate, be configured to mixed solution B1;
Taking 1.1g particle diameter is that the active carbon of 1nm joins in mixed solution A, after vigorous stirring, add step (2) gained mixed solution B1, and control temperature controls 40 DEG C, generates mixed solution C with the speed of dripping of 5mL/min;
10mL absolute ethyl alcohol is fully mixed with 0.2g methylcellulose, vigorous stirring, add 1mL tetrabutyl titanate, be configured to mixed solution B2;
Keep temperature 20 DEG C, mixed solution B2 is joined in mixed solution C with the speed of dripping of 1mL/min;
The mixed solution that obtains is filtered, to filter cake at 120 DEG C after dry 6h, is dryly cooled to room temperature; Then roasting 8h at 350 DEG C, naturally cools to room temperature, obtains modified Fe-TiO
2/ N-AC photochemical catalyst.
By the Fe-TiO of preparation
2/ N-AC photochemical catalyst is used for treatment of dyeing wastewater, and the initial COD of dyeing waste water is 200mg/L, Fe-TiO
2the mass volume ratio of/N-AC photochemical catalyst and waste water is 5g/L, and UV power is 500W, processing time 10h, and wastewater degradation rate is 70%.
Embodiment three:
After fully being mixed with 2mL deionized water by 20mL absolute ethyl alcohol, vigorous stirring, adds 2.2g ferric sulfate and 2mL ammonia mass concentration is the weak aqua ammonia of 1%, is configured to mixed solution A;
10mL absolute ethyl alcohol is fully mixed with 0.1g methylcellulose, vigorous stirring, add 1.5mL tetrabutyl titanate, be configured to mixed solution B1;
Taking 2.4g particle diameter is that the active carbon of 0.8nm joins in mixed solution A, and after vigorous stirring, join in above-mentioned solution by the mixed solution B1 in step (2) with the speed of dripping of 3mL/min, this process temperature controls at 30 DEG C, generates mixed solution C;
10mL absolute ethyl alcohol is fully mixed with 0.1g methylcellulose, under vigorous stirring, adds 1.5mL tetrabutyl titanate, be configured to mixed solution B2;
Join in mixed solution C by mixed solution B2 with the speed of dripping of 3mL/min, this process temperature controls at 15 DEG C;
The mixed solution that obtains is filtered, to filter cake at 110 DEG C after dry 4h, is dryly cooled to room temperature; Then roasting 6h at 450 DEG C, naturally cools to room temperature, obtains modified Fe-TiO
2/ N-AC photochemical catalyst.
By the Fe-TiO of preparation
2/ N-AC photochemical catalyst is used for treatment of dyeing wastewater, and the initial COD of dyeing waste water is 200mg/L, Fe-TiO
2the mass volume ratio of/N-AC photochemical catalyst and waste water is 2g/L, and UV power is 300W, processing time 8h, and wastewater degradation rate is 57%.
Embodiment four:
After fully being mixed with 10mL deionized water by 20mL absolute ethyl alcohol, vigorous stirring, adds 2.1g ferric sulfate and 3mL ammonia mass concentration is the weak aqua ammonia of 2%, is configured to mixed solution A;
10mL absolute ethyl alcohol is fully mixed with 0.12g methylcellulose (dispersant), under vigorous stirring, adds 1.2mL tetrabutyl titanate, be configured to mixed solution B1;
Taking 1.8g particle diameter is that the active carbon of 0.1nm joins in mixed solution A, after vigorous stirring, join in above-mentioned mixed solution by the mixed solution B1 in step (2) with the speed of dripping of 2mL/min, this process temperature controls at 25 DEG C, generates mixed solution C;
10mL absolute ethyl alcohol is fully mixed with 0.12g methylcellulose (dispersant), under vigorous stirring, adds 1.2mL tetrabutyl titanate, be configured to mixed solution B2;
Join in mixed solution C by mixed solution B2 with the speed of dripping of 5mL/min, this process temperature controls at 30 DEG C;
After being filtered the mixed solution that obtains, to filter cake dry 3h at 115 DEG C, be more dryly cooled to room temperature; Then roasting 4h at 550 DEG C, naturally cools to room temperature, obtains modified Fe-TiO
2/ N-AC photochemical catalyst.
By the Fe-TiO of preparation
2/ N-AC photochemical catalyst is used for treatment of dyeing wastewater, and the initial COD of dyeing waste water is 200mg/L, Fe-TiO
2the mass volume ratio of/N-AC photochemical catalyst and dyeing waste water is 3g/L, and UV power is 400W, processing time 7h, and wastewater degradation rate is 62%.
The present invention prepares photochemical catalyst by two-step method, compared with traditional once through method in Sol Gel process, titanium Ester hydrolysis technique, not only increases the yield of catalyst, and has saved the consumption of solvent-absolute ethyl alcohol.The present invention is not by means of only metal pair active component TiO
2carry out modification, and utilize ammoniacal liquor to carry out finishing to carrier active carbon, improve the photocatalytic activity of photochemical catalyst to greatest extent, be particularly useful for when printing and dyeing secondary waste water is degraded effective, photochemical catalyst is reusable.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvement or replacement, these improve or replace and also should be considered as protection scope of the present invention.
Claims (10)
1. a Fe doped Ti O
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, comprises the steps:
(1), after absolute ethyl alcohol and deionized water fully being mixed, vigorous stirring, then adds molysite and weak aqua ammonia, is configured to mixed solution A;
(2) absolute ethyl alcohol is fully mixed with methylcellulose, vigorous stirring, then add tetrabutyl titanate, be configured to mixed solution B1;
(3) active carbon is joined in mixed solution A, after vigorous stirring, add step (2) gained mixed solution B1, and keep constant temperature in dropping process, form mixed solution C;
(4) repeat step (2), prepare mixed solution B2;
(5) under temperature constant state, mixed solution B2 is all added drop-wise in mixed solution C;
(6), after solution step (5) obtained filters, carry out drying to filter cake, taking-up after drying completes also is cooled to room temperature; At 350 DEG C ~ 600 DEG C, after roasting 2 ~ 8h, naturally cool to room temperature, obtain modified Fe-TiO
2/ N-AC photochemical catalyst.
2. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (1), the volume ratio of described absolute ethyl alcohol and deionized water is 1 ~ 10:1.
3. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, the molysite in step (1) is ferric sulfate, and the mass volume ratio of described ferric sulfate and absolute ethyl alcohol and deionized water mixed solution is 0.1 ~ 1g/mL.
4. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (1), in described weak aqua ammonia, the mass concentration of ammonia is 1 ~ 5%, and weak aqua ammonia is 1:5 ~ 20 with absolute ethyl alcohol and deionized water mixed liquor volume ratio.
5. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (2), the mass volume ratio of described methylcellulose and absolute ethyl alcohol is 0.005 ~ 0.02g/mL, and the volume ratio of tetrabutyl titanate and absolute ethyl alcohol is 1:5 ~ 10.
6. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (3), the particle diameter of described active carbon is 0.1 ~ 2mm, and the mass volume ratio of active carbon and mixed solution A is 0.01 ~ 0.1g/mL.
7. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (3), the mixed solution B1 rate of addition be added drop-wise in mixed solution A is 0.5 ~ 5mL/min, and temperature is 15 ~ 40 DEG C.
8. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (5), mixed solution B2 is added drop-wise to the rate of addition 0.5 ~ 5mL/min in mixed solution C, and temperature is 15 ~ 40 DEG C.
9. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, in step (6), the baking temperature of described filter cake 100 ~ 120 DEG C, drying time 6 ~ 12h.
10. Fe doped Ti O according to claim 1
2, ammoniacal liquor modified support active carbon prepares Fe-TiO
2the method of/N-AC photochemical catalyst, is characterized in that, described Fe-TiO
2when/N-AC photochemical catalyst is for the treatment of dyeing waste water, Fe-TiO
2the mass volume ratio of/N-AC photochemical catalyst and dyeing waste water is 1 ~ 5g/L, and UV power is 100 ~ 500W, processing time 5 ~ 10h, and wastewater degradation rate is 50 ~ 70%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106799230A (en) * | 2017-01-16 | 2017-06-06 | 浙江大学 | A kind of charcoal based composite catalyst and its preparation method and application |
| CN109592752A (en) * | 2019-01-03 | 2019-04-09 | 江苏理工学院 | A kind of preparation method of three-phase three-dimensional photovoltaic reaction filler |
| CN109759110A (en) * | 2019-01-03 | 2019-05-17 | 华南理工大学 | A kind of N doping porous carbon loaded titanium dioxide photocatalyst and the preparation method and application thereof |
| CN112844351A (en) * | 2021-01-08 | 2021-05-28 | 杭州神起科技有限公司 | Flower-shaped Fe-doped TiO2Preparation method and application of porous carbon-loaded composite material |
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| CN1899686A (en) * | 2006-07-24 | 2007-01-24 | 同济大学 | Process for preparing iron blended TiO2/active carbon composite visible light catalyst |
| CN101219371A (en) * | 2007-01-08 | 2008-07-16 | 北京化工大学 | Photocatalysis oxidation treated high concentration organic trade waste |
| CN101791570A (en) * | 2010-03-24 | 2010-08-04 | 南京工业大学 | Loaded photocatalyst and preparation method thereof |
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2015
- 2015-05-05 CN CN201510221735.1A patent/CN104841471A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899686A (en) * | 2006-07-24 | 2007-01-24 | 同济大学 | Process for preparing iron blended TiO2/active carbon composite visible light catalyst |
| CN101219371A (en) * | 2007-01-08 | 2008-07-16 | 北京化工大学 | Photocatalysis oxidation treated high concentration organic trade waste |
| CN101791570A (en) * | 2010-03-24 | 2010-08-04 | 南京工业大学 | Loaded photocatalyst and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106799230A (en) * | 2017-01-16 | 2017-06-06 | 浙江大学 | A kind of charcoal based composite catalyst and its preparation method and application |
| CN109592752A (en) * | 2019-01-03 | 2019-04-09 | 江苏理工学院 | A kind of preparation method of three-phase three-dimensional photovoltaic reaction filler |
| CN109759110A (en) * | 2019-01-03 | 2019-05-17 | 华南理工大学 | A kind of N doping porous carbon loaded titanium dioxide photocatalyst and the preparation method and application thereof |
| CN109759110B (en) * | 2019-01-03 | 2022-04-22 | 华南理工大学 | Nitrogen-doped porous carbon loaded titanium dioxide photocatalyst and preparation method and application thereof |
| CN112844351A (en) * | 2021-01-08 | 2021-05-28 | 杭州神起科技有限公司 | Flower-shaped Fe-doped TiO2Preparation method and application of porous carbon-loaded composite material |
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Application publication date: 20150819 |