CN102489290A - Preparation method of nano bismuth vanadate photocatalyst loaded on active carbon fiber - Google Patents
Preparation method of nano bismuth vanadate photocatalyst loaded on active carbon fiber Download PDFInfo
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- CN102489290A CN102489290A CN2011103583342A CN201110358334A CN102489290A CN 102489290 A CN102489290 A CN 102489290A CN 2011103583342 A CN2011103583342 A CN 2011103583342A CN 201110358334 A CN201110358334 A CN 201110358334A CN 102489290 A CN102489290 A CN 102489290A
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- activated carbon
- metavanadate
- photochemical catalyst
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Abstract
The invention relates to a preparation method of a nano bismuth vanadate photocatalyst loaded on an active carbon fiber. The preparation method comprises the following steps of: (1) adding bismuth salt and a stabilizing agent into a phosphate buffering solution, stirring and forming a suspension liquid; dissolving metavanadate in the phosphate buffering solution, then adding into the suspension liquid, and stirring uniformly, thus forming a transparent solution; and (2) using an alkaline solution to adjust the pH value of the transparent solution to be 6.0-8.0, then adding the active carbon fiber at the temperature of 40-100 DEG C, stirring and mixing uniformly, then centrifuging, filtering, cleaning, and then adding into a muffle furnace for calcinations; and finally cooling and grinding, thus obtaining the nano bismuth vanadate photocatalyst. The preparation method is simple and practicable, and is low in requirement for equipment and good in operability; and the loading of the active carbon fiber for powdery bismuth vanadate is uniform, persistently toxic and harmful substances can be degraded efficiently under the conditions of ultraviolet and visible lights, the utilization is simple and convenient and the recovery and the regeneration can be achieved.
Description
Technical field
The invention belongs to the preparation field of nanometer pucherite photochemical catalyst, particularly a kind of preparation method of activated carbon fiber loaded nanometer pucherite photochemical catalyst.
Background technology
In recent years, with titanium dioxide (TiO
2) for the photocatalysis technology of core representative in the environmental pollution improvement field; Particularly the application in waste water difficult for biological degradation processing and air cleaning more and more widely; But because its greater band gap; Only can under UV-irradiation, just have photocatalysis, thereby limit the further expansion of its application.In order to improve TiO
2To the utilization ratio of sunshine, lot of domestic and international experts and scholars are round visible light-responded TiO
2Photochemical catalyst has launched number of research projects, is primarily aimed at TiO
2Photocatalyst surface is structurally-modified, inorganic elements and doped with metal elements modification etc., is intended to enlarge its spectral response range, improves its visible light catalysis activity.However, the TiO of process modification
2Photochemical catalyst still exists problems such as visible light catalysis activity is undesirable, and the light degradation ability is relatively poor at this stage, causes its practicality relatively poor.
Nearest discovers to have the composite oxides pucherite (BiVO of monoclinic system scheelite-type structure
4) under radiation of visible light, just have photocatalytic activity, can produce oxygen and degradable organic pollutant by the decomposition water molecule, be a kind of potential photochemical catalyst.Yet, BiVO
4Absorption property very poor, and the photo-generated carrier that produces is difficult to migration, easy compound, thereby influenced its visible light activity.At present about being directed against BiVO
4Composite modified less with the research report that mixes, in addition about it being carried on the good porous material of absorption property, also few like the report of active carbon etc.; Therefore; How strengthening its absorption in visible-range, and improve its visible light catalysis activity, is to research and develop BiVO at present
4The main research emphasis of high efficiency photocatalyst.
The sewage disposal conventional method mainly contains: physical partition method, biological degradation method, chemical decomposition method etc.; But all there is certain limitation in these methods; Therefore, the researcher begins to be devoted to develop efficient, low energy consumption, applied widely and the water treatment technology of deep oxidation ability arranged.In recent years, a lot of scholars are with TiO
2Be used for the organic pollution of photocatalytic degradation water body, though obtained certain effect, because the restriction of its photoresponse scope causes treatment effect often not ideal enough.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of activated carbon fiber loaded nanometer pucherite photochemical catalyst; Operation is simple for this method; To equipment require low; The activated carbon fiber pucherite load of preparation is even, can be under ultraviolet light and visible light condition efficient degradation persistence poisonous and harmful substance.
The preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst of the present invention comprises:
(1) bismuth salt, stabilizing agent are joined in the phosphate buffer, stir and form suspension; Metavanadate is dissolved in the phosphate buffer, joins then in the above-mentioned suspension, stir, form clear solution; Wherein the amount of substance concentration of bismuth salt and metavanadate is 0.05～0.25mol/L, and the amount of substance concentration of stabilizing agent is 0.01～0.05mol/L;
(2) the pH value of using alkaline solution to regulate above-mentioned clear solution is 6.0～8.0, adds activated carbon fiber down at 40～100 ℃ then, be stirred to mix the back centrifugal, filter, wash; Put into Muffle furnace again; At 250～400 ℃ of following roasting 3～6h,, promptly get after cooling is ground; The activated carbon fiber that wherein adds and the mass ratio of bismuth salt are 2～10: 1.
The mixing time that stirring described in the step (1) forms in the suspension is 30～60min.
Bismuth salt described in the step (1) is bismuth nitrate, bismuth chloride or bismuth acetate.
Stabilizing agent described in the step (1) is gluconic acid sodium salt, disodium ethylene diamine tetraacetate or BTCA.
Metavanadate described in the step (1) is sodium metavanadate, potassium metavanadate or ammonium metavanadate.
The mol ratio of bismuth salt described in the step (1) and metavanadate is 1: 1.
Phosphate buffer described in the step (1) is that the potassium dihydrogen phosphate of 0.05mol/L and the NaOH of 0.035mol/L are formed by amount of substance concentration.
Alkaline solution described in the step (2) is NaOH or the potassium hydroxide aqueous solution of concentration 1.0mol/L～3.0mol/L.
Activated carbon fiber itself is a kind of well behaved adsorbent, have specific area big with characteristics such as high adsorption capacity, in water treatment applications, can also reach the beneficial effect of inorganic pollutions such as absorption removal heavy metal ion simultaneously.The present invention utilizes characteristics such as the unique stratiform hollow structure characteristic of activated carbon fiber, specific area are big, high adsorption capacity, in conjunction with BiVO
4Visible light catalysis activity, the success with nanometer BiVO
4Load on the activated carbon fiber; Be prepared into and have the visible light-responded catalysis material of high catalytic activity; And be applied to the advanced treating of bio-refractory waste water; Can realize efficient removal, particularly conventional treatment is difficult to the effectively persistence micropollutants of removal organic pollution in the water, and the non-secondary pollution problem.
Beneficial effect
(1) preparation method of the present invention is simple, to equipment require lowly, operability is good;
(2) the activated carbon fiber powder pucherite load of the present invention preparation is even, can be under ultraviolet light and visible light condition efficient degradation persistence poisonous and harmful substance, utilize easy and recyclable regeneration.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) bismuth nitrate, disodium ethylene diamine tetraacetate are joined in the phosphate buffer, magnetic agitation 30min forms suspension; Sodium metavanadate evenly is dissolved in phosphate buffer earlier, dropwise joins then in the above-mentioned suspension, constantly magnetic agitation is even, forms clear solution; Wherein bismuth nitrate is 0.05mol/L with the amount of substance concentration of inclined to one side sodium vanadate; Disodium ethylene diamine tetraacetate amount of substance concentration is 0.01mol/L, and phosphate buffer is that the potassium dihydrogen phosphate of 0.05mol/L and the NaOH of 0.035mol/L are formed by amount of substance concentration;
(2) adopting concentration is that the pH value that the sodium hydroxide solution of 1.0mol/L is regulated above-mentioned clear solution is 6.0, and at 40 ℃ of adding activated carbon fibers down, the mass ratio of bismuth nitrate and activated carbon fiber is 1: 2 then; Magnetic agitation is mixed continuously, and centrifugal, filtration is after the washing; Put into Muffle furnace; At 250 ℃ of following roasting 3h, after cooling is ground, the activated carbon fiber photochemical catalyst powder of nanometer pucherite that promptly got load.
Embodiment 2
(1) bismuth acetate, BTCA are joined in the phosphate buffer, magnetic agitation 45min forms suspension; Potassium metavanadate evenly is dissolved in phosphate buffer earlier, dropwise joins then in the above-mentioned suspension, constantly magnetic agitation is even, forms clear solution; Wherein bismuth acetate and potassium metavanadate amount of substance concentration are 0.15mol/L, and BTCA amount of substance concentration is 0.025mol/L, and phosphate buffer is that the potassium dihydrogen phosphate of 0.05mol/L and the NaOH of 0.035mol/L are formed by amount of substance concentration;
(2) adopting concentration is that the pH value that the sodium hydrate aqueous solution of 2.0mol/L is regulated above-mentioned clear solution is 7.0, and at 70 ℃ of adding activated carbon fibers down, the mass ratio of bismuth acetate and activated carbon fiber is 1: 5 then; Magnetic agitation is mixed continuously, and centrifugal, filtration is after the washing; Put into Muffle furnace; At 320 ℃ of following roasting 5h, after cooling is ground, the activated carbon fiber photochemical catalyst powder of nanometer pucherite that promptly got load.
Embodiment 3
(1) bismuth chloride, gluconic acid sodium salt are joined in the phosphate buffer, magnetic agitation 60min forms suspension; Ammonium metavanadate evenly is dissolved in phosphate buffer earlier, dropwise joins then in the above-mentioned suspension, constantly magnetic agitation is even, forms clear solution; Wherein bismuth chloride and ammonium metavanadate amount of substance concentration are 0.25mol/L, and gluconic acid sodium salt amount of substance concentration is 0.05mol/L, and phosphate buffer is that the potassium dihydrogen phosphate of 0.05mol/L and the NaOH of 0.035mol/L are formed by amount of substance concentration;
(2) adopting concentration is that the pH value that the potassium hydroxide aqueous solution of 3.0mol/L is regulated above-mentioned clear solution is 8.0, and at 100 ℃ of adding activated carbon fibers down, the mass ratio of bismuth chloride and activated carbon fiber is 1: 10 then; Magnetic agitation is mixed continuously, and centrifugal, filtration is after the washing; Put into Muffle furnace; At 400 ℃ of following roasting 6h, after cooling is ground, the activated carbon fiber photochemical catalyst powder of nanometer pucherite that promptly got load.
Embodiment 4
The wastewater treatment experiment: the mixing dyeing waste water with the final discharging of certain printing and dyeing mill is a process object; After the micro-filtrate membrane filtration preliminary treatment; Add same amount therein respectively through embodiment 1～example 3 prepared photochemical catalysts, under sunshine, shine 4h continuously, decolorization of dyeing rate and COD
CrClearance is as shown in the table respectively:
| Percent of decolourization | COD CrClearance | |
| Embodiment 1 | 95.2％ | 91.1％ |
| Embodiment 2 | 99.1％ | 97.7％ |
| Embodiment 3 | 98.5％ | 96.1％ |
Claims (8)
1. the preparation method of an activated carbon fiber loaded nanometer pucherite photochemical catalyst comprises:
(1) bismuth salt, stabilizing agent are joined in the phosphate buffer, stir and form suspension; Metavanadate is dissolved in the phosphate buffer, joins then in the above-mentioned suspension, stir, form clear solution; Wherein the amount of substance concentration of bismuth salt and metavanadate is 0.05～0.25mol/L, and the amount of substance concentration of stabilizing agent is 0.01～0.05mol/L;
(2) the pH value of using alkaline solution to regulate above-mentioned clear solution is 6.0～8.0, adds activated carbon fiber down at 40～100 ℃ then, be stirred to mix the back centrifugal, filter, wash; Put into Muffle furnace again; At 250～400 ℃ of following roasting 3～6h,, promptly get after cooling is ground; The activated carbon fiber that wherein adds and the mass ratio of bismuth salt are 2～10: 1.
2. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the mixing time that the stirring described in the step (1) forms in the suspension is 30～60min.
3. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the bismuth salt described in the step (1) is bismuth nitrate, bismuth chloride or bismuth acetate.
4. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the stabilizing agent described in the step (1) is gluconic acid sodium salt, disodium ethylene diamine tetraacetate or BTCA.
5. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the metavanadate described in the step (1) is sodium metavanadate, potassium metavanadate or ammonium metavanadate.
6. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the mol ratio of bismuth salt described in the step (1) and metavanadate is 1: 1.
7. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the phosphate buffer described in the step (1) is that the potassium dihydrogen phosphate of 0.05mol/L and the NaOH of 0.035mol/L are formed by amount of substance concentration.
8. the preparation method of a kind of activated carbon fiber loaded nanometer pucherite photochemical catalyst according to claim 1 is characterized in that: the alkaline solution described in the step (2) is NaOH or the potassium hydroxide aqueous solution of concentration 1.0mol/L～3.0mol/L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102861567A (en) * | 2012-08-23 | 2013-01-09 | 南京大学 | Floating type BiVO4/floating bead composite photocatalyst and preparation method and application thereof |
| CN103623805A (en) * | 2013-07-17 | 2014-03-12 | 上海市环境科学研究院 | Active carbon fiber-loaded NaBiO3-based composite oxide and preparation method thereof, and method for degrading organic dye waste water by using composite oxide |
| CN103736480A (en) * | 2013-12-24 | 2014-04-23 | 桂林电子科技大学 | Quadrangle starlike pucherite for optical catalytic materials as well as preparation method thereof |
| CN103920508A (en) * | 2014-03-28 | 2014-07-16 | 山东大学 | Nitrated carbon fiber loaded bismuth oxyhalide nanoflower and preparation method of nanoflower |
| CN104475100A (en) * | 2014-12-25 | 2015-04-01 | 东华大学 | Preparation method of carbon nano tube composite bismuth molybdate environmentally friendly and deep water treatment agent |
| CN106732805A (en) * | 2016-12-02 | 2017-05-31 | 东华大学 | A kind of fiber/CNT/BiVO4 three-dimensional recyclable efficient catalytic material and its preparation and application |
| CN107413326A (en) * | 2017-05-03 | 2017-12-01 | 东北大学 | A kind of carbon fiber supported liquid membrane burning prepares high activity CQDs/BiVO4The method of composite Nano catalysis material |
| CN112221483A (en) * | 2020-10-27 | 2021-01-15 | 上海市环境科学研究院 | Modularized supported bismuth vanadate photocatalytic material and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102861567A (en) * | 2012-08-23 | 2013-01-09 | 南京大学 | Floating type BiVO4/floating bead composite photocatalyst and preparation method and application thereof |
| CN102861567B (en) * | 2012-08-23 | 2014-05-21 | 南京大学 | Floating type BiVO4/floating bead composite photocatalyst and preparation method and application thereof |
| CN103623805A (en) * | 2013-07-17 | 2014-03-12 | 上海市环境科学研究院 | Active carbon fiber-loaded NaBiO3-based composite oxide and preparation method thereof, and method for degrading organic dye waste water by using composite oxide |
| CN103623805B (en) * | 2013-07-17 | 2015-12-09 | 上海市环境科学研究院 | Activated carbon fiber-loaded based on NaBiO 3composite oxides and preparation method thereof and the method utilizing its degrading organic dye waste water |
| CN103736480A (en) * | 2013-12-24 | 2014-04-23 | 桂林电子科技大学 | Quadrangle starlike pucherite for optical catalytic materials as well as preparation method thereof |
| CN103736480B (en) * | 2013-12-24 | 2016-06-08 | 桂林电子科技大学 | A kind of corner star pucherite as catalysis material and preparation method thereof |
| CN103920508A (en) * | 2014-03-28 | 2014-07-16 | 山东大学 | Nitrated carbon fiber loaded bismuth oxyhalide nanoflower and preparation method of nanoflower |
| CN104475100A (en) * | 2014-12-25 | 2015-04-01 | 东华大学 | Preparation method of carbon nano tube composite bismuth molybdate environmentally friendly and deep water treatment agent |
| CN104475100B (en) * | 2014-12-25 | 2016-11-16 | 东华大学 | A kind of CNT is combined the preparation method of bismuth molybdate green deep water treatment agent |
| CN106732805A (en) * | 2016-12-02 | 2017-05-31 | 东华大学 | A kind of fiber/CNT/BiVO4 three-dimensional recyclable efficient catalytic material and its preparation and application |
| CN107413326A (en) * | 2017-05-03 | 2017-12-01 | 东北大学 | A kind of carbon fiber supported liquid membrane burning prepares high activity CQDs/BiVO4The method of composite Nano catalysis material |
| CN112221483A (en) * | 2020-10-27 | 2021-01-15 | 上海市环境科学研究院 | Modularized supported bismuth vanadate photocatalytic material and preparation method and application thereof |
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Application publication date: 20120613 |