CN109847771A - A kind of bismuth tungstate-carbonitride-silver orthophosphate ternary efficient visible light catalyst and preparation method thereof - Google Patents
A kind of bismuth tungstate-carbonitride-silver orthophosphate ternary efficient visible light catalyst and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of bismuth tungstate-carbonitride-silver orthophosphate ternary efficient visible light catalysts and preparation method thereof, solve the problems, such as that bismuth tungstate photocatalysis performance is not excellent enough.This Three-element composite photocatalyst is made of Bismuth tungstate nano-sheet, azotized carbon nano piece and the nano silver stacked, Bismuth tungstate nano-sheet is 0.8-1 microns long, 0.4-0.6 microns wide, and 0.6-0.8 microns of azotized carbon nano length of a film, 0.2-0.4 microns wide, silver orthophosphate granular size is 50-100 nanometers.Hydro-thermal-precipitation method are applied to the preparation of bismuth tungstate-carbonitride-silver orthophosphate Three-element composite photocatalyst by the present invention, bismuth tungstate-nitridation carbon complex is first synthesized using hydro-thermal method, it reapplies the precipitation method silver orthophosphate is combined in bismuth tungstate-carbonitride, sediment is obtained by filtration, obtains powdered bismuth tungstate-carbonitride-phosphoric acid silver composite that visible light catalytic is had excellent performance after washing, drying.Preparation method of the present invention is simple, and operation is easy, and is conducive to the extensive use of production practices.
Description
Technical field
The present invention relates to visible light catalytic material and preparation method thereof technical field, especially a kind of bismuth tungstate-carbonitride-
Silver orthophosphate ternary efficient visible light catalyst and preparation method thereof.
Background technique
With the continuous development of human society, environmental pollution is getting worse, can effectively administer industry and life is dirty
The technical research of dye is increasingly valued by people.Photocatalysis technology have simple process, it is at low cost, not will cause secondary dirt
The advantages that dye is the emerging technology for solving a great application potential of problem of environmental pollution.Most widely used at present is TiO2
Semiconductor catalyst, but since it is only to ultraviolet light response, and quantum efficiency is low, it is difficult to meet the requirement of the depollution of environment.Therefore,
Develop the emphasis that new and effective visible light catalyst is current photocatalysis technology research.
Special layer structure, band gap be relatively narrow, visible light catalysis activity because having for bismuth tungstate with perovskite-like structure
The advantages that high and stability is good is the hot spot of current catalysis material research.But its quantum efficiency and visible light-responded range are also
It is not ideal enough.Compound hetero-junctions is a kind of effective ways for improving conductor photocatalysis performance, and it is multiple to construct bismuth tungstate base heterojunction
Light combination catalyst improves its quantum efficiency, widens optical response range, so that the photocatalysis performance for improving bismuth tungstate has become wolframic acid
The hot spot of bismuthino photochemical catalyst research.
Summary of the invention
The purpose of the present invention be intended to provide a kind of bismuth tungstate-carbonitride-silver orthophosphate ternary efficient visible light catalyst and its
Preparation method.Hydro-thermal-precipitation method are applied to bismuth tungstate-carbonitride-silver orthophosphate preparation by the present invention, pass through composite nitride carbon
Improve the visible light catalytic performance of bismuth tungstate with silver orthophosphate, preparation condition is mild, at low cost, easy to operate, period is short and
Visible light catalytic efficiency is high, is conducive to actual production.
The technical scheme is that
A kind of bismuth tungstate-carbonitride-silver orthophosphate ternary efficient visible light catalyst, it is powdered bismuth tungstate-nitridation
Carbon-phosphoric acid silver composite is made of, bismuth tungstate nanometer the Bismuth tungstate nano-sheet, azotized carbon nano piece and the nano silver that stack
It is 0.8-1 microns of length of a film, 0.4-0.6 microns wide, 0.6-0.8 microns of azotized carbon nano length of a film, 0.2-0.4 microns wide, phosphoric acid
Argent grain size is 50-100nm, is made using hydro-thermal-precipitation method.Preparation method is first to synthesize bismuth tungstate-nitridation with hydro-thermal method
Carbon complex reapplies the precipitation method and silver orthophosphate is combined in bismuth tungstate-carbonitride, sediment is obtained by filtration, sediment is washed
After washing, drying to obtain the final product.
Bismuth tungstate-carbonitride of the present invention-silver orthophosphate ternary efficient visible light catalyst preparation step is as follows:
1) prepare bismuth tungstate-nitridation carbon complex: weigh a certain amount of cetyl trimethylammonium bromide room-temperature dissolution in
In deionized water, tungstate dihydrate acid sodium is added, magnetic agitation 30 minutes, makes it dissolve, adds five water bismuth nitrates and a certain amount of
Carbonitride forms white suspension, and after continuing stirring 30 minutes, it is polytetrafluoroethylene (PTFE) that suspension, which is poured into 100 milliliters of liners,
Water heating kettle is put into baking oven, is kept the temperature 24 hours at 120 DEG C, is got a yellowish precipitate, respectively with dehydrated alcohol and deionized water from
Heart washing 3 times or more, obtain bismuth tungstate-nitridation carbon complex.
2) it prepares bismuth tungstate-carbonitride-phosphoric acid silver composite: a certain amount of polyvinylpyrrolidone is dissolved into 80%
Ethanol water in, prepared bismuth tungstate-nitridation carbon complex is added, after ultrasonic disperse 15 minutes, 0.005mol/ is added
The silver nitrate aqueous solution of L stirs 30 minutes, then instills the sodium phosphate aqueous solution of 0.004mol/L, continues stirring 50 minutes, will sink
Starch is washed 3 times or more with deionized water, dehydrated alcohol respectively, and freeze-drying obtains faint yellow bismuth tungstate-carbonitride-phosphoric acid
Silver powder.
In technical solution of the present invention, in the bismuth tungstate-nitridation carbon complex preparation step, to guarantee effectively control
The bismuth tungstate of the partial size and pattern of bismuth tungstate-carbonitride processed, the additive amount of cetyl trimethylammonium bromide and theoretical synthesis
Molar ratio is 0.137:1；To guarantee that carbonitride is effectively improved the visible light catalytic performance of bismuth tungstate, the additive amount and reason of carbonitride
Mass ratio by the bismuth tungstate of synthesis is 1:1.
In technical solution of the present invention, in the bismuth tungstate-carbonitride-phosphoric acid silver composite preparation step, to protect
Card silver orthophosphate is effectively improved the wolframic acid of bismuth tungstate-carbonitride visible light catalytic performance, silver nitrate and sodium phosphate and theoretical synthesis
The molar ratio of bismuth is respectively 5:1 and 3.7:1；For the partial size and pattern for controlling institute's compound phosphoric acid silver, polyvinylpyrrolidone and reason
Mass ratio by the silver orthophosphate of synthesis is 1.22:1.
Bismuth tungstate-carbonitride-silver phosphate visible light catalyst of the method for the present invention preparation is used to decline in visible light conditions
Solve organic pollutant.
The present invention has the advantages that
1, the present invention provides a kind of bismuth tungstate-carbonitride-silver orthophosphate ternary visible catalyst and preparation method thereof, systems
Standby product high efficiency photocatalysis degradable organic pollutant under visible light illumination.
2, the present invention prepares bismuth tungstate-carbonitride-silver orthophosphate efficient visible light catalyst using hydro-thermal-adsorption precipitation method,
Bismuth tungstate-nitridation carbon complex is first prepared using hydro-thermal method, cetyl trimethylammonium bromide is added to bismuth tungstate-carbonitride
Microstructure and partial size are controlled, then silver orthophosphate is combined in bismuth tungstate-carbonitride by adsorption precipitation method, and poly- second is added
The microstructure and partial size of alkene pyrrolidone control silver orthophosphate.
Preparation method of the invention is simple, and operation is easy, and is conducive to the extensive use of production practices.
Heretofore described room temperature means 25-35 DEG C of temperature.
Detailed description of the invention
Bismuth tungstate-carbonitride-silver phosphate photocatalyst stereoscan photograph prepared by Fig. 1, the method for the present invention.
Bismuth tungstate-carbonitride-silver phosphate photocatalyst X-ray energy spectrogram prepared by Fig. 2, the method for the present invention.
Bismuth tungstate-carbonitride-silver phosphate photocatalyst X-ray diffractogram prepared by Fig. 3, the method for the present invention.
Bismuth tungstate-carbonitride-silver phosphate photocatalyst uv-visible absorption spectra prepared by Fig. 4, the method for the present invention
Figure.
Bismuth tungstate-carbonitride-silver phosphate photocatalyst prepared by Fig. 5, the method for the present invention is catalyzed drop under visible light illumination
Solve the performance of dye, rhodamine B.
Specific embodiment
Bismuth tungstate-carbonitride of the present invention-silver orthophosphate ternary efficient visible light catalyst is using hydro-thermal-precipitation method preparation: claiming
It takes a certain amount of cetyl trimethylammonium bromide room-temperature dissolution in 80 ml deionized waters, tungstate dihydrate acid sodium, magnetic force is added
Stirring 30 minutes, makes it dissolve, adds five water bismuth nitrates and a certain amount of carbonitride, after continuing stirring 30 minutes, will obtain
Suspension pour into 100 milliliters of liners be polytetrafluoroethylene (PTFE) water heating kettle, be put into baking oven, 120 DEG C keep the temperature 24 hours, obtain
Pale yellow precipitate uses dehydrated alcohol and deionized water centrifuge washing 3 times respectively, obtains bismuth tungstate-nitridation carbon complex.Again by one
Prepared bismuth tungstate-nitrogen is added into 200 milliliter 80% of ethanol water in quantitative polyvinylpyrrolidone room-temperature dissolution
Change carbon complex, after ultrasonic disperse 15 minutes, the silver nitrate aqueous solution of 100 milliliters of 0.005mol/L is added, stirs 30 minutes, then
The sodium phosphate aqueous solution of 100 milliliters of 0.004mol/L is added, continues stirring 50 minutes, sediment is used to deionized water, nothing respectively
Water-ethanol washs 3 times, is freeze-dried 24 hours, obtains flaxen bismuth tungstate-carbonitride-phosphoric acid silver powder.
To guarantee effectively control bismuth tungstate-nitridation carbon complex partial size and pattern, cetyl trimethylammonium bromide
The molar ratio of additive amount and the bismuth tungstate of theoretical synthesis is 0.137:1.
To guarantee that carbonitride is effectively improved the visible light catalytic performance of bismuth tungstate, what the additive amount and theory of carbonitride synthesized
The mass ratio of bismuth tungstate is 1:1.
To guarantee that silver orthophosphate is effectively improved the visible light catalytic performance of bismuth tungstate, silver nitrate and sodium phosphate and theoretical synthesis
The molar ratio of bismuth tungstate is respectively 5:1 and 3.7:1.
For the partial size and pattern for controlling institute's compound phosphoric acid silver, the quality of the silver orthophosphate of polyvinylpyrrolidone and theoretical synthesis
Than for 1.22:1.
Bismuth tungstate-carbonitride-silver orthophosphate ternary photochemical catalyst for below with reference to embodiment being prepared by the method for the present invention and its
Using being described further, but the present invention is not limited only to following embodiments.
Embodiment 1
0.05 gram of cetyl trimethylammonium bromide room-temperature dissolution is weighed in 80 ml deionized waters, is added 0.33 gram two
Water sodium tungstate magnetic agitation 30 minutes, makes it dissolve, and adds 0.97 gram of five water bismuth nitrate and 0.07 gram of carbonitride, is formed white
Suspension after continuing stirring 30 minutes, is poured into the water heating kettle that 100 milliliters of liners are polytetrafluoroethylene (PTFE), is put into baking by color suspension
In case, 24 hours are kept the temperature at 120 DEG C, is got a yellowish precipitate, dehydrated alcohol and deionized water centrifuge washing 3 times is used respectively, obtains
To bismuth tungstate-nitridation carbon complex.0.85 gram of polyvinylpyrrolidone is dissolved into 200 milliliter 80% of ethanol water,
Prepared bismuth tungstate-nitridation carbon complex is added, the nitric acid of 100 milliliters of 0.005mol/L is added after ultrasonic disperse 15 minutes
Silver-colored aqueous solution stirs 30 minutes, adds the sodium phosphate aqueous solution of 100 milliliters of 0.004mol/L, continues stirring 50 minutes, will sink
Starch is washed 3 times with deionized water, dehydrated alcohol respectively, is freeze-dried 24 hours, is obtained faint yellow bismuth tungstate-carbonitride-phosphorus
Sour silver composite powder.
The stereoscan photograph of gained bismuth tungstate-carbonitride-silver orthophosphate composite powder is as shown in Figure 1.As seen from Figure 1,
Powder is made of Bismuth tungstate nano-sheet, azotized carbon nano piece and the nano silver stacked, and the long 0.8-1 of Bismuth tungstate nano-sheet is micro-
Rice, 0.4-0.6 microns wide, 0.6-0.8 microns of azotized carbon nano length of a film, 0.2-0.4 microns wide, silver orthophosphate granular size is
50-100nm.Synthesized bismuth tungstate-carbonitride-silver orthophosphate X-ray energy spectrogram such as Fig. 2.Tungsten can be determined by Fig. 2 and Fig. 1
Sour bismuth-carbonitride-phosphoric acid silver composite by stack Bismuth tungstate nano-sheet (Fig. 2 a, b), azotized carbon nano piece (Fig. 2 c, d) and
Nano silver (Fig. 2 e, f) composition.Fig. 3 is synthesized bismuth tungstate-carbonitride-silver orthophosphate X-ray diffractogram.It can by Fig. 3
Know, the X-ray diffraction peak of bismuth tungstate and silver orthophosphate in bismuth tungstate-carbonitride-silver orthophosphate respectively with standard card JCPDS39-
0256 and JCPDS06-0505 is corresponding.Individual carbonitride X-ray diffraction peak is not detected in sample, the reason is that carbonitride
Crystallinity it is not high, and its main characteristic peak be located at 27.4 °, be overlapped with the diffraction maximum of (131) crystal face of bismuth tungstate.
Bismuth tungstate-carbonitride-phosphoric acid silver composite UV-visible absorption spectrum such as Fig. 4, ABSORPTION EDGE exist
Near 620nm, in visible light region, (400-500nm) has strong absorption.
Embodiment 2
Bismuth tungstate-carbonitride made from the method for the present invention-silver orthophosphate ternary visible catalyst catalytic performance evaluation
Degradation of dye sieve under visible light of bismuth tungstate-carbonitride-silver phosphate visible light catalyst made from the method for the present invention
Red bright B, the dosage of catalyst are 0.05 gram, and the concentration of rhodamine B is 0.01 grams per liter, and volume is 50 milliliters, and light source uses
500W tungsten halogen lamp guarantees that incident light is visible light (420nm≤λ≤800nm) using optical filter, with UV-3600 type ultraviolet-visible
The absorbance change of rhodamine B in spectrophotometer measurement degradation process samples 5 milliliters, after being centrifuged at a high speed in every 3 minutes,
Supernatant liquor is taken to measure.Fig. 5 is bismuth tungstate-carbonitride-silver phosphate photocatalyst of the method for the present invention preparation in visible light
Under the conditions of catalytic degradation dye, rhodamine B curve, as seen from the figure in bismuth tungstate-carbonitride-silver phosphate catalyst work
It, can degradable rhodamine B after 9 minutes under.
Claims (4)
1. a kind of bismuth tungstate-carbonitride-silver orthophosphate ternary efficient visible light catalyst, it is characterised in that: it is powdered wolframic acid
Bismuth-carbonitride-silver orthophosphate is made of, bismuth tungstate nanometer the Bismuth tungstate nano-sheet, azotized carbon nano piece and the nano silver that stack
It is 0.8-1 microns of length of a film, 0.4-0.6 microns wide, 0.6-0.8 microns of azotized carbon nano length of a film, 0.2-0.4 microns wide, phosphoric acid
Argent grain size is 50-100nm.
2. a kind of preparation side of bismuth tungstate-carbonitride as described in claim 1-silver orthophosphate ternary efficient visible light catalyst
Method, it is characterised in that: preparation step is as follows:
1) bismuth tungstate-nitridation carbon complex preparation: a certain amount of cetyl trimethylammonium bromide room-temperature dissolution is weighed in going
In ionized water, tungstate dihydrate acid sodium is added, magnetic agitation 30 minutes, makes it dissolve, adds five water bismuth nitrates and a certain amount of nitrogen
Change carbon, form white suspension, after continuing stirring 30 minutes, suspension is poured into the water that 100 milliliters of liners are polytetrafluoroethylene (PTFE)
Hot kettle, is put into baking oven, keeps the temperature 24 hours at 120 DEG C, gets a yellowish precipitate, washed respectively with dehydrated alcohol and deionized water
3 times or more, obtain bismuth tungstate-nitridation carbon complex；
2) a certain amount of polyvinylpyrrolidone bismuth tungstate-carbonitride-phosphoric acid silver composite preparation: is dissolved into ethanol water
In solution, then bismuth tungstate-nitridation carbon complex is added in this solution, after stirring 30 minutes, 0.005mol/L nitric acid is added
Silver-colored aqueous solution stirs 30 minutes, then instills 0.004mol/L sodium phosphate aqueous solution, continues stirring 50 minutes, sediment is distinguished
It is washed 3 times or more with deionized water, dehydrated alcohol, is freeze-dried, obtains faint yellow bismuth tungstate-carbonitride-phosphoric acid silver powder.
3. the preparation method of bismuth tungstate-carbonitride-silver orthophosphate efficient visible light catalyst according to claim 2, special
Sign is: in the bismuth tungstate-carbonitride preparation step, to guarantee effectively control bismuth tungstate-carbonitride partial size and pattern,
The molar ratio of the additive amount of cetyl trimethylammonium bromide and the bismuth tungstate of theoretical synthesis is 0.137:1；To guarantee carbonitride
It is effectively improved the visible light catalytic performance of bismuth tungstate, the mass ratio of the bismuth tungstate of the additive amount and theory synthesis of carbonitride is 1:1.
4. the preparation method of bismuth tungstate-carbonitride-silver orthophosphate efficient visible light catalyst according to claim 2, special
Sign is: in the bismuth tungstate-carbonitride-silver orthophosphate preparation step, to guarantee that silver orthophosphate is effectively improved bismuth tungstate-carbonitride
Visible light catalytic performance, the molar ratio of the bismuth tungstate of silver nitrate and sodium phosphate and theoretical synthesis is respectively 5:1 and 3.7:1；For
The partial size and pattern of silver orthophosphate are controlled, the mass ratio for the silver orthophosphate that polyvinylpyrrolidone and theory synthesize is 1.22:1.
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