CN112226849B - Composite photocatalyst fiber containing cerium dioxide/bismuth tungstate and preparation method thereof - Google Patents
Composite photocatalyst fiber containing cerium dioxide/bismuth tungstate and preparation method thereof Download PDFInfo
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- CN112226849B CN112226849B CN202010986661.1A CN202010986661A CN112226849B CN 112226849 B CN112226849 B CN 112226849B CN 202010986661 A CN202010986661 A CN 202010986661A CN 112226849 B CN112226849 B CN 112226849B
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- bismuth tungstate
- cerium dioxide
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- polyvinyl alcohol
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 93
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 90
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 83
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 83
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 81
- 239000000835 fiber Substances 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 35
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 30
- 239000002243 precursor Substances 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000009987 spinning Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000001877 deodorizing effect Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000002147 killing effect Effects 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a ceria/bismuth tungstate-containing composite photocatalyst fiber, wherein a ceria/bismuth tungstate photocatalyst presents a two-dimensional lamellar structure, ceria nano-particles are dispersed on the surface of bismuth tungstate, and one part of the ceria/bismuth tungstate photocatalyst is embedded into the fiber and the other part of the ceria/bismuth tungstate photocatalyst is exposed outside. The invention also discloses a preparation method of the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, and provides the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate as well as the preparation method and the application thereof.
Description
Technical Field
The invention belongs to the field of textile engineering, and relates to a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, and a preparation method of the composite photocatalyst fiber.
Background
In order to quickly and effectively treat pollutants such as oil stain and oil stain on the surface of clothes, the photocatalyst fiber is favored by researchers. The application of the photocatalyst in textile is a novel deodorizing and antibacterial fabric developed by utilizing a nano photocatalyst deodorizing agent in a fiber test field in Shigao county of Japan for the first time. At present, research in this regard has also begun domestically. The application technology of the nano photocatalyst on the textile has the advantages of simple process, low cost, no secondary pollution, no toxicity, no irritation, good heat resistance and the like, can oxidize and decompose harmful organic matters and partial inorganic matters with stable structures at normal temperature and normal pressure, and has wide application prospect.
After the nano photocatalyst and the fibers are finished, the nano photocatalyst has the characteristics of small size, large specific surface area, different surface bond state from the inside of the particles, incomplete surface atom coordination and the like, so that the active sites on the surface are increased, uneven atom steps are formed, and a large reaction contact surface is provided. In addition, due to the photocatalytic property of the surface photocatalyst, if the photocatalyst is a visible photocatalyst, when sunlight irradiates the surface of the photocatalyst textile, the photocatalyst on the surface can be excited to generate photo-generated electron-hole pairs, electrons are transferred to the surface and are contacted with air and water on the surface to generate a series of hydroxyl radicals and superoxide radicals with oxidizability, and most of organic pollutants and part of inorganic substances can be degraded. The invention aims to provide a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, a preparation method and application thereof.
Disclosure of Invention
The first purpose of the invention is to provide a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, which has the characteristics of water and oil resistance, ultraviolet shielding and static resistance.
The invention also aims to provide a preparation method of the cerium dioxide/bismuth tungstate-containing composite photocatalyst fiber, which has the characteristics of degrading organic pollutants, inhibiting and killing bacteria and purifying air.
The first technical scheme adopted by the invention is that the cerium dioxide/bismuth tungstate-containing composite photocatalyst fiber is characterized in that a cerium dioxide/bismuth tungstate photocatalyst presents a two-dimensional lamellar structure, cerium dioxide nano particles are dispersed on the surface of bismuth tungstate, one part of the cerium dioxide/bismuth tungstate photocatalyst is embedded into the fiber, and the other part of the cerium dioxide/bismuth tungstate photocatalyst is exposed outside.
The invention adopts another technical scheme that a preparation method of the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate is used for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, and is implemented according to the following steps:
step 1, sequentially adding Na into deionized water 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Uniformly stirring to obtain a mixed solution, transferring the mixed solution into a reaction kettle, and heating for reaction;
step 2, after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a product from the reaction kettle, centrifuging the product, washing the product with deionized water until the washing liquid is neutral, and drying the product to obtain the cerium dioxide/bismuth tungstate photocatalyst;
step 3, weighing polyvinyl alcohol, dissolving the polyvinyl alcohol into deionized water, stirring at constant temperature to prepare polyvinyl alcohol sol, weighing cerium dioxide/bismuth tungstate photocatalyst and citric acid, adding the cerium dioxide/bismuth tungstate photocatalyst and the citric acid into absolute ethyl alcohol, stirring uniformly to obtain mixed liquid, adding the mixed liquid into the polyvinyl alcohol sol, and stirring uniformly to obtain precursor sol;
step 4, putting the precursor sol into an injector, connecting a high-voltage positive electrode with a nozzle and connecting a negative electrode with a receiver, and electrifying to spin;
and 5, drying the collected precursor fiber, then putting the precursor fiber into a muffle furnace for heat preservation, finally preserving the heat at different temperatures in a tubular furnace filled with nitrogen and hydrogen, and taking out the precursor fiber to obtain the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate.
The invention is also characterized in that:
na in the mixed solution in the step 1 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 In a molar ratio of 0.05 to 0.5:0.5 to 5:0.001 to 0.01.
The reaction temperature in the step 1 is 150-180 ℃, and the reaction time is 12-96 h.
The drying temperature of the step 2 is 50-80 ℃, and the drying time is 5-20 h.
The ratio of polyvinyl alcohol to deionized water in the polyvinyl alcohol sol in the step 3 is 1-100 g: 5-500 mL, and the stirring temperature is 70-90 ℃.
The mass ratio of the cerium dioxide/bismuth tungstate photocatalyst in the step 3 to the citric acid is 0.1-10: 0.005-0.5, the volume ratio of the polyvinyl alcohol solution to the mixed solution is 5-500: 1-100, the mixing time of the mixed solution is 0.5-4 h, and the mixing time of the precursor sol is 0.5-2 h.
Step 4, spinning parameters: the included angle between the injector nozzle and the horizontal plane is 15-25 degrees, and the distance between the injector nozzle and the receiver is 15-25 cm; the applied direct current voltage is 15-25 kV; the relative humidity is 45-55%; the indoor temperature is 15-25 ℃; the feeding rate is 3-5 mL/h.
The drying temperature in the step 5 is 50-80 ℃, and the drying time is 5-8 h; the muffle furnace is kept at 540-560 ℃ for 1-5 h; the heat preservation time of the tubular furnace is 2 to 6 hours, and the heating rate is 1 to 4 ℃/min.
The invention has the beneficial effects that:
1. the cerium dioxide/bismuth tungstate-containing composite photocatalyst fiber prepared by the invention has functional performance, especially self-cleaning function.
2. The cerium dioxide/bismuth tungstate-containing composite photocatalyst fiber prepared by the invention can be used for water and oil repellency, ultraviolet shielding and static resistance, and can also be used for degrading organic pollutants, inhibiting and killing bacteria, purifying air and the like.
Drawings
FIG. 1 is a scanning electron microscope image of example 1 of a composite photocatalyst fiber containing cerium oxide/bismuth tungstate according to the present invention;
FIG. 2 is an X-ray diffraction pattern of a composite photocatalyst fiber of example 1 containing cerium oxide/bismuth tungstate according to the present invention;
FIG. 3 is an evaluation graph of rhodamine B photocatalytic degradation in example 1 of the ceria/bismuth tungstate-containing composite photocatalyst fiber of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
The invention relates to a cerium dioxide/bismuth tungstate-containing composite photocatalyst fiber, wherein a cerium dioxide/bismuth tungstate photocatalyst presents a two-dimensional lamellar structure, cerium dioxide nano particles are dispersed on the surface of bismuth tungstate, and one part of the cerium dioxide/bismuth tungstate photocatalyst is embedded in the fiber and the other part of the cerium dioxide/bismuth tungstate photocatalyst is exposed outside.
The invention relates to a preparation method of a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, which is used for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate and is implemented according to the following steps:
step 1, sequentially adding Na into deionized water 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Uniformly stirring to obtain a mixed solution, transferring the mixed solution into a reaction kettle, and heating for reaction;
step 2, after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a product from the reaction kettle, centrifuging the product, washing the product with deionized water until the washing liquid is neutral, and drying the product to obtain the cerium dioxide/bismuth tungstate photocatalyst;
step 3, weighing polyvinyl alcohol, dissolving the polyvinyl alcohol into deionized water, stirring at constant temperature to prepare polyvinyl alcohol sol, weighing cerium dioxide/bismuth tungstate photocatalyst and citric acid, adding the cerium dioxide/bismuth tungstate photocatalyst and the citric acid into absolute ethyl alcohol, uniformly stirring to obtain mixed liquid, adding the mixed liquid into the polyvinyl alcohol sol, and uniformly stirring to obtain precursor sol;
step 4, putting the precursor sol into an injector, connecting a high-voltage positive electrode with a nozzle and connecting a negative electrode with a receiver, and electrifying to spin;
and 5, drying the collected precursor fiber, then putting the precursor fiber into a muffle furnace for heat preservation, finally preserving the heat at different temperatures in a tubular furnace filled with nitrogen and hydrogen, and taking out the precursor fiber to obtain the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate.
Na in the mixed solution in the step 1 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Is 0.05:0.5:0.001.
the reaction temperature in the step 1 is 150 ℃, and the reaction time is 12h.
The drying temperature of the step 2 is 50 ℃, and the drying time is 5h.
The ratio of polyvinyl alcohol to deionized water in the polyvinyl alcohol sol obtained in the step 3 is 1g:5mL, stirring temperature 70 ℃.
The mass ratio of the cerium dioxide/bismuth tungstate photocatalyst in the step 3 to the citric acid is 0.1:0.005, the volume ratio of the polyvinyl alcohol solution to the mixed solution is 5:1, the stirring time of the mixed solution is 0.5h, and the stirring time of the precursor sol is 0.5h.
Step 4, spinning parameters: the included angle between the injector nozzle and the horizontal plane is 15 degrees, and the distance between the injector nozzle and the receiver is 15cm; the applied direct voltage is 15kV; the relative humidity is 45%; the indoor temperature is 15 ℃; the feed rate was 3mL/h.
The drying temperature in the step 5 is 50 ℃, and the drying time is 5 hours; the muffle furnace is kept at 540 ℃ for 1h; the heat preservation time of the tube furnace is 2h, and the heating rate is 1 ℃/min.
As can be seen from fig. 1: the prepared cerium dioxide/bismuth tungstate composite photocatalyst presents a two-dimensional sheet structure.
As can be seen in fig. 2: the prepared photocatalyst is cerium dioxide/bismuth tungstate.
As can be seen in fig. 3: in all prepared materials, the prepared cerium dioxide/bismuth tungstate composite photocatalyst has the highest photocatalytic performance.
Example 2
The invention relates to a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate.
The invention relates to a preparation method of a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, which is used for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate and is implemented according to the following steps:
step 1, sequentially adding Na into deionized water 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Uniformly stirring to obtain a mixed solution, moving the mixed solution into a reaction kettle, and heating for reaction;
step 2, after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a product from the reaction kettle, centrifuging the product, washing the product with deionized water until the washing liquid is neutral, and drying the product to obtain the cerium dioxide/bismuth tungstate photocatalyst;
step 3, weighing polyvinyl alcohol, dissolving the polyvinyl alcohol into deionized water, stirring at constant temperature to prepare polyvinyl alcohol sol, weighing cerium dioxide/bismuth tungstate photocatalyst and citric acid, adding the cerium dioxide/bismuth tungstate photocatalyst and the citric acid into absolute ethyl alcohol, uniformly stirring to obtain mixed liquid, adding the mixed liquid into the polyvinyl alcohol sol, and uniformly stirring to obtain precursor sol;
step 4, putting the precursor sol into an injector, connecting a high-voltage positive electrode with a nozzle and connecting a negative electrode with a receiver, and electrifying to spin;
and 5, drying the collected precursor fiber, then putting the precursor fiber into a muffle furnace for heat preservation, finally preserving the heat at different temperatures in a tubular furnace filled with nitrogen and hydrogen, and taking out the precursor fiber to obtain the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate.
Na in the mixed solution in the step 1 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Is 0.5:5:0.01.
the reaction temperature in the step 1 is 180 ℃, and the reaction time is 96h.
The drying temperature of the step 2 is 80 ℃, and the drying time is 20h.
The ratio of polyvinyl alcohol to deionized water in the polyvinyl alcohol sol obtained in the step 3 is 100g:500mL, stirring temperature 90 ℃.
The mass ratio of the cerium dioxide/bismuth tungstate photocatalyst in the step 3 to the citric acid is 10:0.5, the volume ratio of the polyvinyl alcohol solution to the mixed solution is 500:100, stirring the mixed solution for 4 hours, and stirring the precursor sol for 2 hours.
Step 4, spinning parameters: the included angle between the injector nozzle and the horizontal plane is 25 degrees, and the distance between the injector nozzle and the receiver is 25cm; the applied direct voltage is 25kV; relative humidity of 55%; the indoor temperature is 25 ℃; the feed rate was 5mL/h.
The drying temperature in the step 5 is 80 ℃, and the drying time is 8 hours; the muffle furnace is kept at 560 ℃ for 1-5 h; the heat preservation time of the tube furnace is 6h, and the heating rate is 4 ℃/min.
Example 3
The invention relates to a cerium dioxide/bismuth tungstate-containing composite photocatalyst fiber, wherein a cerium dioxide/bismuth tungstate photocatalyst presents a two-dimensional lamellar structure, cerium dioxide nano particles are dispersed on the surface of bismuth tungstate, and one part of the cerium dioxide/bismuth tungstate photocatalyst is embedded in the fiber and the other part of the cerium dioxide/bismuth tungstate photocatalyst is exposed outside.
The invention relates to a preparation method of a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, which is used for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate and is implemented according to the following steps:
step 1, sequentially adding Na into deionized water 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Uniformly stirring to obtain a mixed solution, transferring the mixed solution into a reaction kettle, and heating for reaction;
step 2, after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a product from the reaction kettle, centrifuging the product, washing the product with deionized water until the washing liquid is neutral, and drying the product to obtain the cerium dioxide/bismuth tungstate photocatalyst;
step 3, weighing polyvinyl alcohol, dissolving the polyvinyl alcohol into deionized water, stirring at constant temperature to prepare polyvinyl alcohol sol, weighing cerium dioxide/bismuth tungstate photocatalyst and citric acid, adding the cerium dioxide/bismuth tungstate photocatalyst and the citric acid into absolute ethyl alcohol, stirring uniformly to obtain mixed liquid, adding the mixed liquid into the polyvinyl alcohol sol, and stirring uniformly to obtain precursor sol;
step 4, putting the precursor sol into an injector, connecting a high-voltage positive electrode with a nozzle and connecting a negative electrode with a receiver, and electrifying to spin;
and 5, drying the collected precursor fiber, then putting the precursor fiber into a muffle furnace for heat preservation, finally preserving the heat at different temperatures in a tubular furnace filled with nitrogen and hydrogen, and taking out the precursor fiber to obtain the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate.
Na in the mixed solution in the step 1 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 In a molar ratio of 0.3:2:0.008.
the reaction temperature in the step 1 is 160 ℃, and the reaction time is 45h.
The drying temperature of the step 2 is 70 ℃, and the drying time is 12h.
The ratio of polyvinyl alcohol to deionized water in the polyvinyl alcohol sol obtained in the step 3 is 30g:150mL, stirring temperature 80 ℃.
The mass ratio of the cerium dioxide/bismuth tungstate photocatalyst in the step 3 to the citric acid is 6:0.4, the volume ratio of the polyvinyl alcohol solution to the mixed solution is 230:60, stirring the mixed solution for 2.5h, and stirring the precursor sol for 1h.
Step 4, spinning parameters: the included angle between the injector nozzle and the horizontal plane is 18 degrees, and the distance between the injector nozzle and the receiver is 22cm; the applied direct voltage is 23kV; relative humidity is 48%; the indoor temperature is 24 ℃; the feed rate was 4mL/h.
The drying temperature in the step 5 is 70 ℃, and the drying time is 7 hours; the muffle furnace is kept at the temperature of 555 ℃ for 3.4h; the heat preservation time of the tube furnace is 4.2h, and the heating rate is 3 ℃/min.
Claims (8)
1. A composite photocatalyst fiber containing cerium dioxide/bismuth tungstate is characterized in that a cerium dioxide/bismuth tungstate photocatalyst presents a two-dimensional lamellar structure, cerium dioxide nanoparticles are dispersed on the surface of the bismuth tungstate, one part of the cerium dioxide/bismuth tungstate photocatalyst is embedded into the fiber, and the other part of the cerium dioxide/bismuth tungstate photocatalyst is exposed outside.
2. A preparation method of a composite photocatalyst fiber containing cerium dioxide/bismuth tungstate, which is used for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate as claimed in claim 1, and is characterized by comprising the following steps:
step 1, sequentially adding Na into deionized water 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 Uniformly stirring to obtain a mixed solution, transferring the mixed solution into a reaction kettle, and heating for reaction;
step 2, after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a product from the reaction kettle, centrifuging the product, washing the product with deionized water until the washing liquid is neutral, and drying the product to obtain the cerium dioxide/bismuth tungstate photocatalyst;
step 3, weighing polyvinyl alcohol, dissolving the polyvinyl alcohol into deionized water, stirring at constant temperature to prepare polyvinyl alcohol sol, weighing the cerium dioxide/bismuth tungstate photocatalyst and citric acid, adding the cerium dioxide/bismuth tungstate photocatalyst and the citric acid into absolute ethyl alcohol, uniformly stirring to obtain mixed liquid, adding the mixed liquid into the polyvinyl alcohol sol, and uniformly stirring to obtain precursor sol;
step 4, putting the precursor sol into an injector, connecting a high-voltage positive electrode with a nozzle and connecting a negative electrode with a receiver, and electrifying to spin;
step 5, drying the collected precursor fibers, then putting the dried precursor fibers into a muffle furnace for heat preservation, and finally, preserving the heat at different temperatures in a tubular furnace filled with nitrogen and hydrogen, and taking out the precursor fibers to obtain the composite photocatalyst fibers containing cerium dioxide/bismuth tungstate;
the mass ratio of the cerium dioxide/bismuth tungstate photocatalyst in the step 3 to the citric acid is 0.1-10: 0.005-0.5, the volume ratio of the polyvinyl alcohol sol to the mixed solution is 5-500: 1 to 100, the mixing time of the mixed solution is 0.5 to 4 hours, and the mixing time of the precursor sol is 0.5 to 2 hours.
3. The method for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate according to claim 2, wherein Na is contained in the mixed solution in the step 1 2 WO 4 ·2H 2 O、Bi(NO 3 ) 3 ·5H 2 O and CeO 2 In a molar ratio of 0.05 to 0.5:0.5 to 5:0.001～0.01。
4. The method for preparing the ceria/bismuth tungstate-containing composite photocatalyst fiber as claimed in claim 3, wherein the reaction temperature in the step 1 is 150-150 ℃ and the reaction time is 12-96 hours.
5. The method for preparing the ceria/bismuth tungstate-containing composite photocatalyst fiber as claimed in claim 4, wherein the drying temperature in the step 2 is 50-50 ℃ and the drying time is 5-20 hours.
6. The method for preparing the ceria/bismuth tungstate-containing composite photocatalyst fiber as claimed in claim 5, wherein the ratio of polyvinyl alcohol to deionized water in the polyvinyl alcohol sol of step 3 is 1-100 g: 5-500 mL, and the stirring temperature is 70-90 ℃.
7. The method for preparing the composite photocatalyst fiber containing cerium dioxide/bismuth tungstate as claimed in claim 6, wherein the spinning parameters in step 4 are as follows: the included angle between the injector nozzle and the horizontal plane is 15-25 degrees, and the distance between the injector nozzle and the receiver is 15-25 cm; the applied direct current voltage is 15-25 kV; the relative humidity is 45-55%; the indoor temperature is 15-25 ℃; the feeding rate is 3-5 mL/h.
8. The method for preparing the ceria/bismuth tungstate-containing composite photocatalyst fiber as claimed in claim 7, wherein the drying temperature in the step 5 is 50-50 ℃, and the drying time is 5-5 hours; the muffle furnace is kept at 540-560 ℃ for 1-5 h; the heat preservation time of the tubular furnace is 2 to 6 hours, and the heating rate is 1 to 4 ℃/min.
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| CN103451773A (en) * | 2012-05-28 | 2013-12-18 | 清华大学 | Bismuth ferrite nano fiber material and preparation method thereof |
| CN107376899A (en) * | 2017-07-19 | 2017-11-24 | 河南师范大学 | The method that one step hydro thermal method synthesizes different-shape bismuth tungstate two dimension catalysis material |
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