CN109261193A - Ultrasound-solvent structure Bi2O2CO3/g-C3N4The method and its application of flower-shaped composite photo-catalyst - Google Patents
Ultrasound-solvent structure Bi2O2CO3/g-C3N4The method and its application of flower-shaped composite photo-catalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002904 solvent Substances 0.000 title claims abstract description 25
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 28
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 16
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 15
- 239000010935 stainless steel Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract 3
- 239000000843 powder Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 7
- 238000006731 degradation reaction Methods 0.000 claims description 7
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 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 claims description 5
- 229940043267 rhodamine b Drugs 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 10
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 5
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 239000010808 liquid waste Substances 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 238000012876 topography Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 19
- 238000012360 testing method Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- 238000002336 sorption--desorption measurement Methods 0.000 description 6
- 238000005286 illumination Methods 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000000622 irritating effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- 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
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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Abstract
The invention discloses ultrasound-solvent structure Bi2O2CO3/g‑C3N4The method and its application of flower-shaped composite photo-catalyst.Bismuth nitrate is dissolved in the in the mixed solvent of ethylene glycol and deionized water, forms the precursor solution of bismuthyl carbonate；Again by g-C3N4It is added in the precursor solution of bismuthyl carbonate, ultrasound, obtained suspension is transferred in polytetrafluoroethylene (PTFE) stainless steel cauldron, is placed in baking oven, solvent thermal reaction, cooled to room temperature rinse gained precipitating deionized water and dehydrated alcohol respectively, centrifuge separation obtains Bi in drying in drying box2O2CO3/g‑C3N4.Synthetic method of the present invention is simple, at low cost, environmental-friendly, the volatilization of the whole nonirritant gas of experiment, the liquid waste processing after simplifying the safeguard procedures and experiment in experimentation.The sample topography of synthesis is intact, of uniform size, and average diameter is about 5 μm, which is expected to be widely applied in photocatalysis field.
Description
Technical field
The invention belongs to inorganic-organic hybrid technical field of micro nano material preparation more particularly to a kind of use ultrasound-are molten
Agent thermal method synthesizes Bi2O2CO3/g-C3N4" green " preparation method of flower-shaped composite photo-catalyst.
Background technique
Photocatalysis technology can be increasingly subject to widely pay close attention to effective solution energy and environmental problem.Bi2O2CO3/g-
C3N4The preparation of flower-shaped composite photo-catalyst is to carry out to two kinds of catalysis materials compound, increases the specific surface area of catalyst, two
Hetero-junctions is formed between the interface that person is in close contact, enhances the transmitting of electronics, and then inhibits the compound of electronics and hole, it can be effective
The catalytic efficiency of ground enhancing photochemical catalyst.
Currently, Bi is prepared2O2CO3/g-C3N4There are many technology of composite photocatalyst, but none does not use the stimulation such as strong acid and strong base
Sex pill, experimentation inevitably generate volatilization irritative gas, and experimental situation is not safe enough.
Summary of the invention
The object of the present invention is to provide a kind of ultrasound-solvent structure Bi2O2CO3/g-C3N4Flower-shaped composite photo-catalyst
" green " preparation method, this method simple process, whole process avoids the use of irritation medicine and reagent, improves experimentation
Safety index, simplify the processing of experimental waste liquid, and the sample prepared is of uniform size, it is reproducible, there is research well
Prospect.
The technical solution adopted by the present invention is that: ultrasound-solvent structure Bi2O2CO3/g-C3N4Flower-shaped composite photo-catalyst
Method, include the following steps:
1) melamine is placed in Muffle furnace, low-temperature bake obtains g-C3N4Powder；
2) under stirring at normal temperature, five water bismuth nitrates is dissolved in the in the mixed solvent of ethylene glycol and deionized water, are continued stirring until
Form clear solution；
3) by g-C obtained by step 1)3N4Powder is added in the resulting clear solution of step 2), and 1~2h of ultrasound is mixed
Close uniform suspension；
4) suspension obtained by step 3) is transferred in polytetrafluoroethylene (PTFE) stainless steel cauldron, it is natural after solvent thermal reaction
It is cooling, obtained solid object is washed, centrifugation and it is dry after, obtain Bi2O2CO3/g-C3N4Flower-shaped composite photo-catalyst.
Further, above-mentioned ultrasound-solvent structure Bi2O2CO3/g-C3N4The method of flower-shaped composite photo-catalyst,
In step 1), the low-temperature bake is that 4~5h is roasted at 550 DEG C.
Further, above-mentioned ultrasound-solvent structure Bi2O2CO3/g-C3N4The method of flower-shaped composite photo-catalyst,
In step 2), the mixed solvent, by volume, ethylene glycol: deionized water=4:1.
Further, above-mentioned ultrasound-solvent structure Bi2O2CO3/g-C3N4The method of flower-shaped composite photo-catalyst,
The Bi2O2CO3/g-C3N4In flower-shaped composite photo-catalyst, in mass ratio, g-C3N4:Bi2O2CO3=1:1~1:3.
Further, above-mentioned ultrasound-solvent structure Bi2O2CO3/g-C3N4The method of flower-shaped composite photo-catalyst,
In step 4), the solvent thermal reaction is solvent thermal reaction 12-13h at 180 DEG C.
The Bi synthesized according to above-mentioned method2O2CO3/g-C3N4Flower-shaped composite photo-catalyst is degraded rhodamine under visible light
Application in B.Method is as follows: in the Bi according to above-mentioned method synthesis2O2CO3/g-C3N4In flower-shaped composite photo-catalyst, it is added
Rhodamine B, it is seen that catalytic degradation under light (λ >=400nm).
The beneficial effects of the present invention are:
1, method whole process of the invention avoids the use of irritation medicine and reagent, the volatilization of nonirritant gas, technique
Simply, at low cost, it environmental-friendly, the problem of simplifying liquid waste processing after the safeguard procedures and experiment in experimentation, improves
The safety index of experiment.
2, the Bi of method of the invention preparation2O2CO3/g-C3N4Flower-shaped composite photocatalyst sample pattern is intact, and size is equal
Even, flower-like structure partial size is about 5 μm.
3, the Bi of method of the invention preparation2O2CO3/g-C3N4The large specific surface area of three-dimensional flower-shaped composite photo-catalyst is
Pure Bi2O2CO34.19 times.
4, method and process of the invention is simple, reproducible, has a good application prospect.
Detailed description of the invention
Fig. 1 is the phase structure using XRD test sample.
Fig. 2 is the microscopic appearance using SEM test specimens sample；
Wherein, a: pure g-C3N4；B: pure Bi2O2CO3；c:Bi2O2CO3/g-C3N4-2；d:Bi2O2CO3/g-C3N4-2。
Fig. 3 is the sample adsorption-desorption isothermal curve tested using nitrogen adsorption-desorption.
Fig. 4 is Bi2O2CO3/g-C3N4- 2 flower-shaped composite catalysts are degraded the RhB of 10mg/L at visible light (λ >=400nm)
UV-visible absorption spectrum.
Fig. 5 is the Bi in different embodiments2O2CO3/g-C3N4Flower-shaped composite photo-catalyst shines at visible light (λ >=400nm)
Lower 80min is penetrated to the degradation effect of RhB.
Specific embodiment
The present invention is described further with reference to the accompanying drawings and embodiments, these embodiments can only be used to illustrate this hair
It is bright, but do not limit the scope of the invention.
The pure g-C of embodiment 13N4Preparation
(1) the preparation method is as follows:
It measures 6g melamine to be added in crucible, in Muffle furnace, is warming up to 550 DEG C with the heating rate of 5 DEG C/min, roasting
4h is burnt to get the pale yellow powder g-C with armorphous nano particle is arrived3N4。
(2) test result
(a) is pure g-C in Fig. 13N4The XRD of sample is detected.As seen from Figure 1, in 13.1 ° and 27.4 ° appearance, two diffraction
Peak corresponds respectively to g-C3N4(100) crystal face and (002) crystal face.
(a) is pure g-C in Fig. 23N4The SEM of sample is detected.From Figure 2 it can be seen that pure g-C3N4It is accumulated in typical stratiform
Structure.
As seen from Figure 3, pure g-C3N4Sample carries out nitrogen adsorption desorption and pore-size distribution test, the pure g- of preparation
C3N4Specific surface area be 15.232m2g-1。
The pure Bi of embodiment 22O2CO3Preparation
(1) the preparation method is as follows:
The in the mixed solvent that five water bismuth nitrate of 0.485g is dissolved in 24ml ethylene glycol and 6ml deionized water is formed is weighed, often
After temperature stirs to clarify, precursor solution is obtained；Precursor solution is transferred to 100ml polytetrafluoroethylene (PTFE) stainless steel cauldron
In, and polytetrafluoroethylene (PTFE) stainless steel cauldron is placed in solvent thermal reaction 12h in 180 DEG C of baking ovens.To the end of reacting, by poly- four
Vinyl fluoride stainless steel cauldron cooled to room temperature, outwells supernatant and obtains sediment.Taking precipitate is in centrifuge tube, through going
After ionized water and each centrifuge washing of dehydrated alcohol 3 times, dry 12h, obtains pure Bi at 80 DEG C2O2CO3Sample.
(2) test result
(b) is pure Bi in Fig. 12O2CO3The XRD of sample is detected.As seen from Figure 1, pure Bi2O2CO3The diffraction maximum of sample
With Bi2O2CO3Standard card (PDF#25-1464) it is completely the same.
(b) is pure Bi in Fig. 22O2CO3The SEM of sample detects figure.From Figure 2 it can be seen that pure Bi2O2CO3Sample is shown as
Class flower-like structure, by loosely assembling with a thickness of tens nanometers of regular nanometer sheet.
As seen from Figure 3, pure Bi2O2CO3Sample carry out nitrogen adsorption desorption and pore-size distribution test, preparation it is pure
Bi2O2CO3Specific surface area be 8.039m2g-1。
3 Bi of embodiment2O2CO3/g-C3N4The preparation of -1 flower-shaped composite photo-catalyst
(1) the preparation method is as follows:
1. 6g melamine is put into 50ml corundum crucible, in Muffle furnace, it is warming up to the heating rate of 5 DEG C/min
550 DEG C, 4h is roasted to get the pale yellow powder g-C with armorphous nano particle is arrived3N4。
2. the in the mixed solvent that five water bismuth nitrate of 0.485g is dissolved in 24ml ethylene glycol and 6ml deionized water is formed is weighed,
Stirring at normal temperature obtains the precursor solution of bismuthyl carbonate to after clarifying.
3. the g-C that 0.25g step 1 is prepared3N4Nano powder is added to the resulting bismuthyl carbonate precursor solution of step 2
In, ultrasonic 1h obtains uniformly mixed suspension.
4. step 3 gained suspension is transferred in 100ml polytetrafluoroethylene (PTFE) stainless steel cauldron, and by polytetrafluoroethylene (PTFE)
Stainless steel cauldron is placed in 180 DEG C of baking ovens, solvent thermal reaction 12h.To the end of reacting, by polytetrafluoroethylene (PTFE) stainless steel reaction
Kettle cooled to room temperature outwells supernatant and obtains sediment, and taking precipitate is each through deionized water and dehydrated alcohol in centrifuge tube
After centrifuge washing 3 times, dry 12h, is obtained in mass ratio, g-C at 80 DEG C3N4:Bi2O2CO3The flower-shaped composite photocatalyst of=1:1
Agent is denoted as Bi2O2CO3/g-C3N4-1。
(2) test result
(c) is Bi in Fig. 12O2CO3/g-C3N4The XRD of -1 flower-shaped composite photo-catalyst is detected.As seen from Figure 1, Bi2O2CO3/
g-C3N4The diffraction maximum of -1 flower-shaped composite photo-catalyst both contains Bi2O2CO3Whole characteristic peaks, and contain g-C3N4Spy
Levy peak.
4 Bi of embodiment2O2CO3/g-C3N4The preparation of -2 flower-shaped composite photo-catalysts
(1) the preparation method is as follows:
1. 6g melamine is put into 50ml corundum crucible, in Muffle furnace, it is warming up to the heating rate of 5 DEG C/min
550 DEG C, 4h is roasted to get the pale yellow powder g-C with armorphous nano particle is arrived3N4。
2. the in the mixed solvent that five water bismuth nitrate of 0.485g is dissolved in 24ml ethylene glycol and 6ml deionized water is formed is weighed,
Stirring at normal temperature obtains the precursor solution of bismuthyl carbonate to after clarifying.
3. the g-C that 0.5g step 1 is prepared3N4Nano powder is added to the resulting bismuthyl carbonate precursor solution of step 2
In, ultrasonic 1h obtains uniformly mixed suspension.
4. step 3 gained suspension is transferred in 100ml polytetrafluoroethylene (PTFE) stainless steel cauldron, and by polytetrafluoroethylene (PTFE)
Stainless steel cauldron is placed in 180 DEG C of baking ovens, solvent thermal reaction 12h.To the end of reacting, by polytetrafluoroethylene (PTFE) stainless steel reaction
Kettle cooled to room temperature outwells supernatant and obtains sediment, and taking precipitate is each through deionized water and dehydrated alcohol in centrifuge tube
After centrifuge washing 3 times, dry 12h, is obtained in mass ratio, g-C at 80 DEG C3N4:Bi2O2CO3The flower-shaped composite photocatalyst of=1:2
Agent is denoted as Bi2O2CO3/g-C3N4-2。
(2) test result
(d) is Bi in Fig. 12O2CO3/g-C3N4The XRD of -2 flower-shaped composite photo-catalysts is detected.As seen from Figure 1, Bi2O2CO3/
g-C3N4The diffraction maximum of -2 flower-shaped composite photo-catalysts both contains Bi2O2CO3Whole characteristic peaks, and contain g-C3N4Spy
Levy peak.
(c) and (d) is Bi in Fig. 22O2CO3/g-C3N4The SEM of -2 flower-shaped composite photo-catalysts is detected.From Figure 2 it can be seen that
Bi2O2CO3/g-C3N4- 2 flower-shaped composite photo-catalysts show as three-dimensional flower-shaped structure.
As seen from Figure 3, Bi2O2CO3/g-C3N4- 2 flower-shaped composite photo-catalysts carry out nitrogen adsorption desorption and pore-size distribution is surveyed
Examination, the Bi of preparation2O2CO3/g-C3N4The specific surface area of -2 flower-shaped composite photo-catalysts is 33.688m2g-1。
5 Bi of embodiment2O2CO3/g-C3N4The preparation of -3 flower-shaped composite photo-catalysts
(1) the preparation method is as follows:
1. 6g melamine is put into 50ml corundum crucible, in Muffle furnace, it is warming up to the heating rate of 5 DEG C/min
550 DEG C, 4h is roasted to get the pale yellow powder g-C with armorphous nano particle is arrived3N4。
2. the in the mixed solvent that five water bismuth nitrate of 0.485g is dissolved in 24ml ethylene glycol and 6ml deionized water is formed is weighed,
Stirring at normal temperature obtains the precursor solution of bismuthyl carbonate to after clarifying.
3. the g-C that 0.75g step 1 is prepared3N4Nano powder is added to the resulting bismuthyl carbonate precursor solution of step 2
In, ultrasonic 1h obtains uniformly mixed suspension.
4. step 3 gained suspension is transferred in 100ml polytetrafluoroethylene (PTFE) stainless steel cauldron, and by polytetrafluoroethylene (PTFE)
Stainless steel cauldron is placed in 180 DEG C of baking ovens, solvent thermal reaction 12h.To the end of reacting, by polytetrafluoroethylene (PTFE) stainless steel reaction
Kettle cooled to room temperature outwells supernatant and obtains sediment, and taking precipitate is each through deionized water and dehydrated alcohol in centrifuge tube
After centrifuge washing 3 times, dry 12h, is obtained in mass ratio, g-C at 80 DEG C3N4:Bi2O2CO3The flower-shaped composite photocatalyst of=1:3
Agent is denoted as Bi2O2CO3/g-C3N4-3。
(2) test result
(e) is Bi in Fig. 12O2CO3/g-C3N4The XRD of -3 flower-shaped composite photo-catalysts is detected.As seen from Figure 1, Bi2O2CO3/
g-C3N4The diffraction maximum of -3 flower-shaped composite photo-catalysts both contains Bi2O2CO3Whole characteristic peaks, and contain g-C3N4Spy
Levy peak.
6 Bi of embodiment2O2CO3/g-C3N4The application of flower-shaped composite photo-catalyst
Bi prepared by embodiment 42O2CO3/g-C3N4- 2 flower-shaped composite photo-catalysts carry out the survey of photocatalyst material performance
Examination.
Method is as follows: with 300w xenon lamp (λ >=400nm) for light source, by 0.05g catalyst Bi2O2CO3/g-C3N4- 2 are added
Into 100ml beaker, then be added 50ml concentration be 10mg/L dye solution rhodamine B, by before catalyst system illumination black
30min is stirred under dark situation, catalyst and dyestuff is made to reach adsorption-desorption balance；It adjusts light intensity center and is just irradiated to catalytic body
It is surface, samples 3ml every 20min after illumination, after being centrifuged 5min with 8000rpm, supernatant liquor uv-3600 is taken to measure solution
Middle residual dye concentration, the catalytic performance of sample is evaluated according to the absorbance of solution.
As a result as shown in figure 4, under visible light illumination, RhB solution is located at the absorption intensity of the characteristic absorption peak at 550nm
It gradually moves to left, reduce with the passage of irradiation time, this illustrates that the molecular structure of RhB is destroyed, so as to cause the decline of its absorbance.
After illumination 60min, substantially without apparent peak in absorption spectrum.Bi2O2CO3/g-C3N4- 2 samples can reach the degradation rate of RhB
To 98%.It can be seen that Bi2O2CO3/g-C3N4- 2 samples have good visible light catalytic performance.
Fig. 5 shows that sample prepared by embodiment 1-5, can by Fig. 5 under visible light illumination to the degradation effect of RhB
See, with the increase of light application time, RhB gradually degrades, Bi2O2CO3/g-C3N4- 2 catalytic degradation efficiency highest.
Claims (7)
1. ultrasound-solvent structure Bi2O2CO3/g-C3N4The method of flower-shaped composite photo-catalyst, which is characterized in that including such as
Lower step:
1) melamine is placed in Muffle furnace, low-temperature bake obtains g-C3N4Powder；
2) under stirring at normal temperature, five water bismuth nitrates is dissolved in the in the mixed solvent of ethylene glycol and deionized water, continue stirring until to be formed
Clear solution；
3) by g-C obtained by step 1)3N4Powder is added in the resulting clear solution of step 2), 1~2h of ultrasound, and it is equal to obtain mixing
Even suspension；
4) suspension obtained by step 3) is transferred in polytetrafluoroethylene (PTFE) stainless steel cauldron, after solvent thermal reaction, natural cooling,
Obtained solid object is washed, centrifugation and it is dry after, obtain Bi2O2CO3/g-C3N4Flower-shaped composite photo-catalyst.
2. ultrasound according to claim 1-solvent structure Bi2O2CO3/g-C3N4The side of flower-shaped composite photo-catalyst
Method, which is characterized in that in step 1), the low-temperature bake is that 4~5h is roasted at 550 DEG C.
3. ultrasound according to claim 1-solvent structure Bi2O2CO3/g-C3N4The side of flower-shaped composite photo-catalyst
Method, which is characterized in that in step 2), the mixed solvent, by volume, ethylene glycol: deionized water=4:1.
4. ultrasound according to claim 1-solvent structure Bi2O2CO3/g-C3N4The side of flower-shaped composite photo-catalyst
Method, which is characterized in that the Bi2O2CO3/g-C3N4In flower-shaped composite photo-catalyst, in mass ratio, g-C3N4:Bi2O2CO3=
1:1~1:3.
5. ultrasound according to claim 1-solvent structure Bi2O2CO3/g-C3N4The side of flower-shaped composite photo-catalyst
Method, which is characterized in that in step 4), the solvent thermal reaction is solvent thermal reaction 12-13h at 180 DEG C.
6. according to the Bi of the described in any item method synthesis of claim 1-52O2CO3/g-C3N4Flower-shaped composite photo-catalyst is can
Application in light-exposed lower rhodamine B degradation.
7. application according to claim 6, which is characterized in that method is as follows: according to described in claim any one of 1-5
Method synthesis Bi2O2CO3/g-C3N4In flower-shaped composite photo-catalyst, rhodamine B is added, it is seen that catalytic degradation under light.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110102328A (en) * | 2019-04-30 | 2019-08-09 | 北华大学 | Cryogenic fluid phase technology prepares flower pattern carbon quantum dot/nitridation carbon quantum dot/super oxygen waltherite Three-element composite photocatalyst |
| CN110575841A (en) * | 2019-09-11 | 2019-12-17 | 哈尔滨理工大学 | Novel photocatalyst material for degrading methylene blue light and preparation method thereof |
| CN111054413A (en) * | 2020-03-05 | 2020-04-24 | 南京师范大学 | Ternary composite multi-effect photocatalyst and preparation method thereof |
| CN112642458A (en) * | 2020-12-23 | 2021-04-13 | 陕西科技大学 | Heterojunction photocatalyst and preparation method and application thereof |
| CN113600215A (en) * | 2021-08-16 | 2021-11-05 | 常州大学 | Porous ball of flowers Ni5P4Capture of g-C3N4Preparation method and application of QDs composite photocatalyst |
| CN113713844A (en) * | 2021-09-29 | 2021-11-30 | 陕西科技大学 | Ag/g-C3N4/Bi2O2CO3Heterojunction photocatalyst and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1591421A1 (en) * | 2004-04-29 | 2005-11-02 | Consorzio Interuniversitario per lo Sviluppo dei Sistemi a Grande Interfase, C.S.G.I | Process for preparing nano- and micro-sized particles of inorganic compounds using a water-structure modifier |
| CN105126888A (en) * | 2015-10-09 | 2015-12-09 | 重庆文理学院 | Gold-supported bismuth subcarbonate material for photocatalysis and preparation method |
| CN106984360A (en) * | 2017-04-06 | 2017-07-28 | 江苏大学 | Bi2O2CO3/PPy/g‑C3N4Composite photo-catalyst and its preparation method and application |
-
2018
- 2018-11-09 CN CN201811331383.5A patent/CN109261193B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1591421A1 (en) * | 2004-04-29 | 2005-11-02 | Consorzio Interuniversitario per lo Sviluppo dei Sistemi a Grande Interfase, C.S.G.I | Process for preparing nano- and micro-sized particles of inorganic compounds using a water-structure modifier |
| CN105126888A (en) * | 2015-10-09 | 2015-12-09 | 重庆文理学院 | Gold-supported bismuth subcarbonate material for photocatalysis and preparation method |
| CN106984360A (en) * | 2017-04-06 | 2017-07-28 | 江苏大学 | Bi2O2CO3/PPy/g‑C3N4Composite photo-catalyst and its preparation method and application |
Non-Patent Citations (3)
| Title |
|---|
| LIN MA ETAL.: "Facile Template-free Synthesis of Bi2O2CO3 Flower-like Architectures in Ethylene Glycol Water System", 《CHEM. LETT.》 * |
| QIAN ZHANG ETAL.: "Synthesis and properties of visible light responsive g-C3N4/Bi2O2CO3 layered heterojunction nanocomposites", 《RSC ADVANCES》 * |
| ZHENYU WANG ETAL.: "Fabrication of Bi2O2CO3/g-C3N4 Heterojunctions for Efficiently Photocatalytic NO in Air Removal: In-Situ Self-Sacrificial Synthesis, Characterizations and Mechanistic Study", 《 APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
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| CN110102328B (en) * | 2019-04-30 | 2022-08-30 | 北华大学 | Flower-type carbon quantum dot/carbon nitride quantum dot/bismuth superoxide carbonate ternary composite photocatalyst prepared by low-temperature solution phase technology |
| CN110575841A (en) * | 2019-09-11 | 2019-12-17 | 哈尔滨理工大学 | Novel photocatalyst material for degrading methylene blue light and preparation method thereof |
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