CN109569731A - A kind of MIL-100 (Fe)/BiOI composite photo-catalyst and its application - Google Patents
A kind of MIL-100 (Fe)/BiOI composite photo-catalyst and its application Download PDFInfo
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- 239000013291 MIL-100 Substances 0.000 title claims abstract description 109
- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 73
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 239000010842 industrial wastewater Substances 0.000 claims abstract description 4
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 51
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Substances [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 229910001868 water Inorganic materials 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims description 10
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims description 10
- 239000008236 heating water Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 238000007146 photocatalysis Methods 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 description 18
- 230000000694 effects Effects 0.000 description 18
- 229910002651 NO3 Inorganic materials 0.000 description 16
- 230000015556 catabolic process Effects 0.000 description 14
- 238000006731 degradation reaction Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 238000002835 absorbance Methods 0.000 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 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- -1 BiOI Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- OQSFCNZFDJKFEY-UHFFFAOYSA-N O([BiH2])[BiH2] Chemical compound O([BiH2])[BiH2] OQSFCNZFDJKFEY-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N bismuth(III) nitrate Inorganic materials [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 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 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
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- 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
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
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- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/842—Iron
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The present invention relates to a kind of MIL-100 (Fe)/BiOI composite photo-catalyst and its applications, belong to photochemical catalyst field.Creatively MIL-100 (Fe)/BiOI composite photo-catalyst is prepared by bismuth oxyiodide and MIL-l00 (Fe) are compound in the present invention, by by Bi (NO3)3·5H2The nitric acid solution of O is added drop-wise to MIL-100 (Fe)-KI mixed liquor and is prepared, preparation-obtained composite photo-catalyst has photocatalysis efficiency high, the advantages of recycling high-efficient, long service life, is highly suitable for being applied in Industrial Wastewater Treatment.
Description
Technical field
The present invention relates to a kind of MIL-100 (Fe)/BiOI composite photo-catalyst and its applications, belong to photochemical catalyst field.
Background technique
Water environment pollution is increasingly becoming the major influence factors for restricting sustainable economic development, how to solve these and hinders people
The problem of class social sustainable development, becomes the difficulty and challenge of countries in the world scientist institute facing.Photocatalysis technology is made
For a kind of novel environment-friendly water treatment technology, new pollutant will not be generated in entire reaction process.Due to its low energy consumption and
Easy to operate, photocatalysis has attracted the concern of many researchers all over the world.In terms of using solar energy, photoelectric conversion is always
It is a very active research field.Photocatalysis technology has many advantages, so the technology is very popular at present, it is excellent
Point mainly has the following: first is that inexhaustible solar energy can be used as light source in photocatalysis technology, utilizing light source activation
Photochemical catalyst.Second is that suitable photochemical catalyst generally all has, cheap, stability is high, without poisoning and can be recycled
The advantages of.Third is that the substance that the Some Organic Pollutants contained in water can be completely degraded not pollute, such as CO2 ,
H2O etc., the inorganic pollution in water are oxidated or reduced into no substance for polluting and being safe from harm.Fourth is that photocatalysis technology operates
Getting up, very simple, the very easy control of operating condition, oxidability is relatively strong and does not have secondary pollution.Currently, domestic
The application study of outer photocatalysis technology is largely embodied in organic wastewater, dyeing and printing sewage, agricultural chemicals waste water, surfactant
In the destruction of oily wastewater.
The greatest problem that photochemical catalyst is faced in practical application at present is that nano-photocatalyst is easy to reunite, two-phase point
It is highly difficult from recycling.In recent years, it is seen that optical response semiconductor has higher than conventional photochemical catalyst in visible light region
Photocatalysis performance, cause the close attention of researcher.Although bismuth-based oxide photochemical catalyst has very strong visible light
Responding ability, but its own Carrier recombination rate is high, photochemical reaction activity is low, limits its photocatalytic applications, this has become
The critical issue that the visible-light photocatalysis materials such as bismuth-based oxide urgently solve at present.Therefore, researcher constantly modifies them
To reach expected result.In response to these disadvantages, researchers are striving to find the method for reasonable to bismuthino
Oxide is modified, it is expected that improving the photocatalytic activity and quantum efficiency of its visible light.
Chinese invention patent ZL201310057514.6 discloses a kind of preparation method of annular shape BiOI microballoon, is related to light
Catalyst.It is by Bi (NO3)3It is dissolved in alcohol and obtains solution A, KI is mixed with oleic acid, obtains solution B；By solution A with it is molten
Liquid B mixing, is poured into autoclave after stirring, after hydro-thermal reaction, is washed, and filtering is dried micro- to get annular shape BiOI russet
Ball.Using bismuth nitrate and KI as raw material, in alcohol and oleic acid mixed liquor, with low-temperature hydrothermal one-step method, it is prepared for circular BiOI
Microballoon.Its photocatalytic activity significantly improves, operation is simple, is prepared and prepares high catalytic activity with application potential
The method of BiOI, but to recycle efficiency poor for the BiOI microballoon that is prepared of this method.
Chinese invention patent application 201610044518.4 discloses one kind using thiocarbamide, chromium acetate and bismuth oxyiodide as raw material
The method for preparing the compound heterogeneous section composite photo-catalyst of CdS/BiOI.Thiocarbamide is added in bismuth oxyiodide dispersion afterwards in deionized water
And cadmium acetate, hydro-thermal reaction is carried out after being uniformly mixed, and then obtain CdS/BiOI heterojunction composite photocatalyst, wherein
CdS and be 0.5-2.0:1 with the molar ratio of BiOI.Prepared nano composite photo-catalyst has excellent visible light catalytic living
Property, the sample degradation rhodamine B activity that the molar ratio of especially CdS and BiOI are 1.0 is best, it is seen that light reaction is dropped after one hour
Solution rate reaches 90%, and the degrading activity than pure BiOI and CdS will be high, but the CdS/BiOI catalytic efficiency being prepared and follows
Ring utilization efficiency is unstable.
Based on this, the present invention is specifically proposed.
Summary of the invention
The present invention provides a kind of MIL-100 (Fe)/BiOI composite photo-catalyst, and the catalyst is by bismuth oxyiodide and MIL-
L00 (Fe) is compound to be prepared, by by Bi (NO3)3·5H2The nitric acid solution of O is added drop-wise to MIL-100 (Fe)-KI mixed liquor
It is prepared, preparation-obtained composite photo-catalyst has the advantages of photocatalysis efficiency is high, long service life, is highly suitable for
It is applied in Industrial Wastewater Treatment.
The present invention is achieved through the following technical solutions above-mentioned technical effect:
A kind of composite photo-catalyst, by bismuth oxyiodide and MIL-l00 (Fe) is compound is prepared.
The preparation method of the composite photo-catalyst specifically include the following steps:
1) preparation of MIL-100 (Fe) material: by trimesic acid and FeCl3·6H2O is dissolved in distilled water, thereto plus
Enter hydrofluoric acid and HNO3After stir and evenly mix, mixed liquor is transferred in reaction kettle, control reaction temperature be 150 DEG C of successive reactions
12h makes to be washed with distilled water after centrifugation, and MIL-100 (Fe) can be obtained in vacuum drying；
2) it prepares MIL-100 (Fe)-KI mixed liquor: weighing MIL-100 (Fe) and potassium iodide is separately added into deionized water, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；
3) preparation of bismuth oxyiodide: by appropriate Bi (NO3)3·5H2O is dissolved in the HNO that pH is 2.03In solution, it is added dropwise
Into MIL-100 (Fe)-KI mixed liquor, the pH to 3 of mixed solution is adjusted using ammonium hydroxide, heating water bath is stirred to react to 85 DEG C
For 24 hours, it is washed after centrifugation using ethyl alcohol and deionized water, MIL-100 (Fe)/BiOI composite photocatalyst can be obtained in vacuum drying
Agent.
The preparation method of composite photo-catalyst described above, the potassium iodide and Bi (NO3)3•5H2The mass ratio of the material of O
For 1:1.
The preparation method of composite photo-catalyst described above, the vacuum drying item of MIL-100 (Fe) in the step 1)
Part is 150 DEG C of vacuum drying 12h, and MIL-100 (Fe)/BiOI composite photo-catalyst vacuum drying condition is in the step 3)
Dry 12h under 40 DEG C of vacuum.
The preparation method of composite photo-catalyst described above, in the MIL-100 (Fe)/BiOI composite photo-catalyst
Every mole of BiOI and 25-87.5g MIL-100 (Fe) carries out compound obtain.Preferably, the MIL-100 (Fe)/BiOI is multiple
Every mole of BiOI and 75g MIL-100 (Fe) carries out compound obtain in light combination catalyst.
The preparation method of composite photo-catalyst described above, specifically comprises the following steps:
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing 20,30,40,60,70mg MIL-100 (Fe) and 0.8 mmol is added separately to going for 30mL
In ionized water, it is vigorously stirred and obtains evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to
In MIL-100 (Fe)-KI mixed liquor, using the pH value of ammonium hydroxide adjustment solution to pH=3, by mixed liquor heating water bath to 85 DEG C,
It continuously stirs for 24 hours；The isolated product of magnetic agitation, after ethyl alcohol and 3 deionized waters of the product by 3 times wash, 40
Dry 12h, can be obtained MIL-100 (Fe)/BiOI composite photo-catalyst of different ratio under DEG C vacuum.
The step 1) specifically include the following steps: weigh 0.8456g trimesic acid and 1.6253g respectively
FeCl3·6H2O is dissolved in 30mL distilled water, and 0.214mL hydrofluoric acid and 0.165 mLHNO is then added3, will after stirring and evenly mixing
Mixed solution is transferred in reaction kettle, 150 DEG C, successive reaction 12h is heated to, to after reaction, pass through centrifugal separation method
The prepared orange colour product of recycling, with distillation water washing 3 times of heat, last 150 DEG C of vacuum drying 12h.
A kind of application of above-mentioned composite photo-catalyst is also claimed in the present invention, and the specially composite photo-catalyst exists
Application in Industrial Wastewater Treatment.It is used to can be used as photochemical catalyst use, 7 table of the embodiment of the present invention when catalysis industry waste water
Bright, under the action of visible light, degradation effect is there has also been being obviously improved, by surveying the discovery of its absorbance, different ratio
The catalytic efficiency of BiOI/MIL-100 (Fe) composite photocatalyst material has a long way to go, and is found by ultraviolet test in bismuth oxyiodide
In manufacturing process, the degradation effect that the composite photocatalyst material of 30mg MIL-100 (Fe) is added is best.With MIL-100 (Fe)
The parabola trend of reduction after first increase is presented in the catalytic of the increase composite photo-catalyst of content, and 30mg MIL-100 is added
(Fe) degradation effect of composite photocatalyst material is best.No matter its degradation effect has significant poor compared with bismuth oxyiodide
Not.The embodiment of the present invention 8 shows to urge photochemical dose to reuse five times for BiOI/MIL-100 (Fe) is compound, finally found that and urge
The utilization rate of agent drops to 90% from 100%, and every recycling is primary, catalytic efficiency decline 2%.It can be seen that the complex light
Catalyst chemical property is stablized, and cyclic utilization rate is high, which is that bismuth oxyiodide exclusive use is not available, therefore it is significant
Better than bismuth oxyiodide photochemical catalyst.
BiOI/MIL-100 (Fe) composite photocatalyst material of the present invention makes the service life and catalytic efficiency of composite material
It greatly improves, has a good application prospect, there is following technical advantage outstanding compared with prior art:
1) a certain amount of MIL-100 (Fe) material can be enhanced bismuth oxyiodide and catch to optical molecule in photoreactivation catalyst of the present invention
The effect of catching greatly improves it to the absorption of visible light, to improve its photocatalysis performance and photocatalysis efficiency.
2) composite photo-catalyst of the present invention greatly increases the degradation efficiency of pollutant.MIL-100 (Fe) material is added
BiOI/MIL-100 (Fe) composite photo-catalyst is compared with the BiOI photochemical catalyst of pure phase, and not only catalytic efficiency greatly increases, right
The degradation time of pollutant shortens, and degradation rate is accelerated.
3) cyclic utilization rate of composite photo-catalyst of the present invention is high, long service life.Pass through the cycle analysis to catalyst
As can be seen that the catalytic performance for recycling five times BiOI/MIL-100 (Fe) composite photocatalyst material is still fine, and urge
Change efficiency and is up to 90%.This feature has very important status in chemical field.
Detailed description of the invention
Fig. 1 is pure phase MIL-100 (Fe), BiOI and MIL-100 (Fe)/BiOI composite photocatalyst material XRD spectrum.
Fig. 2 is pure phase BiOI, pure phase MIL-100 (Fe) and MIL-100 (Fe)/BiOI composite photocatalyst material SEM
Scheme with TEM.
Fig. 3 is that pure phase BiOI, pure phase MIL-100 (Fe) and MIL-100 (Fe)/BiOI composite photocatalyst material are ultraviolet
Diffusing reflection map.
Fig. 4 is that BiOI/MIL-100 (Fe) composite photocatalyst for degrading made of different quality MIL-100 (Fe) will be added
The change curve of the absorbance of rhodamine B solution.
Fig. 5 is that BiOI/MIL-100 (Fe) composite photocatalyst material five times circulations made of 30mgMIL-100 (Fe) are added
Utilize front and back catalytic efficiency.
Specific embodiment
The present invention is further described below by way of specific embodiment, but those skilled in the art should be able to know, the implementation
Example does not limit the range of the invention patent protection in any way.
Embodiment 1
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing the MIL-100 (Fe) and 0.8 mmol of 20mg is added separately in the deionized water of 30mL, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to MIL-100 (Fe)-KI
In mixed liquor, continuously stirred for 24 hours to pH=3 by mixed liquor heating water bath to 85 DEG C using the pH value of ammonium hydroxide adjustment solution；Magnetic
The product that power is sirred and separated, it is dry under 40 DEG C of vacuum after ethyl alcohol and 3 deionized waters of the product by 3 times wash
MIL-100 (Fe)/BiOI composite photo-catalyst can be obtained in 12h.
Embodiment 2
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing the MIL-100 (Fe) and 0.8 mmol of 30mg is added separately in the deionized water of 30mL, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to MIL-100 (Fe)-KI
In mixed liquor, continuously stirred for 24 hours to pH=3 by mixed liquor heating water bath to 85 DEG C using the pH value of ammonium hydroxide adjustment solution；Magnetic
The product that power is sirred and separated, it is dry under 40 DEG C of vacuum after ethyl alcohol and 3 deionized waters of the product by 3 times wash
MIL-100 (Fe)/BiOI composite photo-catalyst can be obtained in 12h.
Embodiment 3
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing the MIL-100 (Fe) and 0.8 mmol of 40mg is added separately in the deionized water of 30mL, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to MIL-100 (Fe)-KI
In mixed liquor, continuously stirred for 24 hours to pH=3 by mixed liquor heating water bath to 85 DEG C using the pH value of ammonium hydroxide adjustment solution；Magnetic
The product that power is sirred and separated, it is dry under 40 DEG C of vacuum after ethyl alcohol and 3 deionized waters of the product by 3 times wash
MIL-100 (Fe)/BiOI composite photo-catalyst can be obtained in 12h.
Embodiment 4
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing the MIL-100 (Fe) and 0.8 mmol of 60mg is added separately in the deionized water of 30mL, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to MIL-100 (Fe)-KI
In mixed liquor, continuously stirred for 24 hours to pH=3 by mixed liquor heating water bath to 85 DEG C using the pH value of ammonium hydroxide adjustment solution；Magnetic
The product that power is sirred and separated, it is dry under 40 DEG C of vacuum after ethyl alcohol and 3 deionized waters of the product by 3 times wash
MIL-100 (Fe)/BiOI composite photo-catalyst can be obtained in 12h.
Embodiment 5
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing the MIL-100 (Fe) and 0.8 mmol of 70mg is added separately in the deionized water of 30mL, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to MIL-100 (Fe)-KI
In mixed liquor, continuously stirred for 24 hours to pH=3 by mixed liquor heating water bath to 85 DEG C using the pH value of ammonium hydroxide adjustment solution；Magnetic
The product that power is sirred and separated, it is dry under 40 DEG C of vacuum after ethyl alcohol and 3 deionized waters of the product by 3 times wash
MIL-100 (Fe)/BiOI composite photo-catalyst can be obtained in 12h.
The bismuth oxyiodide that Comparative Examples 1 are prepared according to following technique
Firstly, nitric acid solution is added in deionized water and is stirred continuously to obtain the HNO that pH is 2.03Solution.Then, in electricity
Precise 0.388g (0.8mmol) Bi (NO on sub- balance3)3·5H2O is dissolved in the HNO of pH=2.0 100mL3In solution, obtain
Bi(NO3)3Solution[5].Secondly, on an electronic balance (0.8mmol) KI solid of precise 0.0528g be added to 30mL go from
In sub- water, stirred evenly with glass bar.Then, by the prepared Bi (NO in front3)3Solution is added dropwise in KI solution.Then
Ammonium hydroxide is added into the mixed solution, adjusts the pH value of solution to pH=3, subsequent heating water bath continuously stirs for 24 hours to 85 DEG C.
Pass through the isolated product of centrifuge, the then ethyl alcohol Jing Guo 3 times and 3 deionized water washings, after washing, at 40 DEG C
Dry 12h, finally obtains the BiOI photochemical catalyst of pure phase under vacuum.
MIL-100 (Fe) material that Comparative Examples 2 are prepared according to following technique
0.8456g trimesic acid and 1.6253g FeCl are weighed respectively3·6H2O is dissolved in 30mL distilled water, is then added
0.214mL hydrofluoric acid and 0.165 mLHNO3, stirring makes it after evenly mixing, and the solution mixed is transferred to the stainless of 50mL
In steel reaction kettle, 150 DEG C are heated to, 12h is then reacted, to after reaction, prepared by centrifugal separation method recycling
Orange colour product, with heat distillation water washing 3 times, last 150 DEG C of vacuum drying 12h.
The physico-chemical property map of the composite photo-catalyst of the present invention of embodiment 6 characterizes
6.1 XRD spectrums characterization
XRD characterization is mainly used for the phase and composition of research institute's synthetic material, can obtain to prepare through detection and implement according to reference
It pure phase BiOI that example 1 is prepared, the MIL-100 (Fe) being prepared according to Comparative Examples 2 and is prepared according to embodiment 2
Obtained MIL-100 (Fe)/BiOI composite photo-catalyst XRD spectrum, map are as shown in Figure 1.We can from figure
Out, there is apparent diffraction maximum in the map of both materials of pure phase BiOI and MIL-100 (Fe), and MIL-100 (Fe)/
The XRD spectrum of BiOI mixing composite material has the diffraction maximum of MIL-100 (Fe), BiOI, MIL-100 (Fe) and BiOI two simultaneously
Kind photochemical catalyst has good plyability, and MIL-100 (Fe)/BiOI composite photo-catalyst has been prepared.
6.2 scanning electron microscope maps
MIL-100 (Fe), BiOI, MIL-100 (Fe)/BiOI pattern are observed by scanning electron microscope, observation result is such as
Shown in lower Fig. 2, from the figure we can see that, pure phase BiOI present sheet, partially have itself reunite scene, degree of scatter compared with
Difference；Pure phase MIL-100 (Fe) present it is blocky, from MIL-100 (Fe)/BiOI composite photocatalyst material SEM shape appearance figure we
As can be seen that BiOI is attached in the duct of MIL-100 (Fe) material in composite photo-catalyst, pure phase MIL-100 is compared
(Fe), the partial size of BiOI composite material and size also opposite reduction, but relative to bismuth oxyiodide, its specific surface area is greatly increased.
6.3 uv drs
It is characterized by optical property of the uv drs to prepared sample, performance is as shown in Figure 3.It can be seen by Fig. 3
BiOI is weaker to light absorpting ability more than 400nm wavelength out, and absorption of the MIL-100 (Fe) to light more than 400nm wavelength
Ability is compared relatively strong with BiOI.By compound that MIL-100 (Fe), BiOI progress is compound, from the graph, it is apparent that
MIL-100 (Fe)/BiOI composite photo-catalyst enhances light absorpting ability more than 400nm wavelength.This may be because of MIL-
100 (Fe) itself are relatively strong to light absorpting ability more than 400nm wavelength and BiOI it is compound after, BiOI is distributed in MIL-
In the internal gutter of 100 (Fe), make it that reunion of itself to be less likely to occur, so that light-exposed surface area increases, catalyst is to light
The capturing ability of molecule is enhanced.Subsequent studied is still needed to about its reason.
The measurement of the catalytic capability of the composite photo-catalyst of the present invention of embodiment 7
The photocatalysis performance of sample is by under visible light, by being simulated using certain density rhodamine B solution is prepared
What waste water was studied.This experimental selection configuration concentration isRhodamine B solution, after preparing solution, weigh
Each 0.1g of MIL-100 (Fe)/BiOI catalysis material and pure phase BiOI of good different ratio prepared above adds it respectively
Enter in six quartz ampoules, the rhodamine B solution that 50ml is prepared then is added into quartz ampoule and places it in photochemical reactor
Among, first under dark condition 30min is handled, so that catalyst is suspended in the solution of rhodamine B using the method for being passed through air
Among, 4-5mL is sampled after dark processing, surveys its absorbance, has a look the effect of dark treatment degradation.Then light source is opened, this
Experiment uses the xenon lamp of 500W for the light source of visible light, and timing samples after turning on light, and centrifugation surveys its absorbance, every very
Clock takes a sample.The sample interval of the experiment is respectively 10min, 20min, 30min, 40min, 50min, 60min, is amounted to
6 samples.
Above-mentioned sample photocatalysis is carried out using the preparation-obtained photochemical catalyst of embodiment 1-5, Comparative Examples 1-2 respectively
Performance test, Fig. 4 are that BiOI/MIL-100 (Fe) composite photocatalyst for degrading sieve made of different quality MIL-100 (Fe) is added
The change curve of the absorbance of red bright B solution.
At dark processing 30 minutes, composite material played certain effect to the degradation of rhodamine B as seen from Figure 4
Fruit, when opening xenon lamp, under the action of visible light, degradation effect is there has also been being obviously improved, by surveying the discovery of its absorbance,
The catalytic efficiency of BiOI/MIL-100 (Fe) composite photocatalyst material of different ratio has a long way to go, and is existed by ultraviolet test discovery
In the manufacturing process of bismuth oxyiodide, the degradation effect that the composite photocatalyst material of 30mg MIL-100 (Fe) is added is best.With
The parabola trend of reduction after first increase is presented in the catalytic of the increase composite photo-catalyst of MIL-100 (Fe) content, is added
The degradation effect of the composite photocatalyst material of 30mg MIL-100 (Fe) is best.No matter its degradation effect has compared with bismuth oxyiodide
There is marked difference.
Actual effect is shown before and after catalyst is added, and as time increases, different quality MIL-100 (Fe) is added
MIL-100 (Fe)/BiOI composite photocatalyst material catalytic effect shows biggish difference, can from actual effect figure
Out, be added 30mgMIL-100 (Fe) made of composite photocatalyst material degradation effect it is best, this also with result phase one above
It causes.
The circulation catalytic performance of the composite photo-catalyst of the present invention of embodiment 8
Fig. 5 is that BiOI/MIL-100 (Fe) made of 30mgMIL-100 (Fe) is added to recycle for composite photocatalyst material five times
Front and back catalytic efficiency.Clearly as can be seen that the catalytic performance of the catalyst is not because of the repetition benefit of catalyst from figure
It is deteriorated with the increase of number.This experiment urges photochemical dose to reuse five times for BiOI/MIL-100 (Fe) is compound, final to send out
The utilization rate of existing catalyst drops to 90% from 100%, and every recycling is primary, catalytic efficiency decline 2%.It can be seen that this is multiple
Light combination catalyst chemical property is stablized, and cyclic utilization rate is high, and it is not available which is that bismuth oxyiodide is used alone, therefore its
It is significantly better than bismuth oxyiodide photochemical catalyst.
Claims (9)
1. a kind of composite photo-catalyst, by bismuth oxyiodide and MIL-l00 (Fe) is compound is prepared.
2. composite photo-catalyst according to claim 1, which is characterized in that preparation method specifically comprises the following steps:
1) preparation of MIL-100 (Fe) material: by trimesic acid and FeCl3·6H2O is dissolved in distilled water, is added thereto
Hydrofluoric acid and HNO3After stir and evenly mix, mixed liquor is transferred in reaction kettle, control reaction temperature be 150 DEG C of successive reaction 12h,
Make to be washed with distilled water after centrifugation, MIL-100 (Fe) can be obtained in vacuum drying；
2) it prepares MIL-100 (Fe)-KI mixed liquor: weighing MIL-100 (Fe) and potassium iodide is separately added into deionized water, acutely
Stirring to obtain evenly dispersed MIL-100 (Fe)-KI mixed liquor；
3) preparation of bismuth oxyiodide: by appropriate Bi (NO3)3·5H2O is dissolved in the HNO that pH is 2.03In solution, it is added dropwise to
In MIL-100 (Fe)-KI mixed liquor, the pH to 3 of mixed solution is adjusted using ammonium hydroxide, heating water bath is stirred to react for 24 hours to 85 DEG C,
It is washed after centrifugation using ethyl alcohol and deionized water, MIL-100 (Fe)/BiOI composite photo-catalyst can be obtained in vacuum drying.
3. composite photo-catalyst according to claim 2, which is characterized in that the potassium iodide and Bi (NO3)3•5H2The object of O
The amount ratio of matter is 1:1.
4. composite photo-catalyst according to claim 2, which is characterized in that MIL-100's (Fe) is true in the step 1)
Empty drying condition is 150 DEG C of vacuum drying 12h, and MIL-100 (Fe)/BiOI composite photo-catalyst vacuum is dry in the step 3)
Dry condition is dry 12h under 40 DEG C of vacuum.
5. composite photo-catalyst according to claim 2, which is characterized in that MIL-100 (the Fe)/BiOI is compound
Every mole of BiOI and 25-87.5g MIL-100 (Fe) carries out compound obtain in photochemical catalyst.
6. composite photo-catalyst according to claim 2, which is characterized in that MIL-100 (the Fe)/BiOI complex light
Every mole of BiOI and 75g MIL-100 (Fe) carries out compound obtain in catalyst.
7. composite photo-catalyst according to claim 5, which is characterized in that the preparation method of the composite photo-catalyst
Specifically include the following steps:
Weigh the Bi (NO of 0.8 mmol3)3•5H2O is simultaneously dissolved in the nitric acid solution of pH=2.0 100mL and obtains Bi
(NO3)3Solution；The KI for weighing 20,30,40,60,70mg MIL-100 (Fe) and 0.8 mmol is added separately to going for 30mL
In ionized water, it is vigorously stirred and obtains evenly dispersed MIL-100 (Fe)-KI mixed liquor；By Bi (NO3)3Solution is added dropwise to
In MIL-100 (Fe)-KI mixed liquor, using the pH value of ammonium hydroxide adjustment solution to pH=3, by mixed liquor heating water bath to 85 DEG C,
It continuously stirs for 24 hours；The isolated product of magnetic agitation, after ethyl alcohol and 3 deionized waters of the product by 3 times wash, 40
Dry 12h, can be obtained MIL-100 (Fe)/BiOI composite photo-catalyst of different ratio under DEG C vacuum.
8. composite photo-catalyst according to claim 2, which is characterized in that the preparation method of the composite photo-catalyst
Specifically include the following steps: the step 1) specifically include the following steps: weigh respectively 0.8456g trimesic acid and
1.6253g FeCl3·6H2O is dissolved in 30mL distilled water, and 0.214mL hydrofluoric acid and 0.165 mLHNO is then added3, stirring
Mixed solution is transferred in reaction kettle after mixing, 150 DEG C, successive reaction 12h are heated to, to after reaction, pass through centrifugation
The prepared orange colour product of separation method recycling, with distillation water washing 3 times of heat, last 150 DEG C of vacuum drying 12h.
9. application of the composite photo-catalyst described in claim 1-8 in Industrial Wastewater Treatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110152736A (en) * | 2019-05-07 | 2019-08-23 | 同济大学 | Expanded perlite-iodine oxygen bismuth composite photo-catalyst for oily waste water treatment |
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