CN107162051B - The preparation method of flower-shaped BiOCl photochemical catalyst and BiOCl photochemical catalyst obtained and application - Google Patents
The preparation method of flower-shaped BiOCl photochemical catalyst and BiOCl photochemical catalyst obtained and application Download PDFInfo
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- CN107162051B CN107162051B CN201710287367.XA CN201710287367A CN107162051B CN 107162051 B CN107162051 B CN 107162051B CN 201710287367 A CN201710287367 A CN 201710287367A CN 107162051 B CN107162051 B CN 107162051B
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000003054 catalyst Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims abstract description 42
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims abstract description 42
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 35
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 17
- 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 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 12
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000000376 reactant Substances 0.000 claims abstract description 10
- 239000012670 alkaline solution Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 19
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000010276 construction Methods 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000002957 persistent organic pollutant Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 235000002639 sodium chloride Nutrition 0.000 claims description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 3
- 229940012189 methyl orange Drugs 0.000 claims description 3
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- POJOORKDYOPQLS-UHFFFAOYSA-L barium(2+) 5-chloro-2-[(2-hydroxynaphthalen-1-yl)diazenyl]-4-methylbenzenesulfonate Chemical compound [Ba+2].C1=C(Cl)C(C)=CC(N=NC=2C3=CC=CC=C3C=CC=2O)=C1S([O-])(=O)=O.C1=C(Cl)C(C)=CC(N=NC=2C3=CC=CC=C3C=CC=2O)=C1S([O-])(=O)=O POJOORKDYOPQLS-UHFFFAOYSA-L 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 22
- 238000007146 photocatalysis Methods 0.000 abstract description 13
- 230000007547 defect Effects 0.000 abstract description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [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 23
- 229940043267 rhodamine b Drugs 0.000 description 23
- 230000015556 catabolic process Effects 0.000 description 16
- 238000006731 degradation reaction Methods 0.000 description 16
- 238000005352 clarification Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 230000001376 precipitating effect Effects 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000012901 Milli-Q water Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 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 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- AZQWKYJCGOJGHM-UHFFFAOYSA-N para-benzoquinone Natural products O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000007857 degradation product Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- -1 property bright red Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229940005561 1,4-benzoquinone Drugs 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001454 anthracenes Chemical class 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003256 environmental substance Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 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
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
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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
-
- 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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- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
The present invention provides the preparation method of flower-shaped BiOCl photochemical catalyst and BiOCl photochemical catalyst obtained and applications, described method includes following steps: (1) bismuth nitrate and maltose being added in water, and chloride solution is added dropwise, stirring forms bismuth presoma；The mole dosage ratio of the bismuth nitrate and maltose are as follows: 1:(0.2-3)；(2) pH value of bismuth presoma is adjusted to by 5.0-6.5 using alkaline solution, forms reactant；(3) reactant is subjected at 150-160 DEG C reaction 24-30h, is precipitated；(4) washing of precipitate for obtaining step (3), it is dry, obtain the BiOCl photochemical catalyst of flower-like structure.The present invention overcomes the defect of existing BiOCl photochemical catalyst preparation method, gained BiOCl photochemical catalyst can be good at responding to visible light, visible light photocatalysis active with higher and with good stability and reusable property.
Description
Technical field
The invention belongs to the systems of environmental chemical engineering photocatalysis water-treatment technology field more particularly to flower-shaped BiOCl photochemical catalyst
Preparation Method and BiOCl photochemical catalyst obtained and application.
Background technique
In recent years, problem of environmental pollution is paid attention to by more and more countries.Socio-economic development is very rapid, in fossil
Under the premise of the energy is largely consumed, photocatalysis technology has been expedited the emergence of, photocatalysis technology is green environment friendly technology, and the sun
Can be inexhaustible, it is current ideal clean energy resource, novel photocatalyst undoubtedly becomes research hotspot instantly.Mesh
Preceding international symposium is to TiO2It studies extensively and gos deep into as photochemical catalyst, still, TiO2Band-gap energy is larger, therefore can only absorbing wavelength
Ultraviolet light less than 387nm, cannot respond to visible light, hinder its development and application, therefore preparing can be with responding to visible light
Novel photocatalysis material becomes research hotspot instantly.Bismuth oxychloride (BiOCl) is the more visible light-responded light of current research
One of catalyst.Currently, being mostly used semiconductors coupling in the world, noble metal loading, transient metal doped and nonmetalloid mixing
The methods such as miscellaneous improve photocatalyst activity, these methods reduce the recombination probability of light induced electron and photohole, thus bright
The performance of the aobvious degradating organic dye for improving photochemical catalyst.But these method processes are cumbersome, higher cost, need largely again
Miscellaneous equipment.It thus needs to need a kind of simple, efficient and green preparation method.
Summary of the invention
In view of the above drawbacks of the prior art, one of main object of the present invention is to provide flower-shaped BiOCl photochemical catalyst
Preparation method, the preparation method, which has, is not necessarily to complex device, easy to operate, low in cost, to can be used for factory's serialization big
The advantages that amount production.
In order to achieve the above object, the present invention adopts the following technical scheme that, the preparation method of flower-shaped BiOCl photochemical catalyst,
Described method includes following steps:
(1) bismuth nitrate and maltose are added in water, and chloride solution is added dropwise, stirring forms bismuth presoma；It is described
The mole dosage ratio of bismuth nitrate and maltose are as follows: 1:(0.2-3)；
(2) pH value of bismuth presoma is adjusted to by 5.0-6.5 using alkaline solution, forms reactant；
(3) reactant is subjected at 150-160 DEG C reaction 24-30h, is precipitated；
(4) washing of precipitate for obtaining step (3), it is dry, obtain the BiOCl photochemical catalyst of flower-like structure.
As a further preference, in the step (1), the chloride is selected from potassium chloride, sodium chloride and ammonium chloride.
As a further preference, in the step (1), the mole dosage ratio of the bismuth nitrate and maltose are as follows: 1:
(0.3-1.5)。
As a further preference, in the step (2), the alkaline solution is selected from potassium hydroxide, sodium hydroxide and ammonia
Water.
As a further preference, in the step (2), the pH value of the bismuth presoma is adjusted to 6.0.
As a further preference, in the step (3), reactant is reacted for 24 hours at 160 DEG C.
As a further preference, in the step (4), the washing includes: more using deionized water and dehydrated alcohol
Secondary washing, the drying include: the at a temperature of vacuum drying at 30-50 DEG C.
Another object of the present invention is to provide one kind BiOCl photochemical catalyst as made from above-mentioned preparation method, gained light
Catalyst can be good at responding to visible light, visible light photocatalysis active with higher and it is with good stability and
Reusable property.
One kind BiOCl photochemical catalyst as made from above-mentioned preparation method, the photochemical catalyst are by sheet construction unit group
The flat flower-like structure dressed up, thickness≤105nm of the photochemical catalyst construction unit, the forbidden bandwidth of the photochemical catalyst are
1.5-2.8eV。
Another object of the present invention is to provide a kind of application of BiOCl photochemical catalyst as made from above-mentioned preparation method,
The photochemical catalyst can be applied to degradable organic pollutant in organic wastewater under the irradiation of visible light or ultraviolet light.
As a further preference, the organic pollutant is selected from rhodamine B, methyl orange, methylene blue and reactive brilliant red.
The beneficial effects of the present invention are: the present invention passes through nitrate and chlorine using bismuth nitrate, chloride and maltose as raw material
BiOCl photochemical catalyst is prepared in reaction between compound.Temperature of the preparation method of the present invention when being reacted is only 150-
160 DEG C, energy consumption is less.In addition, remaining is preparing reagent used in catalyst process, such as water, chloride and lye etc.
It is cheap and easy to get, the reagent of no pollution to the environment, therefore the environment friendly of this catalyst is embodied well.And this method exists
Step simple and convenient during preparation, this step of the pH value of more complicated adjusting bismuth presoma, and do not have to be adjusted to
Strong acid or highly basic, only with being adjusted to faintly acid.
Preparation method of the present invention is not necessarily to large amount of complex equipment, easy temperature control system, easy to operate, cost compared to other methods
It is lower, found by performance test, properties of sample is stable and visible light photocatalysis active with higher, thus be expected to future into
Row large-scale industrial production.Through characterizing, synthetic sample is flat flower-shaped point assembled by a large amount of sheet construction units
Level structure BiOCl.
Detailed description of the invention
Fig. 1 is the XRD spectra for adding BiOCl made from the preparation method of the embodiment of the present invention of not same amount maltose.
Fig. 2 a-2d is the SEM photograph for adding BiOCl made from the preparation method of the embodiment of the present invention of not same amount maltose.
Fig. 3 a-3d is TEM and the SAED photograph for adding BiOCl made from the preparation method of the embodiment of the present invention of 0.5g maltose
Piece.
Fig. 4 a-4b is the DRS figure for adding BiOCl made from the preparation method of the embodiment of the present invention of not same amount maltose.
Fig. 5 is the ultraviolet-ray visible absorbing graph of relation of RhB in light application time and solution.
Fig. 6 a is to add not same amount maltose under visible light to influence schematic diagram to the photocatalytic activity of BiOCl degradation RhB.
Fig. 6 b is to add not same amount maltose under ultraviolet light to influence schematic diagram to the photocatalytic activity of BiOCl degradation RhB.
Fig. 7 a is to add different free radical inhibitors under visible light and degrade to the BiOCl being prepared by 0.5g maltose
The photocatalytic activity of RhB influences.
Fig. 7 b is to add the BiOCl degradation RhB that 0.1g maltose is prepared in different free radical inhibitors under ultraviolet light
Photocatalytic activity influence.
Fig. 8 a is to add the degradation of BiOCl made from the preparation method of the embodiment of the present invention of 0.5g maltose RhB under visible light
Circulation experiment schematic diagram.
Fig. 8 b is to add the degradation of BiOCl made from the preparation method of the embodiment of the present invention of 0.1g maltose RhB under ultraviolet light
Circulation experiment schematic diagram.
Specific embodiment
The present invention as provide flower-shaped BiOCl photochemical catalyst preparation method and made from BiOCl photochemical catalyst and application,
Overcome the defect of existing BiOCl photochemical catalyst preparation method, gained photochemical catalyst can be good at responding to visible light, have compared with
High visible light photocatalysis active and with good stability and reusable property.
In order to solve drawbacks described above, the main thought of the embodiment of the present invention is:
The preparation method of the flower-shaped BiOCl photochemical catalyst of the embodiment of the present invention, described method includes following steps:
(1) bismuth nitrate and maltose are added in ultrapure water water, and chloride solution is added dropwise, stirring forms bismuth forerunner
Body；The mole dosage ratio of the bismuth nitrate and maltose are as follows: 1:(0.2-3)；
(2) pH value of bismuth presoma is adjusted to by 5.0-6.5 using alkaline solution, forms reactant；
(3) reactant is subjected at 150-160 DEG C reaction 24-30h, is precipitated；
(4) washing of precipitate for obtaining step (3), it is dry, obtain the BiOCl photochemical catalyst of flower-like structure.
Bismuth source is typically chosen bismuth nitrate, such as commercially available Bi (NO in synthesis process3)3·5H2O, bismuth nitrate decomposes in water
At basic salt.The chloride is soluble easily in water, is configured to solution for standby.The water is preferably deionized water or ultrapure water
The less water of equal impurity.
It when being stirred described in step (1), is typically disposed under the conditions of 15-40 DEG C of room temperature, bismuth can be formed when stirring 0.5-1h
Presoma when if you need to be transferred to bismuth presoma in reaction kettle, can continue to stir.
In step (2), the alkaline solution is selected from potassium hydroxide, sodium hydroxide and ammonium hydroxide, and the alkaline solution will be before bismuth
It drives body and is adjusted to faintly acid, use magnetic stirrer when necessary.
In step (3), for the temperature of reaction at 150-160 DEG C, energy consumption is less.
In step (4), deionized water can be used and dehydrated alcohol repeatedly washs, and is dried in 30-50 DEG C of at a temperature of vacuum
It is dry, the BiOCl photochemical catalyst of the controllable flat flower-like structure of size is finally obtained, the BiOCl photochemical catalyst construction unit
The forbidden bandwidth of thickness≤105nm, the photochemical catalyst is controllable to 1.5-2.8eV.
The embodiment of the present invention carries out the crystallinity for the BiOCl sample being prepared, purity and object phase composition with XRD
Analysis；It is analyzed with pattern of the SEM to sample；TEM then carries out further point to the pattern of sample and microstructure
Analysis；DRS tests the light absorption threshold value and band-gap energy of sample.And using RhB as target degradation product, the photocatalysis of BiOCl is had studied
Activity, it is demonstrated experimentally that BiOCl photochemical catalyst visible light catalysis activity with higher.
In order to which the objectives, technical solutions, and advantages of the present invention are more clearly understood, with reference to embodiments, to the present invention
It is further elaborated.Specific data are only to explain the present invention involved in specific example described herein, not
For limiting the present invention.
Embodiment 1
The five water bismuth nitrates of 0.48507g and the maltose of 0.5g are weighed in beaker using electronic balance；Compound concentration is
The Klorvess Liquid of 0.2mol/L and the potassium hydroxide solution of 1mol/L；25mL deionized water is added into beaker, and adds dropwise
The Klorvess Liquid for entering the 0.2mol/L of 10mL stirs when being added dropwise, after being added dropwise, continues that 0.5h, shape is stirred at room temperature
At certain density bismuth presoma；Bismuth presoma in beaker is transferred in inner liner of reaction kettle, continues to be stirred at room temperature；It uses
Prepared potassium hydroxide solution adjusts bismuth presoma pH to 6.0；Reaction kettle is installed, baking oven is put into, is carried out at 160 DEG C
Hydro-thermal reaction for 24 hours, is precipitated；It washs by precipitating milli-Q water to clarification, then with dehydrated alcohol to clarification, is put into true
Empty drying box is dried at 40 DEG C, and target product BiOCl can be obtained.
Embodiment 2
The five water bismuth nitrates of 0.48507g and the maltose of 0.1g are weighed in beaker using electronic balance；Compound concentration is
The Klorvess Liquid of 0.2mol/L and the potassium hydroxide solution of 1mol/L；25mL deionized water is added into beaker, and adds dropwise
The Klorvess Liquid for entering the 0.2mol/L of 10mL stirs when being added dropwise, after being added dropwise, continues that 0.5h, shape is stirred at room temperature
At certain density bismuth presoma；Bismuth presoma in beaker is transferred in inner liner of reaction kettle, continues to be stirred at room temperature；It uses
Prepared potassium hydroxide solution adjusts bismuth presoma pH to 6.0；Reaction kettle is installed, baking oven is put into, is carried out at 160 DEG C
Hydro-thermal reaction for 24 hours, is precipitated；It washs by precipitating milli-Q water to clarification, then with dehydrated alcohol to clarification, is put into true
Empty drying box is dried at 40 DEG C, and target product BiOCl can be obtained.
Embodiment 3
The five water bismuth nitrates of 0.48507g and the maltose of 0.3g are weighed in beaker using electronic balance；Compound concentration is
The sodium chloride solution of 0.5mol/L and the sodium hydroxide solution of 1.5mol/L；25mL deionized water is added into beaker, and dropwise
The sodium chloride solution of the 0.5mol/L of 10mL is added, is stirred when being added dropwise, after being added dropwise, continues that 0.5h is stirred at room temperature,
Form certain density bismuth presoma；Bismuth presoma in beaker is transferred in inner liner of reaction kettle, continues to be stirred at room temperature；Make
Bismuth presoma pH to 6.0 is adjusted with prepared sodium hydroxide solution；Reaction kettle is installed, baking oven is put into, is carried out at 155 DEG C
The hydro-thermal reaction of 26h, is precipitated；It washs by precipitating milli-Q water to clarification, then with dehydrated alcohol to clarification, is put into true
Empty drying box is dried at 30 DEG C, and target product BiOCl can be obtained.
Embodiment 4
The five water bismuth nitrates of 0.48507g and the maltose of 1.0g are weighed in beaker using electronic balance；Compound concentration is
The ammonium chloride solution of 0.1mol/L and the ammonia spirit of 0.5mol/L；25mL deionized water is added into beaker, and is added dropwise
The ammonium chloride solution of the 0.1mol/L of 15mL is stirred when being added dropwise, and after being added dropwise, is continued that 1h is stirred at room temperature, is formed one
Determine the bismuth presoma of concentration；Bismuth presoma in beaker is transferred in inner liner of reaction kettle, continues to be stirred at room temperature；Use preparation
Good ammonia spirit adjusts bismuth presoma pH to 6.5；Reaction kettle is installed, baking oven is put into, the hydro-thermal of 30h is carried out at 150 DEG C
Reaction, is precipitated；It washs by precipitating milli-Q water to clarification, then with dehydrated alcohol to clarification, is put into vacuum oven,
It is dried at 50 DEG C, target product BiOCl can be obtained.
Embodiment 5
Weigh the Bi (NO of 0.48507g3)3·5H2The maltose of O and 0.07g is in beaker；Compound concentration is 0.2mol/l
Potassium chloride and 1mol/l potassium hydroxide solution；25ml ultrapure water is added into beaker, and 10ml is added dropwise into cup and configures
0.2mol/l Klorvess Liquid, and after 0.5h is stirred at room temperature, form certain density bismuth precursor；By the bismuth in beaker
Presoma is transferred in reaction kettle, continues to stir；The pH value of bismuth presoma is adjusted to 6.0 using the potassium hydroxide solution of 1mol/l；
Reaction kettle is carried out to hydro-thermal reaction for 24 hours at 160 DEG C, is precipitated；Precipitating deionized water and dehydrated alcohol are repeatedly washed
Wash, it is rear using vacuum oven 40 DEG C at a temperature of dry, BiOCl photochemical catalyst can be obtained.
Embodiment 6
Weigh the Bi (NO of 0.48507g3)3·5H2The maltose of O and 1.08g is in beaker；Compound concentration is 0.2mol/l
Potassium chloride and 1mol/l potassium hydroxide solution；25ml ultrapure water is added into beaker, and 10ml is added dropwise into cup and configures
0.2mol/l Klorvess Liquid, and after 0.5h is stirred at room temperature, form certain density bismuth precursor；By the bismuth in beaker
Presoma is transferred in reaction kettle, continues to stir；The pH value of bismuth presoma is adjusted to 6.0 using the potassium hydroxide solution of 1mol/l；
Reaction kettle is carried out to hydro-thermal reaction for 24 hours at 160 DEG C, is precipitated；Precipitating deionized water and dehydrated alcohol are repeatedly washed
Wash, it is rear using vacuum oven 40 DEG C at a temperature of dry, BiOCl photochemical catalyst can be obtained.
Fig. 1 is the 1-4 preparation method system of the embodiment of the present invention for adding not same amount maltose (0.1g, 0.3g, 0.5g, 1.0g)
The XRD spectra of the BiOCl obtained.It can be seen from the figure that diffraction maximum position and standard card (JCPDS:85-0861) complete one
It causes, illustrates that synthetic sample is pure phase BiOCl；Discovery is examined, diffraction maximum peak shape is sharp, and intensity is larger, synthesized by explanation
Sample have good crystallinity.
Fig. 2 a-2d is the present invention reality for adding not same amount maltose (2a:0.1g, 2b:0.3g, 2C:0.5g, 2d:1.0g)
Apply the SEM photograph of BiOCl made from a preparation method.Synthetic sample is the flat flower assembled by a large amount of sheet construction units
Shape hierarchical structure BiOCl.Fig. 2 a is the SEM photograph for adding the BiOCl of 0.1g maltose, it can be seen from the figure that construction unit
Maximum gauge be 103nm, be made of a large amount of sheet construction units it is flat flower-shaped, such structure be conducive to photoproduction electricity
Son-hole separation, to significantly promote photocatalyst activity.
Fig. 3 a-3d is TEM and the SAED photograph for adding BiOCl made from the preparation method of the embodiment of the present invention of 0.5g maltose
Piece.Further demonstrate the flat flower-like structure of sample.It can be seen that obvious clearly lattice fringe from TEM photo, illustrate sample
Product have good crystallinity, and calculating interplanar distance is 0.275nm, and corresponding is (110) face；SAED photo is it is found that synthesized
Sample be monocrystalline.
Fig. 4 a-4b is the DRS figure for adding BiOCl made from the preparation method of the embodiment of the present invention of not same amount maltose.It cuts
Collimation method can calculate addition 0.1g, 0.3g, 0.5g, 1.0g maltose BiOCl forbidden bandwidth be respectively 2.78eV,
2.51eV、2.25eV、1.76eV。
The effect of the method for the BiOCl photocatalyst treatment organic wastewater of preparation of the embodiment of the present invention in order to obtain, to this
The BiOCl photochemical catalyst of inventive embodiments preparation, which carries out following a series of experiments, to be proved:
The embodiment of the present invention has studied catalyst of the embodiment of the present invention for catalytic treatment organic wastewater by taking rhodamine B as an example
When process, to the degradation effect of organic pollutant in water environment, but the embodiment of the present invention is not limited to only to rhodamine B
It working, other pollutants of degrading also can achieve the effect of similar catalytic degradation, such as: methyl orange, methylene blue and work
The Anthraquinones such as property bright red, quinone imides, oxa anthracenes and azo organic pollutant.
Photocatalytic degradation test:
Using LED light as light source, a set of cups outer layer is by condensed water to ensure that light-catalyzed reaction carries out at a constant temperature.With dense
Degree is 20mg/L, rhodamine B (RhB) solution that volume is 100mL does target degradation product, and catalyst is added to having comprising RhB
In machine waste water solution.Prior to absorption stirring 30min under dark unglazed environment before light-catalyzed reaction, to ensure to reach absorption
Balance, sampling is primary at regular intervals after turning on light, every sub-sampling 1.0mL, reaction time 30min.With 0.45 μm after sampling
Water system syringe membrane filtration removes remaining a small amount of catalyst in sample, is placed in 5mL quartz colorimetric utensil, and it is ultrapure that 2mL is added
Water uses absorbance (maximum absorption wavelength λ=554nm, or in wave-length coverage 200- of ultraviolet-visual spectrometer detection filtrate
700nm carries out full wavelength scanner).With the degradation rate C/C of pollutant0Characterize the photocatalysis performance of composite catalyst.
Fig. 5 is the ultraviolet-ray visible absorbing graph of relation of RhB in light application time and solution.With rhodamine B at 554nm
Characteristic absorption peak indicates rhodamine B concentration.
Fig. 6 a is to add not same amount maltose under visible light to influence schematic diagram to the photocatalytic activity of BiOCl degradation RhB.
Fig. 6 b is the photocatalytic activity figure for adding the degradation of BiOCl synthesized by not same amount maltose RhB under ultraviolet light.It can be seen that
Under visible light and ultraviolet light, BiOCl can realize effective degradation to rhdamine B；With TiO2(P25) fine compared to having
Photocatalytic activity and economy.By comparing discovery, it is seen that under light, the light of the BiOCl of addition 0.5g maltose preparation is urged
It is best to change performance；Under ultraviolet light, the photocatalysis performance of the BiOCl of addition 0.1g maltose preparation is best.
Fig. 7 a is to add the BiOCl degradation RhB that 0.5g maltose is prepared in different free radical inhibitors under visible light
Photocatalytic activity influence.Fig. 7 b is to add what 0.1g maltose was prepared in different free radical inhibitors under ultraviolet light
The photocatalytic activity of BiOCl degradation RhB influences.As it can be seen that the inhibitory effect of 1,4-benzoquinone is most strong in figure, therefore it could be speculated that super oxygen from
It is played a major role by base to the degradation of organic pollutant.
Fig. 8 a is to add the degradation of BiOCl made from the preparation method of the embodiment of the present invention of 0.5g maltose RhB under visible light
Circulation experiment schematic diagram.Fig. 8 b is under ultraviolet light, made from the preparation method of the embodiment of the present invention of addition 0.1g maltose
The circulation experiment schematic diagram of BiOCl degradation RhB.As it can be seen that BiOCl is recovered recycles five times in figure, photocatalysis performance is basic
No change has taken place, illustrates that properties of samples is stablized, there is good stability and reusable property.
Technical solution in above-mentioned the embodiment of the present application, at least have the following technical effects or advantages:
The present invention passes through the reaction between nitrate and chloride, preparation using bismuth nitrate, chloride and maltose as raw material
BiOCl photochemical catalyst out.Temperature of the preparation method of the present invention when being reacted is only 150-160 DEG C, and energy consumption is less.In addition,
Remaining is preparing reagent used in catalyst process, such as water, chloride and lye etc., be it is cheap and easy to get, to environment without dirt
The reagent of dye, therefore the environment friendly of this catalyst is embodied well.And this method step letter during preparation
It is easy to be convenient, this step of the pH value of more complicated adjusting bismuth presoma, and do not have to be adjusted to strong acid or highly basic, only using will
It is adjusted to faintly acid.
Preparation method of the present invention is not necessarily to large amount of complex equipment, easy temperature control system, easy to operate, cost compared to other methods
It is lower, found by performance test, properties of sample is stable and visible light photocatalysis active with higher, thus be expected to future into
Row large-scale industrial production.Through characterizing, synthetic sample is flat flower-shaped point assembled by a large amount of sheet construction units
Level structure BiOCl.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.Obviously, those skilled in the art can be to the present invention
Carry out various modification and variations without departing from the spirit and scope of the present invention.If in this way, these modifications and changes of the present invention
Within the scope of the claims of the present invention and its equivalent technology, then the present invention is also intended to encompass these modification and variations and exists
It is interior.
Claims (9)
1. the preparation method of flower-shaped BiOCl photochemical catalyst, it is characterised in that: described method includes following steps:
(1) bismuth nitrate and maltose are added in water, and chloride solution is added dropwise, stirring forms bismuth presoma；The nitric acid
The mole dosage ratio of bismuth and maltose are as follows: 1: (0.2-3)；
(2) pH value of bismuth presoma is adjusted to by 5.0-6.5 using alkaline solution, forms reactant；
(3) reactant is subjected at 150-160 DEG C reaction 24-30h, is precipitated；
(4) washing of precipitate for obtaining step (3), it is dry, obtain the BiOCl photochemical catalyst of flower-like structure；
The BiOCl photochemical catalyst is the flat flower-like structure assembled by sheet construction unit, and the photochemical catalyst constructs list
First thickness≤105nm, the forbidden bandwidth of the photochemical catalyst are 1.5-2.8eV.
2. the preparation method of flower-shaped BiOCl photochemical catalyst according to claim 1, it is characterised in that: the step (1)
In, the chloride is selected from potassium chloride, sodium chloride and ammonium chloride.
3. the preparation method of flower-shaped BiOCl photochemical catalyst according to claim 1, it is characterised in that: the step (1)
In, the mole dosage ratio of the bismuth nitrate and maltose are as follows: 1: (0.3-1.5).
4. the preparation method of flower-shaped BiOCl photochemical catalyst according to claim 1, it is characterised in that: the step (2)
In, the alkaline solution is selected from potassium hydroxide, sodium hydroxide and ammonium hydroxide.
5. the preparation method of flower-shaped BiOCl photochemical catalyst according to claim 1, it is characterised in that: the step (2)
In, the pH value of the bismuth presoma is adjusted to 6.0.
6. the preparation method of flower-shaped BiOCl photochemical catalyst according to claim 1, it is characterised in that: the step (3)
In, reactant is reacted for 24 hours at 160 DEG C.
7. the preparation method of flower-shaped BiOCl photochemical catalyst according to claim 1, it is characterised in that: the step (4)
In, the washing includes: repeatedly to be washed using deionized water and dehydrated alcohol, the drying include: 30-50 DEG C at a temperature of
Vacuum drying.
8. the application of BiOCl photochemical catalyst made from the preparation method as described in claim any one of 1-7, it is characterised in that: institute
BiOCl photochemical catalyst is stated under the irradiation of visible light or ultraviolet light, can be applied to degradable organic pollutant in organic wastewater.
9. the application of BiOCl photochemical catalyst according to claim 8, it is characterised in that: the organic pollutant is selected from sieve
Red bright B, methyl orange, methylene blue and reactive brilliant red.
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