CN107008462A - The preparation method of flower-shaped and spherical BiOCl photochemical catalysts and obtained photochemical catalyst and application - Google Patents
The preparation method of flower-shaped and spherical BiOCl photochemical catalysts and obtained photochemical catalyst and application Download PDFInfo
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- CN107008462A CN107008462A CN201710287035.1A CN201710287035A CN107008462A CN 107008462 A CN107008462 A CN 107008462A CN 201710287035 A CN201710287035 A CN 201710287035A CN 107008462 A CN107008462 A CN 107008462A
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000003054 catalyst Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 74
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 44
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 229920002472 Starch Polymers 0.000 claims abstract description 29
- 235000019698 starch Nutrition 0.000 claims abstract description 29
- 239000008107 starch Substances 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 13
- 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 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 12
- 239000012670 alkaline solution Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 39
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 17
- 239000001103 potassium chloride Substances 0.000 claims description 14
- 235000011164 potassium chloride Nutrition 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 235000002639 sodium chloride Nutrition 0.000 claims description 5
- 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
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 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 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
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 239000002957 persistent organic pollutant Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 19
- 230000008569 process Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000003643 water by type Substances 0.000 description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 19
- 238000007146 photocatalysis Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000011941 photocatalyst Substances 0.000 description 9
- 230000008859 change Effects 0.000 description 7
- 230000000593 degrading effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000002242 deionisation method Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000011807 nanoball Substances 0.000 description 2
- 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 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 150000001454 anthracenes Chemical class 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000356 contaminant 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
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- AZQWKYJCGOJGHM-UHFFFAOYSA-N para-benzoquinone Natural products O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- -1 quinone imides Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
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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
- 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
-
- 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
-
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
-
- 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
-
- 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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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention provides the preparation method of flower-shaped and spherical BiOCl photochemical catalysts and obtained photochemical catalyst and application, the preparation method includes：(1) bismuth nitrate and starch are added in water, stirs, obtains the mixed liquor of bismuth-containing；The quality amount ratio of the bismuth nitrate and starch is：(0.3‑5)：1；(2) chloride solution is added dropwise in the mixed liquor that step (1) is obtained, stirs, obtain the precursor solution of bismuth-containing；(3) pH value of the precursor solution for the bismuth-containing for being obtained step (2) using alkaline solution and acid solution is adjusted to 5.0 6.5, stirs to form reactant；(4) step (3) gained reactant is carried out at 150 160 DEG C reacting 24 30h, precipitated；(5) washing of precipitate for obtaining step (4), dries, obtains flower-shaped and spherical morphology BiOCl powders.Advantages of nontoxic raw materials that the inventive method is used is harmless, green and healthy and process is simple, and prepared photochemical catalyst has good photocatalytic activity.
Description
Technical field
The invention belongs to the preparation of photochemical catalyst preparing technical field, more particularly to flower-shaped and spherical BiOCl photochemical catalysts
Method and obtained photochemical catalyst and application.
Background technology
In recent years, problem of environmental pollution is paid attention to by increasing country.Socio-economic development is very rapid, in fossil
On the premise of the energy is by a large amount of 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 preferably clean energy resource, novel photocatalyst undoubtedly turns into study hotspot instantly.Mesh
It is preceding in the world to TiO2Study extensively and go deep into as photochemical catalyst, still, TiO2Band-gap energy is larger, thus can only absorbing wavelength it is small
In 387nm ultraviolet light, it is impossible to responding to visible light, its development and application is hindered, therefore preparation can be with the new of responding to visible light
Type catalysis material turns into study hotspot instantly.Bismoclite (BiOCl) is a kind of novel semi-conductor photochemical catalyst, but relatively low
Visible light utilization ratio limit its practical application.At present, semiconductors coupling, noble metal loading, transition gold are used in the world
Belong to the method such as doping and the doping of nonmetalloid to improve photocatalyst activity, these methods reduce light induced electron and photoproduction
The recombination probability in hole, so as to significantly improve the performance of the degradating organic dye of photochemical catalyst.But these procedures are numerous
Trivial, cost is higher, need large amount of complex equipment.
The content of the invention
For the drawbacks described above of prior art, one of main object of the present invention is to provide flower-shaped and spherical BiOCl light
The preparation method of catalyst, advantages of nontoxic raw materials that the preparation method is used is harmless, green and healthy and process is simple, is conducive to engineering
Change extensive preparation, prepared photochemical catalyst has good photocatalytic activity.
In order to achieve the above object, the present invention is adopted the following technical scheme that, the preparation of flower-shaped and spherical BiOCl photochemical catalysts
Method, methods described comprises the following steps：
(1) bismuth nitrate and starch are added in water, stirs, obtains the mixed liquor of bismuth-containing；The bismuth nitrate and starch
Quality amount ratio be：(0.3-5)：1；
(2) chloride solution is added dropwise in the mixed liquor that step (1) is obtained, stirs, obtain the forerunner of bismuth-containing
Liquid solution；
(3) pH value of the precursor solution for the bismuth-containing for being obtained step (2) using alkaline solution and acid solution is adjusted to 5.0-
6.5, stir to form reactant；
(4) step (3) gained reactant is subjected to reaction 24-30h at 150-160 DEG C, precipitated；
(5) washing of precipitate for obtaining step (4), dries, obtains flower-shaped and spherical morphology BiOCl powders.
As further preferably, in the step (1), the quality amount ratio of the bismuth nitrate and starch is：(1.5-
5)：1.
As further preferably, in the step (2), the chloride is selected from potassium chloride, sodium chloride and ammonium chloride.
As further preferably, in the step (2), the mole dosage ratio of the bismuth nitrate and chloride is：1：
(1-2)。
As further preferably, in the step (3), the alkaline solution is selected from potassium hydroxide, sodium hydroxide and ammonia
Water, the acid solution is selected from nitric acid.
As further preferably, in the step (3), the pH value of the bismuth-containing precursor solution mixed liquor is adjusted to 6.0.
As further preferred, in the step (4), reactant is subjected to reaction 24h at 160 DEG C.
It is described another object of the present invention is to provide a kind of BiOCl photochemical catalysts as made from above-mentioned preparation method
BiOCl photochemical catalysts are the flower-shaped and chondritic that micro-nano of BiOCl is stacked into, and the thickness of described micro-nano is 25-
30nm。
Another object of the present invention is to provide a kind of application of the BiOCl photochemical catalysts as made from above-mentioned preparation method,
The BiOCl photochemical catalysts can be applied to degradable organic pollutant in organic wastewater under the irradiation of visible ray or ultraviolet light.
As further preferably, the organic pollution is selected from rhodamine B, methyl orange, methylene blue and reactive brilliant red.
As further preferably, the quality usage ratio of the organic pollution and BiOCl photochemical catalysts is 1:(20-
30)。
The beneficial effects of the invention are as follows：The present invention is by controlling Bi (NO3)3Different amounts of starch is added in solution, after will be molten
The pH value of liquid is adjusted to faintly acid, to obtain the different sizes with more preferable photocatalytic activity and the BiOCl nano materials of pattern.
Preparation method of the present invention using green safety raw material, method is simple, process is easily operated, can be continuously produced.This method exists
The temperature for carrying out hydro-thermal reaction is only 150-160 DEG C, and energy consumption is less.In addition, remaining examination for being used in catalyst process is prepared
Agent, such as water, chloride and alkali lye, acid solution etc., are reagent cheap and easy to get, environmentally safe, therefore embody well
The environment friendly of this catalyst.And this method step simple and convenient during preparation, complex regulation pH value
This step, and without being adjusted to strong acid or highly basic, only with being adjusted to faintly acid.
Flower-shaped, spherical morphology the BiOCl nano materials being prepared by the method for the present invention have compared with other BiOCl materials
There is high, the higher specific surface area of crystallinity, can be adsorbed more while more reactivity sites can be provided
Many pollutants, are conducive to improving the photocatalysis efficiency of photochemical catalyst.By active testing under visible light, obtained result
Show that the BiOCl nano materials for preparing and going out by the present invention have good stability and repeatable usability, with fine
Photocatalytic activity and economy.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram (XRD) of BiOCl photochemical catalysts prepared by the embodiment of the present invention.
Fig. 2 a-2d are the stereoscan photograph (SEM) of BiOCl photochemical catalysts prepared by the embodiment of the present invention.
Fig. 3 is BiOCl photocatalyst for degrading RhB prepared by embodiment of the present invention all-wave scanning figure.
Fig. 4 is that the embodiment of the present invention adds BiOCl photocatalyst for degrading RhB solution efficacies prepared by different amounts of starch
Figure.
The BiOCl photochemical catalyst cycle performance figures that Fig. 5 is prepared for the embodiment of the present invention of addition 0.1g starch.
Embodiment
The present invention is by providing the preparation method and obtained photochemical catalyst of flower-shaped and spherical BiOCl photochemical catalysts and answering
With solving the defect of the preparation method and photocatalysis performance of existing BiOCl photochemical catalysts etc..
In order to solve drawbacks described above, the main thought of the embodiment of the present invention is：
The embodiment of the present invention is flower-shaped and preparation method of spherical BiOCl photochemical catalysts, and methods described comprises the following steps：
(1) bismuth nitrate and starch are added in water, stirs, obtains the mixed liquor of bismuth-containing；The bismuth nitrate and starch
Quality amount ratio be：(0.3-5)：1；
(2) chloride solution is added dropwise in the mixed liquor that step (1) is obtained, stirs, obtain the forerunner of bismuth-containing
Liquid solution；
(3) pH value of the precursor solution for the bismuth-containing for being obtained step (2) using alkaline solution and acid solution is adjusted to 5.0-
6.5, stir to form reactant；
(4) step (3) gained reactant is subjected to reaction 24-30h at 150-160 DEG C, precipitated；
(5) washing of precipitate for obtaining step (4), dries, obtains flower-shaped and spherical morphology BiOCl powders.
The nitric acid bismuth raw material is typically chosen containing the crystallization water, such as commercially available Bi (NO3)3·5H2O, the nitric acid in water
Bismuth resolves into basic salt.The chloride is soluble in water, is configured to solution for standby, chloride can be added into water during preparation
In, ultrasonic 20-40min is uniformly mixing to obtain chloride solution.The water preferably for the impurity such as deionized water or ultra-pure water compared with
Few water.
Before reaction, when such as the reactant of step (3) need to be transferred in reactor, reactant can be shifted using water.
In step (3), the alkaline solution is selected from potassium hydroxide, sodium hydroxide and ammoniacal liquor, the alkaline solution and acid solution
Mixed liquor is adjusted to faintly acid, if necessary using magnetic stirrer.
In step (5), can repeatedly it be washed using deionized water and absolute ethyl alcohol, and vacuum is dried at a temperature of 30-50 DEG C
It is dry, finally obtain controllable flower-shaped, chondritic the BiOCl powders of size.
BiOCl microstructure and its photocatalytic activity have a direct relation, therefore change microstructure and be considered as pair
A kind of approach that BiOCl is modified, specifically refers to not change BiOCl thing phase, is made by changing synthetic method or adjustment
Optimize BiOCl microstructure for technique, to prepare the surface area higher BiOCl nano materials of big, crystallinity, so as to change
It is apt to its photocatalytic activity.With the increase of amount of starch, the quantity of nanometer sheet also increases, and causes gap between piece and piece increasingly
It is small, gradually form the micro-nano ball that surface is made up of nanometer sheet.The BiOCl of flower-shaped, spherical hierarchy not only can significantly increase
Plus BiOCl surface area can also promote the separation and transmission of photo-generated carrier there is provided more reactivity sites.
In order to which the objects, 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 involved by specific example described herein are only to explain the present invention, not
For limiting the present invention.
Embodiment 1
Weigh the Bi (NO that quality is 0.48507g3)3·5H2O and 0.1g starch adds 15ml deionizations in beaker
Water, stirs at room temperature, obtains the mixed liquor of bismuth-containing, weighs 2.238g KCl and is added in 150ml ultra-pure waters, ultrasound
30min, is stirred until homogeneous and obtains KCl solution.Pipette the KCl solution that 10ml prepares to be titrated in bismuth-containing mixed liquor, stirring is equal
It is even, form bismuth-containing precursor solution；Above-mentioned bismuth-containing precursor solution is transferred to 50ml by beaker with 10ml deionized waters high
Press in reactor；KOH 5.611g are weighed, are dissolved in 50ml deionized waters, it is standby；25ml concentrated nitric acids are measured to be dissolved in
It is standby in 25ml deionized waters；With above-mentioned KOH, HNO prepared3Solution in reactor is adjusted pH to 6.0, stirring by solution
Autoclave is twisted after uniform；Autoclave is reacted into 24h in 160 DEG C of baking ovens, precipitated；Obtained precipitation is used
After deionized water and ethanol washing for several times, 40 DEG C of drying, that is, obtain flower-shaped, spherical morphology BiOCl light in vacuum drying chamber
Catalyst powder.
Embodiment 2
Weigh the Bi (NO that quality is 0.48507g3)3·5H2O and 0.3g starch adds 15ml deionizations in beaker
Water, stirs at room temperature, obtains the mixed liquor of bismuth-containing, weighs 2.238g KCl and is added in 150ml ultra-pure waters, ultrasound
30min, is stirred until homogeneous and obtains KCl solution.Pipette the KCl solution that 10ml prepares to be titrated in bismuth-containing mixed liquor, stirring is equal
It is even, form bismuth-containing precursor solution；Above-mentioned bismuth-containing precursor solution is transferred to 50ml by beaker with 10ml deionized waters high
Press in reactor；KOH 5.611g are weighed, are dissolved in 50ml deionized waters, it is standby；25ml concentrated nitric acids are measured to be dissolved in
It is standby in 25ml deionized waters；With above-mentioned KOH, HNO prepared3Bismuth-containing precursor solution in reactor is adjusted pH by solution
To 6, autoclave is twisted after stirring；Autoclave is reacted into 24h in 160 DEG C of baking ovens, precipitated；It will obtain
Precipitation washed for several times with deionized water and ethanol after, in vacuum drying chamber 40 DEG C drying, that is, obtain flower-shaped, spherical morphology
BiOCl photochemical catalyst powders.
Embodiment 3
Weigh the Bi (NO that quality is 0.48507g3)3·5H2O and 0.5g starch adds 15ml deionizations in beaker
Water, stirs at room temperature, obtains the mixed liquor of bismuth-containing, weighs 2.238g KCl and is added in 150ml ultra-pure waters, ultrasound
30min, is stirred until homogeneous and obtains KCl solution.Pipette the KCl solution that 10ml prepares to be titrated in bismuth-containing mixed liquor, stirring is equal
It is even, form bismuth-containing precursor solution；Above-mentioned bismuth-containing precursor solution is transferred to 50ml by beaker with 10ml deionized waters high
Press in reactor；KOH 5.611g are weighed, are dissolved in 50ml deionized waters, it is standby；25ml concentrated nitric acids are measured to be dissolved in
It is standby in 25ml deionized waters；With above-mentioned KOH, HNO prepared3Bismuth-containing precursor solution in reactor is adjusted pH by solution
To 6, autoclave is twisted after stirring；Autoclave is reacted into 24h in 160 DEG C of baking ovens, precipitated；It will obtain
Precipitation washed for several times with deionized water and ethanol after, in vacuum drying chamber 40 DEG C drying, that is, obtain flower-shaped, spherical morphology
BiOCl photochemical catalyst powders.
Embodiment 4
Weigh the Bi (NO that quality is 0.48507g3)3·5H2O and 1.0g starch adds 15ml deionizations in beaker
Water, stirs at room temperature, obtains the mixed liquor of bismuth-containing, weighs 2.238g KCl and is added in 150ml ultra-pure waters, ultrasound
30min, is stirred until homogeneous and obtains KCl solution.Pipette the KCl solution that 10ml prepares to be titrated in bismuth-containing mixed liquor, stirring is equal
It is even, form bismuth-containing precursor solution；Above-mentioned bismuth-containing precursor solution is transferred to 50ml by beaker with 10ml deionized waters high
Press in reactor；KOH 5.611g are weighed, are dissolved in 50ml deionized waters, it is standby；25ml concentrated nitric acids are measured to be dissolved in
It is standby in 25ml deionized waters；With above-mentioned KOH, HNO prepared3Bismuth-containing precursor solution in reactor is adjusted pH by solution
To 6, autoclave is twisted after stirring；Autoclave is reacted into 24h in 160 DEG C of baking ovens, precipitated；It will obtain
Precipitation washed for several times with deionized water and ethanol after, in vacuum drying chamber 40 DEG C drying, that is, obtain flower-shaped, spherical morphology
BiOCl photochemical catalyst powders.
Embodiment 5
Weigh the Bi (NO that quality is 0.48507g3)3·5H2O and 0.08g starch adds 15ml deionizations in beaker
Water, stirs at room temperature, obtains the mixed liquor of bismuth-containing, weighs 1.754g NaCl and is added in 150ml ultra-pure waters, ultrasound
30min, is stirred until homogeneous and obtains NaCl solution.Pipette the NaCl solution that 5ml prepares to be titrated in bismuth-containing mixed liquor, stirring is equal
It is even, form bismuth-containing precursor solution；Above-mentioned bismuth-containing precursor solution is transferred to 50ml by beaker with 10ml deionized waters high
Press in reactor；NaOH 3.99g are weighed, are dissolved in 50ml deionized waters, it is standby；25ml concentrated nitric acids are measured to be dissolved in
It is standby in 25ml deionized waters；With above-mentioned NaOH, HNO prepared3Bismuth-containing precursor solution in reactor is adjusted pH by solution
To 5.0, autoclave is twisted after stirring；Autoclave is reacted into 30h in 150 DEG C of baking ovens, precipitated；Will
After the precipitation arrived is washed for several times with deionized water and ethanol, 30 DEG C of drying, that is, obtain flower-shaped, spherical morphology in vacuum drying chamber
BiOCl photochemical catalyst powders.
Embodiment 6
Weigh the Bi (NO that quality is 0.48507g3)3·5H2O and 0.80g starch adds 20ml deionizations in beaker
Water, stirs at room temperature, obtains the mixed liquor of bismuth-containing, weighs 1.605g ammonium chlorides and is added in 150ml ultra-pure waters, ultrasound
30min, is stirred until homogeneous and obtains ammonium chloride solution.The ammonium chloride solution that 10ml prepares is pipetted to be titrated in bismuth-containing mixed liquor,
Stir, form bismuth-containing precursor solution；Above-mentioned bismuth-containing precursor solution is transferred to by beaker with 10ml deionized waters
In 50ml autoclaves；KOH 5.611g are weighed, are dissolved in 50ml deionized waters, it is standby；Measure 25ml concentrated nitric acids
It is dissolved in 25ml deionized waters, it is standby；With above-mentioned KOH, HNO prepared3Solution is by bismuth-containing precursor solution in reactor
PH is adjusted to 6.5, autoclave is twisted after stirring；Autoclave is reacted into 26h in 155 DEG C of baking ovens, sunk
Form sediment；After obtained precipitation is washed for several times with deionized water and ethanol, in vacuum drying chamber 50 DEG C drying, that is, obtain it is flower-shaped,
The BiOCl photochemical catalyst powders of spherical morphology.
Fig. 1 is the X-ray diffraction spectrogram (XRD) of BiOCl photochemical catalysts prepared by 1-4 of the embodiment of the present invention.With standard
BiOCl collection of illustrative plates compares, and the BiOCl for adding four kinds of not same amount Starch synthesis does not have found miscellaneous peak, shows in products therefrom without miscellaneous
Matter is present, and products therefrom is pure phase；Discovery is examined, products therefrom diffraction maximum peak shape is sharp, shows that products therefrom has good
Good crystallinity.
Fig. 2 a-2d are the stereoscan photograph (SEM) of BiOCl photochemical catalysts prepared by 1-4 of the embodiment of the present invention.Fig. 2 a are
Plus BiOCl photochemical catalysts prepared by 0.1g starch；The BiOCl photochemical catalysts that Fig. 2 b are prepared for addition 0.3g starch；Fig. 2 c are to add
BiOCl photochemical catalysts prepared by 0.5g starch；The BiOCl photochemical catalysts that Fig. 2 d are plus prepared by 1.0g starch.Such as Fig. 2 a-2d institutes
Show, the BiOCl for adding 0.1g Starch synthesis is the flower-like structure stacked by nanometer sheet, with the increase of amount of starch, nanometer
The quantity of piece also increases, and causes the gap between piece and piece less and less, gradually form surface by nanometer sheet constitute it is micro-nano
Ball.
In order to obtain the embodiment of the present invention preparation BiOCl photocatalyst treatment organic wastewaters method effect, to this
BiOCl photochemical catalysts prepared by inventive embodiments, which carry out following a series of experiments, to be proved：
The embodiment of the present invention have studied catalysis material of the embodiment of the present invention by taking rhodamine B as an example is used for catalytic treatment organic waste
During water process, its degradation effect to organic pollution in water environment, but the embodiment of the present invention is not limited to only to Luo Dan
Bright B works, and other pollutants of degrading can also reach the effect of similar catalytic degradation, for example：Methyl orange, methylene blue and
The Anthraquinones such as reactive brilliant red, quinone imides, the organic pollution of oxa anthracenes and azo.
Photocatalytic degradation is tested：
(1) RhB solution is configured
20mg RhB solid powders are weighed, plus deionized water is configured to 1L RhB solution；
(2) dark adsorption treatment
The BiOCl photochemical catalysts for weighing the preparation of the 50mg embodiment of the present invention are put into the RhB solution that 100ml has been configured, and are surpassed
Sonication 5min is well mixed to solution, is put into reactor and is passed through condensed water, keeps reaction temperature within 20-25 DEG C, black
Magnetic agitation 30min ensures that BiOCl photochemical catalysts reach that adsorption/desorption is put down with RhB solution before visible light exposure again under dark situation
Weighing apparatus.The above-mentioned solution of 1.5ml is pipetted with liquid-transfering gun afterwards, is sampled as dark absorption.
(3) visible light photocatalysis is tested
Photocatalysis test is carried out in the test system voluntarily assembled, it is seen that light source is 618W/m2LED, adjust LED
Lamp height, makes LED at BiOCl-RhB mixed solution liquid levels 9cm；Be passed through condensed water keep reaction temperature 20-25 DEG C with
It is interior, during visible light exposure, magnetic agitation is kept to BiOCl-RhB mixed solutions, at interval of 5min time pipettes
Sampling 1.5ml mixed liquors are put into centrifuge tube and arranged in numerical order in order, until the color of RhB solution is taken off substantially.
(4) absorbance of test sampling sample, investigates catalyst light degradation property.
Sample is put into 12000r/min centrifugations 5min in centrifuge and obtains supernatant, takes 1ml to use light splitting light after diluting 3 times
The absorbance of degree meter (Shanghai instrument Yuan Xi Co., Ltds UV-8000S types ultraviolet-uisible spectrophotometer) test sample.According to
The linear relationship of RhB solution concentrations and absorbance calculates the concentration C of RhB in samplet/C0, compare the photocatalysis feelings of different time
Condition.As a result as shown in Figure 3,4.The change procedure signal that Fig. 3 is BiOCl photocatalyst for degrading RhB prepared by the embodiment of the present invention
Figure.Curve in Fig. 3 from top to bottom is represented respectively：The top curve is not add the situation of system during BiOCl photochemical catalysts, connect down
Come be followed successively by plus during BiOCl photochemical catalysts system situation (reaction time is followed successively by 0,10,30,50,70,100min).
Fig. 4 is that 1-4 of the embodiment of the present invention adds BiOCl photocatalyst for degrading RhB solution prepared by different amounts of starch
Schematic diagram.Found according to experimental data analysis, there is BiOCl photochemical catalysts prepared by the present invention good photocatalysis to live
Property, 100min simulating pollution things RhB clearance can reach 97.1%.In BiOCl photocatalyst for degrading water prepared by the present invention
Dyestuff contaminant, it is simple to operate, effective degraded to rhdamine B can be achieved, degradation rate is high under visible light, and environment is controlled
Reason is significant.In addition, the method for dyestuff is to aquatic organism nonhazardous in BiOCl photocatalyst for degrading water prepared by the present invention
Effect, environmental protection, the problem of secondary pollution is produced to water environment.And BiOCl photocatalytic material can be urged using sunshine
Change dyestuff in degradation water, method is simple to operate, and operating cost is low, adds the economic feasibility of this method.
(5) catalyst cycle performance is tested.
With after RhB solution of being degraded in above-mentioned identical system, catalyst is reclaimed, the RhB for continuing degraded same system is molten
Liquid, circulates five times, compares degradation effect, as shown in Figure 5.It can be seen that BiOCl light prepared by present invention method is urged
Agent shows preferable photocatalysis performance in degraded RhB solution, has good stability in circulation experiment.
Technical scheme in above-mentioned the embodiment of the present application, at least has the following technical effect that or advantage：
The present invention is by controlling Bi (NO3)3Different amounts of starch is added in solution, after the pH value of solution is adjusted to weak acid
Property, to obtain the different sizes with more preferable photocatalytic activity and the BiOCl nano materials of pattern.Preparation method of the present invention is used
The raw material of green safety, method are simple, process is easily operated, can be continuously produced.This method is carrying out the temperature of hydro-thermal reaction
Only 150-160 DEG C, energy consumption is less.In addition, remaining reagent for being used in catalyst process is prepared, such as water, chloride and alkali
Liquid, acid solution etc., are reagent cheap and easy to get, environmentally safe, therefore embody the environment-friendly of this catalyst well
Property.And this method step simple and convenient during preparation, complex this step of regulation pH value, and without being adjusted
Strong acid or highly basic are saved, only with being adjusted to faintly acid.
Flower-shaped, spherical morphology the BiOCl nano materials being prepared by the method for the present invention have compared with other BiOCl materials
There is high, the higher specific surface area of crystallinity, can be adsorbed more while more reactivity sites can be provided
Many pollutants, are conducive to improving the photocatalysis efficiency of photochemical catalyst.By active testing under visible light, obtained result
Show that the BiOCl nano materials for preparing and going out by the present invention have good stability and repeatable usability, with fine
Photocatalytic activity and economy.
, but those skilled in the art once know basic creation although preferred embodiments of the present invention have been described
Property concept, then can make other change and modification to these embodiments.So, appended claims are intended to be construed to include excellent
Select embodiment and fall into having altered and changing for the scope of the invention.Obviously, those skilled in the art can be to the present invention
Carry out various changes and modification without departing from the spirit and scope of the present invention.So, if these modifications and variations of the present invention
Belong within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to exist comprising these changes and modification
It is interior.
Claims (10)
1. the preparation method of flower-shaped and spherical BiOCl photochemical catalysts, it is characterised in that：Methods described comprises the following steps：
(1) bismuth nitrate and starch are added in water, stirs, obtains the mixed liquor of bismuth-containing；The matter of the bismuth nitrate and starch
Measuring amount ratio is：(0.3-5)：1；
(2) chloride solution is added dropwise in the mixed liquor that step (1) is obtained, stirs, the presoma for obtaining bismuth-containing is molten
Liquid；
(3) pH value of the precursor solution for the bismuth-containing for being obtained step (2) using alkaline solution and acid solution is adjusted to 5.0-6.5, stirs
Mix and be formed uniformly reactant；
(4) step (3) gained reactant is subjected to reaction 24-30h at 150-160 DEG C, precipitated；
(5) washing of precipitate for obtaining step (4), dries, obtains flower-shaped and spherical morphology BiOCl powders.
2. the preparation method of according to claim 1 flower-shaped and spherical BiOCl photochemical catalysts, it is characterised in that：The step
Suddenly in (1), the quality amount ratio of the bismuth nitrate and starch is：(1.5-5)：1.
3. the preparation method of according to claim 1 flower-shaped and spherical BiOCl photochemical catalysts, it is characterised in that：The step
Suddenly in (2), the chloride is selected from potassium chloride, sodium chloride and ammonium chloride, the mole dosage ratio of the bismuth nitrate and chloride
For：1：(1-2).
4. the preparation method of according to claim 1 flower-shaped and spherical BiOCl photochemical catalysts, it is characterised in that：The step
Suddenly in (3), the alkaline solution is selected from potassium hydroxide, sodium hydroxide and ammoniacal liquor, and the acid solution is selected from nitric acid.
5. the preparation method of according to claim 1 flower-shaped and spherical BiOCl photochemical catalysts, it is characterised in that：The step
Suddenly in (3), the pH value of the bismuth-containing precursor solution mixed liquor is adjusted to 6.0.
6. the preparation method of according to claim 1 flower-shaped and spherical BiOCl photochemical catalysts, it is characterised in that：The step
Suddenly in (4), reactant is subjected to reaction 24h at 160 DEG C.
7. BiOCl photochemical catalysts made from the preparation method as described in claim any one of 1-6, it is characterised in that：It is described
BiOCl photochemical catalysts are the flower-shaped and chondritic that micro-nano of BiOCl is stacked into, and the thickness of described micro-nano is 25-
30nm。
8. the application of BiOCl photochemical catalysts made from the preparation method as described in claim any one of 1-6, it is characterised in that：
The BiOCl photochemical catalysts can be applied to degradable organic pollutant in organic wastewater under the irradiation of visible ray or ultraviolet light.
9. the application of BiOCl photochemical catalysts according to claim 8, it is characterised in that：The organic pollution is selected from sieve
Red bright B, methyl orange, methylene blue and reactive brilliant red.
10. the application of BiOCl photochemical catalysts according to claim 8, it is characterised in that：The organic pollution with
The quality usage ratio of BiOCl photochemical catalysts is 1:(20-30).
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| CN108722462A (en) * | 2018-04-27 | 2018-11-02 | 华中师范大学 | A kind of ammonia modification chlorine oxygen bismuth micron ball and preparation method thereof |
| CN109261174A (en) * | 2018-11-14 | 2019-01-25 | 哈尔滨理工大学 | A kind of BiOCl micron ring and preparation method |
| CN110433830A (en) * | 2019-08-19 | 2019-11-12 | 上海电力大学 | A kind of preparation method being modified flower-shaped bismuth oxyiodide photochemical catalyst |
| CN111185202A (en) * | 2020-03-18 | 2020-05-22 | 辽宁石油化工大学 | Three-dimensional flower-shaped Bi12O17Cl2Method for preparing photocatalyst |
| CN111686767A (en) * | 2020-05-21 | 2020-09-22 | 华南理工大学 | Microspherical Bi3O4Preparation and application of Cl/BiOI compound |
| CN113461054A (en) * | 2021-07-28 | 2021-10-01 | 中国科学院上海硅酸盐研究所 | BiOCl powder and preparation method and application thereof |
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| CN109261174A (en) * | 2018-11-14 | 2019-01-25 | 哈尔滨理工大学 | A kind of BiOCl micron ring and preparation method |
| CN109261174B (en) * | 2018-11-14 | 2021-04-02 | 哈尔滨理工大学 | BiOCl micron ring and preparation method thereof |
| CN110433830A (en) * | 2019-08-19 | 2019-11-12 | 上海电力大学 | A kind of preparation method being modified flower-shaped bismuth oxyiodide photochemical catalyst |
| CN111185202A (en) * | 2020-03-18 | 2020-05-22 | 辽宁石油化工大学 | Three-dimensional flower-shaped Bi12O17Cl2Method for preparing photocatalyst |
| CN111185202B (en) * | 2020-03-18 | 2022-11-29 | 辽宁石油化工大学 | Three-dimensional flower-shaped Bi 12 O 17 Cl 2 Method for preparing photocatalyst |
| CN111686767A (en) * | 2020-05-21 | 2020-09-22 | 华南理工大学 | Microspherical Bi3O4Preparation and application of Cl/BiOI compound |
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Application publication date: 20170804 |