CN108502926B - BiOCl nano-rings and its synthetic method - Google Patents
BiOCl nano-rings and its synthetic method Download PDFInfo
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- CN108502926B CN108502926B CN201810460435.2A CN201810460435A CN108502926B CN 108502926 B CN108502926 B CN 108502926B CN 201810460435 A CN201810460435 A CN 201810460435A CN 108502926 B CN108502926 B CN 108502926B
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000002063 nanoring Substances 0.000 title claims abstract description 76
- 238000010189 synthetic method Methods 0.000 title claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 76
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 47
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 37
- 239000007864 aqueous solution Substances 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 17
- 238000005530 etching Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052783 alkali metal Inorganic materials 0.000 claims description 13
- 150000001340 alkali metals Chemical class 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000001103 potassium chloride Substances 0.000 claims description 11
- 235000011164 potassium chloride Nutrition 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- FIMTUWGINXDGCK-UHFFFAOYSA-H dibismuth;oxalate Chemical compound [Bi+3].[Bi+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O FIMTUWGINXDGCK-UHFFFAOYSA-H 0.000 claims description 4
- 230000002045 lasting effect Effects 0.000 claims description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 31
- 230000015572 biosynthetic process Effects 0.000 abstract description 11
- 238000003786 synthesis reaction Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract 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 description 17
- 229940012189 methyl orange Drugs 0.000 description 17
- 230000015556 catabolic process Effects 0.000 description 15
- 238000006731 degradation reaction Methods 0.000 description 15
- 238000007146 photocatalysis Methods 0.000 description 14
- 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 14
- 229940043267 rhodamine b Drugs 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 230000002950 deficient Effects 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 7
- 125000004122 cyclic group Chemical group 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 238000005286 illumination Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- -1 hydrogen ions Chemical class 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 229920002562 Polyethylene Glycol 3350 Polymers 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 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
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical group O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
- QGWDKKHSDXWPET-UHFFFAOYSA-E pentabismuth;oxygen(2-);nonahydroxide;tetranitrate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[O-2].[Bi+3].[Bi+3].[Bi+3].[Bi+3].[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QGWDKKHSDXWPET-UHFFFAOYSA-E 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention belongs to field of nanometer material technology, a kind of BiOCl nano-rings and its synthetic method are specifically disclosed, the synthetic method will be the following steps are included: (1) will contain Bi3+、Cl‑Heating reaction is carried out with the aqueous solution of polyethylene glycol, obtains BiOCl nanometer sheet;(2) BiOCl nanometer sheet is etched in acid solution.BiOCl nano-rings can be obtained in synthetic method of the invention, not only filled up BiOCl nano-rings synthesis aspect blank, but also obtained BiOCl nano-rings compared with Traditional center not apertures BiOCl nanometer sheet have higher photocatalytic activity.Moreover, the synthetic method step is simple, easily controllable, obtained BiOCl nano-rings regular appearance, not only scientific research value with higher, photocatalytic applications value also with higher.
Description
Technical field
The present invention relates to nano materials, and in particular, to a kind of BiOCl nano-rings and its synthetic method.
Background technique
Fossil fuel in the links that we live all be it is indispensable, the non-renewable and reserves that gradually decrease are
Also along with serious environmental pollution when being caused energy crisis, and being consumed.Currently, Photocatalitic Technique of Semiconductor is considered
It is to solve the more promising technology of both of these problems.
In recent years, the controlledly synthesis of the new pattern of BiOCl and its photocatalytic activity research cause the great interest of people, main
It wants the reason is that BiOCl is as important conductor photocatalysis material a kind of in bismuth based compound, by bismuth oxygen layer [Bi2O2]2+With it is double
[Cl]-Sheath is alternately arranged along c-axis direction and constitutes unique layer structure, and this layer structure can be in [Bi2O2]2+Layer and
[Cl]-The separation that internal electric field is conducive to photo-generate electron-hole pair is formed between layer, to have high catalytic performance.
But report at present it is mostly be BiOCl nanometer sheet, hierarchical structure patterns and their photocatalysis such as micron ball
Activity.And cyclic annular nanometer sheet (also referred to as nano-rings) passes through because its center is easy to fluid, is on the one hand conducive to point of nano material
It dissipates, convenient for application;On the other hand it also will increase and the contact area of the fluid containing pollutant, the property of promotion BiOCl nanometer sheet
Energy.However, cause nano-rings synthesis difficult because material such as forward grows at the reasons to nanometer sheet in the synthesis process, it is therefore, existing at present
Having technology does not have the report of BiOCl ring-type nanometer sheet.
Summary of the invention
The object of the present invention is to provide a kind of BiOCl nano-rings and its synthetic method, synthetic method of the invention is available
BiOCl nano-rings have not only filled up the blank of BiOCl nano-rings synthesis aspect, but also in obtained BiOCl nano-rings relatively routine
The heart not apertures BiOCl nanometer sheet have higher photocatalytic activity.Moreover, the synthetic method step is simple, is easy to control
It makes, obtained BiOCl nano-rings regular appearance, not only scientific research value with higher, photocatalytic applications valence also with higher
Value.
To achieve the goals above, the present invention provides a kind of synthetic method of BiOCl nano-rings, the synthetic method packets
It includes following steps: (1) Bi will be contained3+、Cl-Heating reaction is carried out with the aqueous solution of polyethylene glycol, obtains BiOCl nanometer sheet;(2)
BiOCl nanometer sheet is etched in acid solution;Wherein, Cl is provided-Substance be alkali metal chlorizated salt;Wherein, acid solution is that nitric acid is molten
The mixed solution of liquid, sulfuric acid solution or nitric acid and sulfuric acid.
The present invention also provides a kind of BiOCl nano-rings synthesized according to previously described synthetic method.
Through the above technical solutions, the present invention has obtained BiOCl nano-rings, BiOCl nano-rings synthesis side has not only been filled up
The blank in face, and obtained BiOCl nano-rings are living with higher photocatalysis compared with the BiOCl nanometer sheet of Traditional center not apertures
Property.Moreover, the synthetic method step is simple, easily controllable, obtained BiOCl nano-rings regular appearance, not only have compared with
High scientific research value, photocatalytic applications value also with higher.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is influence of the different time etching to BiOCl nano-rings: (a) the SEM figure of 3h etching, (b) SEM of 6h etching
Figure;(c) the TEM figure of 6h etching;(d) different time etches corresponding XRD diagram;
Fig. 2 is influence of the PEG of different molecular weight to BiOCl nanometer sheet: (a) PEG-3350, (b) PEG-4000, (c)
PEG-6000, (d) PEG-10000;
Fig. 3 is influence of the different acid solutions to etching BiOCl nanometer sheet: (a) HF solution, (b) acetic acid solution, (c) sulfuric acid is molten
Liquid, (d) nitric acid solution;
Influence of the difference chlorine source Fig. 4 to synthesis BiOCl nanometer sheet: (a) KCl, (b) HCl, (c) CTAC, (d) NaCl;
Fig. 5 be different amounts PEG to synthesis BiOCl nanometer sheet influence: (a) 0.05g, (b) 0.1g, (c) 0.15g,
(d)0.2g;
Fig. 6 is the photocatalysis analysis chart in application examples 1: (a) degradation curve of MO (10mg/L);(b) with BiOCl nano-rings
When for photochemical catalyst, the UV-visible spectrum of MO solution;
Fig. 7 is the photocatalysis analysis chart in application examples 2: (a) degradation curve of MO (30mg/L);(b) with BiOCl nano-rings
When for photochemical catalyst, the UV-visible spectrum of MO solution;
Fig. 8 is the photocatalysis analysis chart in application examples 3: (a) degradation curve of RhB (10mg/L);(b) with BiOCl nanometers
When ring is photochemical catalyst, the UV-visible spectrum of RhB solution;
Fig. 9 is the photocatalysis analysis chart in application examples 4: (a) degradation curve of RhB (30mg/L);(b) with BiOCl nanometers
When ring is photochemical catalyst, the UV-visible spectrum of RhB solution;
Figure 10 is the degradation curve of phenol (10mg/L) in the presence of the different catalysts in application examples 5;
Figure 11 is BiOCl nano-rings in application examples 6 to 10mg/L Photocatalytic Degradation of Methyl Orange recycling rate of waterused figure.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of synthetic method of BiOCl nano-rings, the synthetic method will be the following steps are included: (1) will
Contain Bi3+、Cl-Heating reaction is carried out with the aqueous solution of polyethylene glycol, obtains BiOCl nanometer sheet;(2) by BiOCl nanometer sheet in
It is etched in acid solution;Wherein, Cl is provided-Substance be alkali metal chlorizated salt;Wherein, acid solution is nitric acid solution, sulfuric acid solution or nitre
The mixed solution of acid and sulfuric acid.
Through the above technical solutions, the defective BiOCl nanometer sheet in center can be obtained in step (1) in the present invention, by step
Suddenly (2), the defective continuous expansion in the center of BiOCl nanometer sheet simultaneously penetrate, and obtain BiOCl nano-rings.The BiOCl that the present invention obtains
Nano-rings have not only filled up the blank of BiOCl nano-rings synthesis aspect, but also obtained BiOCl nano-rings are not compared with Traditional center
The BiOCl nanometer sheet of apertures has higher photocatalytic activity.Moreover, the synthetic method step is simple, easily controllable, obtains
The BiOCl nano-rings regular appearance arrived, not only scientific research value with higher, photocatalytic applications also with higher are worth.
In the above-mentioned technical solutions, for Bi in aqueous solution3+And Cl-The ratio between the amount of substance, can in a wider range into
Row adjustment, as long as meeting the requirement of above-mentioned technical proposal, can be obtained target BiOCl nano-rings.It is a kind of more excellent in the present invention
In the embodiment of choosing, in order to obtain the defective nanometer sheet in center after step (1) and further obtain regular appearance
BiOCl nano-rings improve combined coefficient, it is preferable that Bi in aqueous solution3+And Cl-The ratio between the amount of substance be 1:0.8-1.2.
Further, for Bi in aqueous solution3+Concentration, in above-mentioned Bi3+And Cl-The feelings that determine of the ratio between the amount of substance
It under condition, can be adjusted in a wider range, in order to obtain the BiOCl nano-rings of regular appearance, improve combined coefficient, preferably
Ground, Bi in aqueous solution3+Concentration be 20-50mmol/L.
Similarly, it for the additive amount of polyethylene glycol, can be adjusted in a wider range, it has been investigated that, with poly- second
The increase of glycol dosage has various sizes of nanometer sheet to coexist, but the influence to the thickness and central defect of nanometer sheet is unobvious.
In order to reduce synthesis cost, combined coefficient is improved, it is preferable that in aqueous solution: the Bi relative to 1mmol3+, the quality of polyethylene glycol
Content is 0.05-0.1g.
In addition, can be adjusted in a wider range for the condition of heating reaction, regular appearance in order to obtain
BiOCl nano-rings improve combined coefficient, it is preferable that it is 140-180 DEG C that the condition for heating reaction, which includes: temperature,.
Certainly, it for the time of heating reaction, can be adjusted in a wider range, in order to obtain regular appearance
BiOCl nano-rings improve combined coefficient, it is preferable that the time for heating reaction is 8-15h.
Under the premise of acid solution is the mixed solution of nitric acid solution, sulfuric acid solution or nitric acid and sulfuric acid, for H in acid solution+
Concentration, can be adjusted in a wider range, in order to obtain the BiOCl nano-rings of regular appearance, improve combined coefficient, preferably
Ground, H in acid solution+Concentration be 0.8-1.5mol/L.
Certainly, it for the dosage of acid solution, can be adjusted in a wider range, in order to improve reaction efficiency, it is preferable that phase
For 1g BiOCl nanometer sheet, the dosage of acid solution is 100-600mL.
Moreover, it for etch period, can be adjusted in a wider range, in order to obtain the nanometer of regular appearance
Ring, it is preferable that etch period 1-8h.
It is further preferred that BiOCl nano-rings of regular appearance in order to obtain, it is preferable that etch period 3-6h.
It for the operating condition of etching, can adjust in a wider range, surface can be used by the nanometer sheet in step (1)
It coats the various ways such as acid solution, immersion to carry out, in a kind of preferred embodiment of the present invention, in order to improve etching efficiency and obtain
To the nano-rings of regular appearance, it is preferable that the specific steps of etching include: by BiOCl nanometer sheet ultrasonic disperse into acid solution, hold
Continuous stirring.
In technical solution above, for containing Bi in step (1)3+、Cl-It was formed with the aqueous solution of polyethylene glycol
Journey can be adjusted in a wider range, such as can also will provide Bi directly by material dissolution in a water3+Substance,
Alkali metal chlorizated salt and polyethylene glycol difference are soluble in water, then three is mixed, and can also dissolve, then remix two-by-two,
Realize the present invention.Certainly for mixed process, the present invention is also not required, and can directly be toppled over, and can also be added dropwise, and can be achieved
The present invention.
In more preferred embodiment of the invention a kind of, the defective BiOCl nanometer sheet in center in order to obtain, more into
One step is conducive to obtain the BiOCl nano-rings of regular appearance, it is preferable that contains Bi3+、Cl-Pass through with the aqueous solution of polyethylene glycol
Following manner obtains: alkali metal chlorizated salt and polyethylene glycol being pre-dissolved in water, ultrasonic disperse, is then added dropwise to predissolve and mentions
For Bi3+Substance aqueous solution in, mix 20-40min.
Further, Bi is provided with dissolved with the aqueous solution of alkali metal chlorizated salt and polyethylene glycol and predissolve in advance3+Object
The volume ratio of the aqueous solution of matter can be adjusted in a wider range, in order to obtain the defective BiOCl nanometer sheet in center, more into
One step is conducive to obtain the BiOCl nano-rings of regular appearance, it is preferable that in advance dissolved with the water-soluble of alkali metal chlorizated salt and polyethylene glycol
Liquid and predissolve are provided with Bi3+Substance aqueous solution volume ratio be 1:0.8-1.2.
In a kind of preferred embodiment of the present invention, in order to improve reaction efficiency, yield is improved, it is preferable that further include
Product after heating reaction in step (1) is cooled down, the step repeatedly washed and dried with distilled water and/or ethyl alcohol.
In the above-mentioned technical solutions, those skilled in the art are for providing Bi3+Substance can be adjusted in a wider range
It is whole, in order to further make raw material simple and easy to get, it is preferable that provide Bi3+Substance be bismuth nitrate and/or bismuth oxalate.
In the above-mentioned technical solutions, for alkali metal chlorizated salt can there are many selections, such as magnesium chloride, calcium chloride, chlorine
Change aluminium, potassium chloride etc., in order to further make raw material simple and easy to get and improve reaction efficiency and yield, it is preferable that alkali metal chlorination
Salt is at least one of sodium chloride, potassium chloride and lithium chloride.
The number-average molecular weight of polyethylene glycol can be selected in a wider range, through studying, with polyethylene glycol point
The increase of son amount, nanometer sheet become closer to square, but little on the influence of center rejected region, and explanation will obtain nano-rings
Shape structure, the molecular weight of PEG are not major influence factors.In order to further make raw material simple and easy to get and improve reaction efficiency and production
Rate, it is preferable that the number-average molecular weight of polyethylene glycol is 3350-10000.
The present invention also provides a kind of BiOCl nano-rings synthesized according to previously described synthetic method.
Through the above technical solutions, the present invention has obtained BiOCl nano-rings, BiOCl nano-rings synthesis side has not only been filled up
The blank in face, and obtained BiOCl nano-rings are living with higher photocatalysis compared with the BiOCl nanometer sheet of Traditional center not apertures
Property.Moreover, the synthetic method step is simple, easily controllable, obtained BiOCl nano-rings regular appearance, not only have compared with
High scientific research value, photocatalytic applications value also with higher.
The present invention will be described in detail by way of examples below.
Embodiment 1
By 1mmol Bi (NO3)3·5H2O ultrasonic dissolution is labeled as solution A into 15mL distilled water.1mmol KCl is added
Into 15mL distilled water, 0.1g polyethylene glycol (PEG-6000) is added after ultrasonic dissolution, ultrasonic disperse is labeled as B solution.B is molten
Drop is added in solution A, then stirs mixed solution 30 minutes.It is finally transferred in the autoclave of 40mL, 160 DEG C add
Heat 12 hours.After reaction, cooled to room temperature, product distilled water, ethanol washing are dry to constant weight, Product Labeling
For BiOCl-S.
Above-mentioned synthetic product is weighed into 0.03g ultrasonic disperse to 15mL 1molL-1HNO3In solution, continuously stir
6h obtains final product, Product Labeling BiOCl-R.
Embodiment 2
(1) bismuth nitrate, sodium chloride and polyethylene glycol (number-average molecular weight 3350) is soluble in water, Bi will be contained3+、Cl-
140 DEG C of heating reaction 15h are carried out at the aqueous solution of polyethylene glycol, obtain BiOCl nanometer sheet;Bi in aqueous solution3+Concentration be
20mmol/L, Bi in aqueous solution3+And Cl-The ratio between the amount of substance be 1:0.8;Bi relative to 1mmol3+, the matter of polyethylene glycol
Amount content is 0.05g;
Product after heating reaction in step (1) is cooled down, is repeatedly washed with distilled water and ethyl alcohol and dry;
(2) lasting to stir by BiOCl nanometer sheet ultrasonic disperse in the nitric acid solution of 0.8mol/L, etch 3h;Relative to
1g BiOCl nanometer sheet, the dosage of nitric acid solution are 100mL.
Embodiment 3
(1) bismuth nitrate, potassium chloride and polyethylene glycol (number-average molecular weight 10000) is soluble in water, Bi will be contained3+、Cl-
180 DEG C of heating reaction 8h are carried out at the aqueous solution of polyethylene glycol, obtain BiOCl nanometer sheet;Bi in aqueous solution3+Concentration be
50mmol/L, Bi in aqueous solution3+And Cl-The ratio between the amount of substance be 1:1.2;Bi relative to 1mmol3+, the matter of polyethylene glycol
Amount content is 0.1g;
Product after heating reaction in step (1) is cooled down, is repeatedly washed with ethyl alcohol and dry;
(2) lasting to stir by BiOCl nanometer sheet ultrasonic disperse in the sulfuric acid solution of 0.5mol/L, etch 8h;Relative to
1g BiOCl nanometer sheet, the dosage of nitric acid solution are 600mL.
Embodiment 4
(1) bismuth oxalate, potassium chloride and polyethylene glycol (number-average molecular weight 4000) is soluble in water, Bi will be contained3+、Cl-
160 DEG C of heating reaction 10h are carried out at the aqueous solution of polyethylene glycol, obtain BiOCl nanometer sheet;Bi in aqueous solution3+Concentration be
30mmol/L, Bi in aqueous solution3+And Cl-The ratio between the amount of substance be 1:1;Bi relative to 1mmol3+, the quality of polyethylene glycol
Content is 0.05g;
Product after heating reaction in step (1) is cooled down, is repeatedly washed with distilled water and dry;
(2) lasting to stir by BiOCl nanometer sheet ultrasonic disperse in the nitric acid solution of 1mol/L, etch 1h;Relative to 1g
BiOCl nanometer sheet, the dosage of nitric acid solution are 300mL.
Embodiment 5
BiOCl nano-rings are synthesized according to the method for embodiment 1, the difference is that etch period is 3h.To embodiment 1 and implement
Gained BiOCl nano-rings are detected in example 5, the result is shown in Figure 1, in Fig. 1: (a) being the BiOCl that etching 3h is obtained in embodiment 5
SEM (scanning electron microscope) figure of nano-rings (b) etches the BiOCl nano-rings SEM figure that 6h is obtained in embodiment 1;(c) in embodiment 1
TEM (transmission electron microscope) figure for the BiOCl nano-rings that etching 6h is obtained;(d) BiOCl nanometers in embodiment 5 and embodiment 1
Ring corresponding XRD (X-ray diffraction) figure, to study influence of the etch period to sample topography.
Found out by SEM figure in Fig. 1, sample is nanometer cyclic structure, and nanometer sheet centre bore is significantly greater than etching after etching 6h
3h.TEM figure further confirms that sample is nanometer cyclic structure.It can be seen that spreading out for etched rear sample from the XRD spectrum provided
Penetrate peak and both correspond to BiOCl (JCPDS No.06-0249), and do not detect other impurity peaks, illustrate synthetic product compared with
It is pure.
Similarly, there is nanometer cyclic structure, warp and BiOCl in the SEM figure of the BiOCl nano-rings in embodiment 2-4
(JCPDS No.06-0249) is compareed, and does not detect other impurity peaks.
It is presumed that reaction mechanism of the invention are as follows: bismuth oxalate, bismuth nitrate are susceptible to hydrolysis in water, generate alkali formula nitric acid
Bismuth, while a large amount of hydrogen ions are discharged, so that solution is in acidic environment.After the polyglycol solution of alkali metal chlorizated salt is added, chlorine
Ion attack basic bismuth nitrate generates BiOCl nucleus.Hydrogen ion is adsorbed on BiOCl nucleus (001) crystalline substance by H-O key in solution
Face, then anisotropic growth is the laminated structure of exposure (001) crystal face.PEG is nonionic surfactant, passes through hydroxyl oxygen
Atom is coordinated with bismuth, is adsorbed on BiOCl (001) crystal face, ultimately forms the defective BiOCl nanometer sheet of (001) crystal face.When
Defective BiOCl is put into HNO3Or in sulfuric acid solution after, thus rejected region is opened due to higher reactivity, etching reaction
Begin.As etch period extends, etching degree is deepened, and gradually forms BiOCl nano-rings.
Embodiment 6
It is prepared according to the method for embodiment 1, the difference is that polyethylene (PEG-6000) is changed to PEG- respectively
3350, PEG-4000, PEG-10000, i.e. PEG number-average molecular weight are respectively 3350,4000,10000.
To the carry out sem analysis for the BiOCl nanometer sheet that step (1) obtains, Fig. 2 is obtained, in Fig. 2: (a) PEG-3350, (b)
PEG-4000, (c) PEG-6000, (d) PEG-10000 study the PEG (3350-10000) of different molecular weight to nanometer sheet with this
The influence at central defect position.As seen from Figure 2, with the increase of PEG molecular weight, nanometer sheet becomes closer to square, but
Center rejected region is influenced little.Illustrate to obtain a nanometer cyclic structure, the molecular weight of PEG is not major influence factors.
After etched, BiOCl nano-rings can be obtained.
Embodiment 7
It is prepared according to the method for embodiment 1, the difference is that the dosage of polyethylene (PEG-6000) is replaced with respectively
0.1g, 0.15g, 0.2g.
To the carry out sem analysis for the BiOCl nanometer sheet that step (1) obtains, Fig. 5 is obtained, the dosage of PEG-6000 point in Fig. 5
Not are as follows: (a) 0.05g, (b) 0.1g, (c) 0.15g, (d) 0.2g, to study influence of the different PEG dosages to nanometer sheet pattern.From
SEM figure can be seen that, as PEG dosage less (0.05g, 0.1g), the more uniform square nanometer sheet of appearance and size can be obtained.
With the increase of dosage, there is various sizes of nanometer sheet to coexist, but the influence to the thickness and central defect of nanometer sheet is unobvious.
After acid solution etches, nano-rings can be obtained.
Comparative example 1
It is prepared according to the synthetic method of embodiment 1, unlike, nitric acid solution is replaced with into HF solution.
Comparative example 2
It is prepared according to the synthetic method of embodiment 1, unlike, nitric acid solution is replaced with into acetic acid solution.
Through carrying out sem analysis to the product in embodiment 1, embodiment 3 and comparative example 1, comparative example 2, different acid solutions are obtained
(unitary acid concentration is 1molL-1, the concentration of sulfuric acid is 0.51molL-1) SEM that nanometer sheet in step (1) etches is schemed,
As a result as shown in Figure 3: (a) acid solution is HF solution, and (b) acid solution is acetic acid solution, and (c) acid solution is sulfuric acid solution, and (d) acid solution is nitre
Acid solution.Fig. 3 gives the BiOCl nanometer sheet under four kinds of different acid etches.It is found by Fig. 3, sample stirs in HF and acetic acid
After 6h, BiOCl nanometer sheet center is not etched, and keeps original state.After stirring 6h in sulfuric acid and nitric acid solution, the central part of piece
Divide and successfully etched, forms cyclic structure.Show that the BiOCl nanometer sheet presoma of this paper can be by sulfuric acid quarter, Nitric acid etching cyclization.
Comparative example 3
It is prepared according to the synthetic method of embodiment 1, unlike, potassium chloride is replaced with into hydrochloric acid.
Comparative example 4
It is prepared according to the synthetic method of embodiment 1, unlike, potassium chloride is replaced with into hexadecyltrimethylammonium chloride
(CTAC)。
Sem analysis, research are carried out through the product to the step (1) in embodiment 1, embodiment 2 and comparative example 3, comparative example 4
Influence using different chlorine sources to nanometer sheet pattern, as a result as shown in figure 4, in Fig. 4: (a) KCl, (b) HCl, (c) CTAC, (d)
NaCl;Find out from SEM figure, the uniform BiOCl nanometer sheet of pattern can be obtained using KCl and NaCl, and piece center is defective;
And when with hydrochloric acid and hexadecyltrimethylammonium chloride (CTAC), then it cannot get the BiOCl that piece center is defective and pattern is uniform
Nanometer sheet.After further acid etching, it cannot be formed and be received with the nanometer sheet that hydrochloric acid and hexadecyltrimethylammonium chloride (CTAC) obtain
Meter Huan.
Application examples 1
In the case where temperature is 30 DEG C and illumination condition by the BiOCl-S and each 0.04g of BiOCl-R in embodiment 1, respectively with
Aqueous solution 40mL containing methyl orange (MO) (10mg/L) is contacted.As a result as shown in fig. 6, the degradation of (a) MO (10mg/L)
Curve;(b) when being photochemical catalyst with BiOCl-R (BiOCl nano-rings), the UV-visible spectrum of MO solution, in figure curve from
The corresponding photocatalysis duration of top to bottm is from short to long;As it can be seen that BiOCl-R nano-rings sample shows higher photocatalytic activity,
100% MO (10mg/L) can be degradable in 2 minutes under sunlight irradiation, and BiOCl-R nano-rings degradation rate is
Twice of nanometer sheet BiOCl-S.
Through detecting, the BiOCl nano-rings in embodiment 1-7 equally have the light of the center of the being substantially better than not nanometer sheet of apertures
Catalytic degradation efficiency.
As it can be seen that BiOCl nano-rings of the invention have preferable photocatalytic activity, photocatalytic pollutant degradation of the invention
Method have the characteristics that it is high-efficient.
Application examples 2
In the case where temperature is 30 DEG C and illumination condition by the BiOCl-S and each 0.04g of BiOCl-R in embodiment 1, respectively with
Aqueous solution 40mL containing methyl orange (MO) (30mg/L) is contacted.As a result as shown in fig. 7, the degradation of (a) MO (30mg/L)
Curve;(b) when being photochemical catalyst with BiOCl-R (BiOCl nano-rings), the UV-visible spectrum of MO solution, in figure curve from
The corresponding photocatalysis duration of top to bottm is from short to long;As it can be seen that BiOCl-R nano-rings sample shows higher photocatalytic activity,
100% MO (30mg/L) can be degradable in 10 minutes under sunlight irradiation, hence it is evident that better than the drop of nanometer sheet BiOCl-S
Solve efficiency.
Application examples 3
In the case where temperature is 30 DEG C and illumination condition by the BiOCl-S and each 0.04g of BiOCl-R in embodiment 1, respectively with
Aqueous solution 40mL containing rhodamine B (RhB) (10mg/L) is contacted.As a result as shown in figure 8, the drop of (a) RhB (10mg/L)
Solution curve;(b) when being photochemical catalyst with BiOCl-R (BiOCl nano-rings), the UV-visible spectrum of RhB solution is bent in figure
Corresponding photocatalysis duration is from short to long from top to bottom for line;It lives as it can be seen that BiOCl-R nano-rings sample shows higher photocatalysis
Property, 100% RhB (10mg/L) can be degradable in 4 minutes under sunlight irradiation, and BiOCl-R nano-rings degradation speed
Rate is 2.5 times of nanometer sheet BiOCl-S.
Application examples 4
In the case where temperature is 30 DEG C and illumination condition by the BiOCl-S and each 0.04g of BiOCl-R in embodiment 1, respectively with
Aqueous solution 40mL containing rhodamine B (RhB) (30mg/L) is contacted.As a result as shown in figure 9, the drop of (a) RhB (30mg/L)
Solution curve;(b) when being photochemical catalyst with BiOCl-R (BiOCl nano-rings), the UV-visible spectrum of RhB solution is bent in figure
Corresponding photocatalysis duration is from short to long from top to bottom for line;It lives as it can be seen that BiOCl-R nano-rings sample shows higher photocatalysis
Property, 100% RhB (10mg/L) can be degradable in 14 minutes under sunlight irradiation, and the catalysis of BiOCl-R nano-rings
Activity is substantially better than BiOCl-S nanometer sheet.
Application examples 5
It is compareed according to catalytic activity of the application examples 1 to BiOCl-R, BiOCl-S nanometer sheet, unlike, MO is become
More 10mg/L phenol, the results are shown in Figure 10, it is seen then that the catalytic activity of BiOCl-R is better than BiOCl-S sample, in 40 minutes
Phenol is by BiOCl-R catalyst degradation 90%.
Through detecting, the BiOCl nano-rings in embodiment 1-7 equally have the light of the center of the being substantially better than not nanometer sheet of apertures
Catalytic degradation efficiency.
As it can be seen that BiOCl nano-rings of the invention have preferable photocatalytic activity, photocatalytic pollutant degradation of the invention
Method have the characteristics that it is high-efficient.
Application examples 6
According to the method for application examples 1, using the BiOCl-R sample in 0.04g embodiment 1 to 40mL10mg/L methyl orange water
Solution photocatalytic degradation carries out repeating to degrade 5 times, the degradation efficiency after observation recycling, as a result as shown in figure 11, it is seen then that
Stability is preferable in the photocatalytic process for the BiOCl nano-rings of BiOCl-R, and recycling rate of waterused is higher.
Five forward and backward diffraction patterns of circulation, discovery are being carried out using X-ray diffraction analysis BiOCl-R photochemical catalyst
BiOCl-R photochemical catalyst recycle for five times forward and backward diffraction maximum change substantially it is small, it is seen then that BiOCl-R photochemical catalyst is urged in light
Stability is preferable during change, and recycling rate of waterused is higher.
Similarly, through detecting, the BiOCl nano-rings in embodiment 1-7 all have that stability is preferable, and recycling rate of waterused is higher
A little.
It can be seen that BiOCl nano-rings of the invention have excellent photocatalytic activity and reusing and it is ring
Shape can reduce use condition, therefore, this product is that there is the efficiency light of practical value to urge as a result, convenient for dispersing in a liquid
Agent.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (14)
1. a kind of synthetic method of BiOCl nano-rings, which is characterized in that the synthetic method the following steps are included:
(1) Bi will be contained3+、Cl-Heating reaction is carried out with the aqueous solution of polyethylene glycol, obtains BiOCl nanometer sheet;
(2) BiOCl nanometer sheet is etched in acid solution;
Wherein, Cl is provided-Substance be alkali metal chlorizated salt;
Wherein, acid solution is the mixed solution of nitric acid solution, sulfuric acid solution or nitric acid and sulfuric acid;
Wherein, H in acid solution+Concentration be 0.8-1.5mol/L;Etch period is 1-8h.
2. synthetic method according to claim 1, wherein Bi in aqueous solution3+And Cl-The ratio between the amount of substance be 1:0.8-
1.2。
3. synthetic method according to claim 1, wherein Bi in aqueous solution3+Concentration be 20-50mmol/L.
4. synthetic method according to claim 2, wherein in aqueous solution: the Bi relative to 1mmol3+, the matter of polyethylene glycol
Amount content is 0.05-0.1g.
5. synthetic method according to claim 1, wherein it is 140-180 DEG C that the condition for heating reaction, which includes: temperature,;
And/or time 8-15h.
6. synthetic method according to claim 1, wherein relative to 1g BiOCl nanometer sheet, the dosage of acid solution is 100-
600mL。
7. synthetic method according to claim 1, wherein etch period 3-6h.
8. synthetic method according to claim 6, wherein the specific steps of etching include: by BiOCl nanometer sheet ultrasound point
It is dissipated in acid solution, it is lasting to stir.
9. synthetic method according to claim 1-8, wherein contain Bi3+、Cl-With the aqueous solution of polyethylene glycol
It obtains in the following manner:
Alkali metal chlorizated salt and polyethylene glycol are pre-dissolved in water, ultrasonic disperse, are then added dropwise to predissolve and are provided with Bi3+Object
In the aqueous solution of matter, 20-40min is mixed.
10. synthetic method according to claim 9, wherein in advance dissolved with the aqueous solution of alkali metal chlorizated salt and polyethylene glycol
Bi is provided with predissolve3+Substance aqueous solution volume ratio be 1:0.8-1.2.
11. synthetic method according to claim 9, wherein further include being carried out to the product after heating reaction in step (1)
It cools down, the step repeatedly washed and dried with distilled water and/or ethyl alcohol.
12. synthetic method according to claim 9, wherein provide Bi3+Substance be bismuth nitrate and/or bismuth oxalate;
And/or alkali metal chlorizated salt is at least one of sodium chloride, potassium chloride and lithium chloride;
And/or the number-average molecular weight of polyethylene glycol is not more than 10000.
13. synthetic method according to claim 12, wherein the number-average molecular weight of polyethylene glycol is 3350-10000.
14. the BiOCl nano-rings that -13 described in any item synthetic methods synthesize according to claim 1.
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