CN109261174B - BiOCl micron ring and preparation method thereof - Google Patents
BiOCl micron ring and preparation method thereof Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 43
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 39
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 abstract 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 abstract 1
- 230000001954 sterilising effect Effects 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 29
- 239000011941 photocatalyst Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000001105 regulatory effect Effects 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
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- -1 bromine ions Chemical class 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
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- 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
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Abstract
The invention discloses a BiOCl micron ring and a preparation method thereof. The material prepared by the invention can be used in the fields of photocatalytic energy conversion, photocatalytic solar energy purification, photocatalytic sterilization and the like. The preparation method comprises the steps of firstly dissolving bismuth nitrate powder into a mixed solution of nitric acid and citric acid, then adjusting the pH value of the solution, carrying out hydrothermal reaction on the solution to obtain BiOBr powder with an exposed (010) surface, and replacing bromide ions in the BiOBr powder with chloride ions in added NaCl to obtain the BiOCl micron ring. The invention has the advantages of simple operation, low preparation temperature, mild reaction conditions and the like, and provides a rapid preparation method for the BiOCl micron ring.
Description
Technical Field
The invention belongs to the technical field of inorganic synthesis, and relates to a BiOCl micron ring and a preparation method thereof.
Background
The photocatalysis technology has the advantages of low energy consumption, mild purification conditions, no secondary pollution and the like for purifying organic pollutants. The semiconductor photocatalytic oxidation technology utilizes photo-generated electron hole pairs generated by illumination to oxidize and degrade organic pollutants, and has high reaction efficiency and low cost, so the semiconductor photocatalytic oxidation technology is valued by researchers. Bismuth oxychloride (BiOCl) is a photocatalyst developed in recent years, is cheap, readily available and environmentally friendly, and is a potential photocatalyst material, and the key of the photocatalytic technology is the photocatalyst, so that the preparation of the photocatalyst is very critical.
BiOCl is tetragonal phase, and a flaky and micron spherical BiOCl powder material can be obtained through regulating and controlling process parameters. For example, Li or the like in Bi (NO)3)3•5H2O, KCl is used as a main raw material, and the BiOCl micron sphere is obtained after hydrothermal reaction for 12 h at 160 ℃ under the regulation of ethylene glycol (Environ. Sci. Polluti. Res., 2017, 24: 9556-9565). Jiang et al Bi (NO)3)3•5H2O, KCl is used as a main raw material, and the pH value of the solution is adjusted to 6.0 by NaOH solution, thus obtaining the BiOCl nano-sheet (J. Am. chem. Soc., 2012, 134: 4473-one 4476). Is provided withThe BiOCl morphological characteristics are counted and enriched, and the purpose of regulating and controlling the performance of the BiOCl can be achieved. Based on the method, the prepared BiOBr nanosheet is used as a main raw material, and the bromine ions in the BiOBr are replaced by the chloride ions through the solubility product difference of the BiOBr and the BiOCl to obtain the BiOCl micron ring. The invention provides a new method for developing BiOCl materials with morphological characteristics, low cost and high efficiency.
Disclosure of Invention
The invention aims to provide a BiOCl micron ring and a preparation method thereof.
The above purpose is realized by the following technical scheme:
a BiOCl micron ring and a preparation method thereof, the preparation method comprises the following steps:
step 1, adding a certain amount of Bi (NO)3)3•5H2O is dissolved in a mixed solution of nitric acid and citric acid, wherein Bi (NO)3)3•5H2The concentration of O is 0.2-0.5 mol/L, and the molar ratio of nitric acid to citric acid is 2: (1-2), adding 0.2-0.5 mol/L KBr solution, wherein Bi (NO)3)3•5H2The mol ratio of O to KBr is 1:1, and then the pH value is adjusted by NaOH solution until the pH value of the mixed solution is 5.5-6.0;
step 2, putting the solution obtained in the step 1 into a reaction kettle, carrying out hydrothermal reaction at 140-180 ℃ for 14-20 hours, filtering, and cleaning to obtain (010) surface exposed BiOBr powder;
step 3, dispersing the powder in the step 2 into 100mL of deionized water, adding 0.02-0.05 mol/L of NaCl solution, keeping the molar ratio of BiOBr to the NaCl solution at 1 (3-10), then continuously stirring for 30-120 min, and keeping the temperature of the solution at 60-95 ℃;
and 4, repeatedly washing the powder obtained in the step 3 by using deionized water to obtain the BiOCl micron ring.
Description of the drawings:
FIG. 1 is an X-ray diffraction pattern of a BiOCl minicircle of example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a BiOCl microring in example 1 of the present invention;
FIG. 3 is a representation of the photocatalytic performance of BiOCl minicycles in inventive example 1 versus BiOCl in inventive example 3.
Has the advantages that:
1. the annular BiOCl photocatalyst obtained according to the invention has wide development prospect in the aspects of photocatalytic pollutant treatment, photocatalytic air purification and the like.
The tetragonal phase BiOCl particles are annular, and the photocatalytic performance of the annular tetragonal phase BiOCl is greatly improved compared with that of the conventional tetragonal phase BiOCl.
The specific implementation mode is as follows:
example 1:
step 1, adding a certain amount of Bi (NO)3)3•5H2O is dissolved in a mixed solution of nitric acid and citric acid, wherein Bi (NO)3)3•5H2The concentration of O is 0.3 mol/L, the molar ratio of nitric acid to citric acid is 2:1, and then 0.2-0.5 mol/L KBr solution is added, wherein Bi (NO)3)3•5H2Adjusting the pH value of the mixed solution to 6.0 by using NaOH solution until the molar ratio of O to KBr is 1: 1;
step 2, putting the solution obtained in the step 1 into a reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 14 hours, filtering and cleaning the precipitate to obtain (010) surface exposed BiOBr powder;
step 3, dispersing the powder in the step 2 into 100mL of deionized water, adding 0.03 mol/L of NaCl solution, keeping the molar ratio of BiOBr to NaCl solution at 1:8, then continuing stirring for 60min, and keeping the temperature of the solution at 80 ℃;
and 4, cleaning the powder obtained in the step 3 by using deionized water, and drying to obtain the BiOCl micron ring.
Example 2:
step 1, adding a certain amount of Bi (NO)3)3•5H2O is dissolved in the mixed solution of nitric acid and citric acid, Bi (NO)3)3•5H2The concentration of O is 0.4 mol/L, wherein the molar ratio of nitric acid to citric acid is 2:1, then adding 0.2-0.5 mol/L KBr solution, wherein Bi (NO)3)3•5H2Adjusting the pH value of the mixed solution to 6.0 by using NaOH solution until the molar ratio of O to KBr is 1: 1;
step 2, putting the solution obtained in the step 1 into a reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 18 hours, filtering and cleaning the precipitate to obtain BiOBr powder with an exposed (010) surface;
step 3, dispersing the powder in the step 2 into 100mL of deionized water, adding 0.05mol/L of NaCl solution, keeping the molar ratio of BiOBr to NaCl solution at 1:7, then continuing stirring for 70min, and keeping the temperature of the solution at 80 ℃;
and 4, repeatedly washing the powder obtained in the step 3 by using deionized water to obtain the BiOCl micron ring.
Example 3:
step 1, adding a certain amount of Bi (NO)3)3•5H2Dissolving O in mixed solution of nitric acid and citric acid, wherein Bi (NO)3)3•5H2The concentration of O is 0.3 mol/L, the molar ratio of nitric acid to citric acid is 2:1, and then 0.2-0.5 mol/L NaCl solution and Bi (NO) are added3)3•5H2Adjusting the pH value with NaOH solution until the pH value of the mixed solution is 6.0, wherein the molar ratio of O to NaCl is 1: 1;
and 2, putting the solution obtained in the step 1 into a reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 14 hours, filtering the precipitate, and cleaning to obtain BiOCl powder.
Application example 1
0.1g of the BiOCl microring obtained in example 1 and 0.1g of the BiOCl nanosheet obtained in example 3 were taken and mixed with a rhodamine solution (100 mL, 20 mg. L) respectively-1) And (3) mixing, stirring for 30 minutes in the dark, starting a xenon lamp, taking a certain volume of reaction liquid every 30 minutes, testing the absorbance of the solution after centrifugation and filtration, and testing the decolorization rate of the photocatalyst on rhodamine by using the change of the absorbance.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, and those skilled in the art can make various modifications without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (2)
1. A BiOCl micro-ring is characterized in that the BiOCl micro-ring consists of tetragonal phase BiOCl, the micro-morphology of powder particles is annular, and the BiOCl micro-ring is prepared by the following steps:
step 1, preparing nitric acid and citric acid into solution according to a certain proportion, and adding a certain amount of Bi (NO)3) 3•5H2Dissolving O in the solution, and then adding 0.2-0.5 mol/L KBr solution, wherein the molar ratio of nitric acid to citric acid is 2 (1-2), and Bi (NO)3) 3•5H2O concentration of 0.2 to 0.5mol/L, Bi (NO)3) 3•5H2Adjusting the molar ratio of O to KBr to be 1:1, and then adjusting the pH value by using a NaOH solution until the pH value of the mixed solution is 5.5-6.0;
step 2, putting the solution obtained in the step 1 into a reaction kettle, carrying out hydrothermal reaction for 14-20 hours at the temperature of 140-180 ℃, filtering and cleaning the precipitate to obtain (010) face exposed BiOBr powder;
step 3, dispersing the powder in the step 2 into 100mL of deionized water, adding 0.02-0.05 mol/L of NaCl solution, keeping the molar ratio of BiOBr to NaCl solution at 1 (3-10), and then continuously stirring for 30-120 min, keeping the temperature of the solution at 60-95 ℃;
and 4, repeatedly washing the powder obtained in the step 3 by using deionized water to obtain the BiOCl micron ring.
2. A preparation method of BiOCl micron ring is characterized in that the prepared product consists of tetragonal phase BiOCl, the micro-morphology of powder particles is annular, and the preparation process comprises the following steps:
step 1, preparing nitric acid and citric acid into solution according to a certain proportion, and adding a certain amount of Bi (NO)3) 3•5H2Dissolving O in the solution, and then adding 0.2-0.5 mol/L KBr solution, wherein the nitric acid and the KBr solutionThe molar ratio of citric acid is 2 (1-2), and Bi (NO)3) 3•5H2O concentration of 0.2 to 0.5mol/L, Bi (NO)3) 3•5H2Adjusting the molar ratio of O to KBr to be 1:1, and then adjusting the pH value by using a NaOH solution until the pH value of the mixed solution is 5.5-6.0;
step 2, putting the solution obtained in the step 1 into a reaction kettle, carrying out hydrothermal reaction for 14-20 hours at the temperature of 140-180 ℃, filtering and cleaning the precipitate to obtain (010) face exposed BiOBr powder;
step 3, dispersing the powder in the step 2 into 100mL of deionized water, adding 0.02-0.05 mol/L of NaCl solution, keeping the molar ratio of BiOBr to NaCl solution at 1 (3-10), and then continuously stirring for 30-120 min, keeping the temperature of the solution at 60-95 ℃;
and 4, repeatedly washing the powder obtained in the step 3 by using deionized water to obtain the BiOCl micron ring.
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|---|---|---|---|---|
| CN103055903A (en) * | 2013-01-21 | 2013-04-24 | 武汉理工大学 | Preparation method of visible light catalytic material with adjustable BiOI-AgI spherical solid solution |
| CN103708424A (en) * | 2013-12-18 | 2014-04-09 | 江苏大学 | Preparation method of {001} crystal surface-exposed BioBr square nanosheet |
| CN107008462A (en) * | 2017-04-27 | 2017-08-04 | 武汉纺织大学 | The preparation method of flower-shaped and spherical BiOCl photochemical catalysts and obtained photochemical catalyst and application |
| CN107930653A (en) * | 2017-11-29 | 2018-04-20 | 哈尔滨理工大学 | A kind of preparation method rich in low price bismuth, the chlorine bismuth oxybromide of preferred orientation |
| CN108031479A (en) * | 2017-10-30 | 2018-05-15 | 哈尔滨理工大学 | A kind of preparation method of beta bismuth oxide-bismoclite |
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Patent Citations (5)
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|---|---|---|---|---|
| CN103055903A (en) * | 2013-01-21 | 2013-04-24 | 武汉理工大学 | Preparation method of visible light catalytic material with adjustable BiOI-AgI spherical solid solution |
| CN103708424A (en) * | 2013-12-18 | 2014-04-09 | 江苏大学 | Preparation method of {001} crystal surface-exposed BioBr square nanosheet |
| CN107008462A (en) * | 2017-04-27 | 2017-08-04 | 武汉纺织大学 | The preparation method of flower-shaped and spherical BiOCl photochemical catalysts and obtained photochemical catalyst and application |
| CN108031479A (en) * | 2017-10-30 | 2018-05-15 | 哈尔滨理工大学 | A kind of preparation method of beta bismuth oxide-bismoclite |
| CN107930653A (en) * | 2017-11-29 | 2018-04-20 | 哈尔滨理工大学 | A kind of preparation method rich in low price bismuth, the chlorine bismuth oxybromide of preferred orientation |
Non-Patent Citations (1)
| Title |
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| "Synthesis and Facet-Dependent Photoreactivity of BiOCl Single-Crystalline Nanosheets";Jing Jiang et al.;《J. Am. Chem. Soc.》;20120314;第134卷(第10期);第4473-4476页 * |
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