CN107746075B - Preparation method of beta bismuth oxide with strong visible light absorption capacity - Google Patents
Preparation method of beta bismuth oxide with strong visible light absorption capacity Download PDFInfo
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- 230000031700 light absorption Effects 0.000 title claims abstract description 22
- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 20
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 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 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 61
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- 239000002243 precursor Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 29
- 239000011521 glass Substances 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 12
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 230000003197 catalytic effect Effects 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
- 238000002156 mixing Methods 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000011941 photocatalyst Substances 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of beta bismuth oxide with strong visible light absorption capacity. At present, bismuth oxide has problems in relevant catalytic application, for example, the light absorption capability of bismuth oxide is not strong, so that the photocatalytic activity is low, and the photocatalytic activity cannot meet the actual requirement. The preparation method comprises the following steps: respectively mixing the solution containing bismuth nitrate, nitric acid and citric acid with the solution containing citric acid and sodium metaaluminate, adjusting pH value, water bath, drying, grinding, washing, calcining in air atmosphere, and calcining in N2And carrying out heat treatment in the atmosphere to obtain the beta bismuth oxide powder with strong visible light absorption capacity. The invention has simple preparation process and strong visible light absorption capability of the product.
Description
Technical Field
The invention relates to a preparation method of beta bismuth oxide with strong visible light absorption capacity, which is applied to the field of environmental purification.
Background
With the increasing environmental pollution, the photocatalytic technology has attracted much attention in the fields of air purification, sewage treatment, sterilization and the like due to the characteristics of economy, environmental protection and the like, bismuth oxide gradually becomes a research hotspot in the field of novel photocatalyst development in recent years, however, the photocatalytic activity is low, the light absorption capacity is weak, Jiang and the like synthesize β -Bi as the main raw material2O3(J. Mater. chem. A,2015, 3,5119) and patent CN104826623B disclose a bismuth oxide photocatalyst, a preparation method and application thereof, and obtain a nano flower-shaped β -bismuth oxide visible light photocatalyst, the documents and the patent successfully apply a hydrothermal method to prepare a β -bismuth oxide nano material, at present, β -Bi2O3The problems exist in the field of photocatalysis, for example, the weak visible light absorption capacity causes the lower photocatalytic activity of the catalyst, the lower photocatalytic activity is difficult to meet the actual requirement, how to prepare β -Bi with strong visible light response capacity2O3There have been no reports.
Disclosure of Invention
The invention aims to provide a preparation method of beta bismuth oxide with strong visible light absorption capacity.
The above purpose is realized by the following technical scheme:
a preparation method of beta bismuth oxide with strong visible light absorption capacity comprises the following steps:
step 1, 5.145 g of Bi (NO) was charged through a glass container at normal temperature3)3•5H2Dissolving O in HNO with the concentration of 1-4 mol/L3And adding citric acid with the concentration of 0.2-1 mol/L into the solution to form a mixed solution, carrying out magnetic stirring in the dissolving process, continuing stirring for 30-60 min after the chemical substances are completely dissolved, then adjusting the pH value by using a NaOH solution with the concentration of 1-4 mol/L, controlling the dropping speed of the NaOH solution at 0.5-2 mL/min, and gradually testing the pH value until the pH value of the mixed solution is 7.
Step 2, 2mmol of citric acid and 2mmol of Na [ Al (OH) ] were put through a glass vessel at ordinary temperature4]Adding the mixture into deionized water to enable the preparation concentration of the mixture to be 0.2-1 mol/L, simultaneously stirring by magnetic force, and after the mixed solution is completely dissolved, continuing stirring for 30-60 min to generate a solution B.
And 3, dripping the solution A into the solution B through a new glass container at normal temperature, adjusting the pH value of the solution by using a NaOH solution with the concentration of 1-4 mol/L, controlling the dripping speed of the NaOH solution at 0.5-2 mL/min, gradually testing the pH value until the pH value of the solution is 7, and then continuously stirring for 30-60 min to obtain a solution C.
And 4, carrying out water bath on the solution C for 4-15 h at the heating temperature of 70-100 ℃, and stirring by using an electric stirrer in the water bath process, wherein the rotating speed is controlled to be 30-90 rpm, so as to obtain a precursor D.
And 5, drying the precursor D at the heating temperature of 120-160 ℃, controlling the drying time to be 6-12 h, and grinding to obtain a precursor E.
Step 6, repeatedly cleaning the precursor E with deionized water for 3-5 times at normal temperature to remove Na in the precursor E+And Al3+And (4) ionizing, and drying at the heating temperature of 60-120 ℃ for 12-24 h to obtain a precursor F.
Step 7, in the airCalcining the precursor F at 315-370 ℃ for 2-7 h in a gas atmosphere to obtain β -Bi2O3And (3) powder.
Step 8, a certain amount of β -Bi2O3Putting the powder into a vacuum tube furnace, vacuumizing, and introducing N2Maintenance of N2Is at 1 atmosphere and is heat treated at 200-350 ℃ for 2-9 h to obtain black β -Bi with strong visible light absorption capacity2O3And (3) powder.
Has the advantages that:
1. the result of the invention is a photocatalyst, energy shortage and environmental pollution are the major challenges facing human beings at present, and the photocatalytic technology can convert low-density solar energy into high-density chemical energy and directly utilize sunlight to degrade and mineralize various pollutants in water and air. Therefore, the photocatalysis technology has wide development prospect in the aspects of environmental purification and new energy development.
2. Compared with the prior art, the beta bismuth oxide with strong visible light absorption capacity provided by the invention provides a method which is easy to realize industrialization.
3. The beta bismuth oxide with strong visible light absorption capacity prepared by the invention has more obvious enhancement of light absorption capacity compared with pure beta bismuth oxide, the absorption edge of the beta bismuth oxide generates obvious red shift, the enhancement of the visible light absorption capacity improves the probability of generating photo-generated electrons and holes in the photocatalyst, and the increase of the photocatalytic efficiency is promoted.
Description of the drawings:
FIG. 1 is a contrast diagram of X-ray diffraction of beta bismuth oxide with strong visible light absorption ability, which is prepared in example 1 of the present invention.
FIG. 2 is a light absorption spectrum of beta bismuth oxide having a strong visible light absorption ability according to example 1 of the present invention.
The specific implementation mode is as follows:
example 1:
the present invention is further described in detail below by way of specific examples, which will enable one skilled in the art to more fully understand the present invention, but which are not intended to limit the invention in any way.
Step 1, 5.145 g of Bi (NO) was charged through a glass container at normal temperature3)3•5H2Dissolving O in HNO with the concentration of 1.5mol/L3And adding citric acid with the concentration of 0.5mol/L into the solution to form mixed solution, magnetically stirring in the dissolving process, continuously stirring for 30min after the chemical substances are completely dissolved, then adjusting the pH value by using NaOH solution with the concentration of 1.5mol/L, controlling the dropping speed of the NaOH solution at 2mL/min, and gradually testing the pH value until the pH value of the mixed solution is 7.
Step 2, 2mmol of citric acid and 2mmol of Na [ Al (OH) ] were put through a glass vessel at ordinary temperature4]Adding the mixture into deionized water to enable the preparation concentration of the mixture to be 0.5mol/L, simultaneously stirring by magnetic force, and continuing stirring for 30min after the mixed solution is completely dissolved to generate a solution B.
And 3, dripping the solution A into the solution B through a new glass container at normal temperature, adjusting the pH value of the solution by using a NaOH solution with the concentration of 1.5mol/L, controlling the dripping speed of the NaOH solution at 2mL/min, gradually testing the pH value until the pH value of the solution is 7, and then continuing stirring for 30min to obtain a solution C.
And 4, carrying out water bath on the solution C for 14h at the heating temperature of 70 ℃, and stirring by using an electric stirrer in the water bath process, wherein the rotating speed is controlled to be 30rpm, so as to obtain a precursor D.
And 5, drying the precursor D at the heating temperature of 120 ℃, controlling the drying time to be 12h, and grinding to obtain a precursor E.
Step 6, repeatedly cleaning the precursor E with deionized water for 3 times at normal temperature to remove Na in the precursor E+And Al3+And (4) ionizing, and drying for 14h at the heating temperature of 80 ℃ to obtain a precursor F.
Step 7, calcining the precursor F at 355 ℃ for 3h in air atmosphere to obtain β -Bi2O3And (3) powder.
Step 8, a certain amount of β -Bi2O3Putting the powder into a vacuum tube furnace, vacuumizing, and introducing N2Maintenance of N2Is 1 atm, and is heat-treated at 260 ℃ for 6 hours to obtain β -Bi having a strong visible light absorbing ability in black color2O3And (3) powder.
Example 2:
step 1, 5.145 g of Bi (NO) was charged through a glass container at normal temperature3)3•5H2Dissolving O in HNO with the concentration of 2 mol/L3And adding citric acid with the concentration of 0.8 mol/L into the solution to form mixed solution, magnetically stirring in the dissolving process, continuously stirring for 50min after the chemical substances are completely dissolved, then adjusting the pH value by using NaOH solution with the concentration of 2 mol/L, controlling the dropping speed of the NaOH solution at 1.5mL/min, and gradually testing the pH value until the pH value of the mixed solution is 7.
Step 2, 2mmol of citric acid and 2mmol of Na [ Al (OH) ] were put through a glass vessel at ordinary temperature4]Adding the mixture into deionized water to enable the preparation concentration of the mixture to be 0.6 mol/L, simultaneously stirring by magnetic force, and continuing stirring for 40min after the mixed solution is completely dissolved to generate a solution B.
And 3, dripping the solution A into the solution B through a new glass container at normal temperature, adjusting the pH value of the solution by using a 2 mol/L NaOH solution, controlling the dripping speed of the NaOH solution at 1.5mL/min, gradually testing the pH value until the pH value of the solution is 7, and then continuing stirring for 40min to obtain a solution C.
And 4, carrying out water bath on the solution C for 12h at the heating temperature of 80 ℃, and stirring by using an electric stirrer in the water bath process, wherein the rotating speed is controlled to be 40rpm, so as to obtain a precursor D.
And 5, drying the precursor D at the heating temperature of 130 ℃, controlling the drying time to be 10h, and grinding to obtain a precursor E.
Step 6, repeatedly cleaning the precursor E with deionized water for 3 times at normal temperature to remove Na in the precursor E+And Al3+And (4) ionizing, and drying at the heating temperature of 85 ℃ for 12h to obtain a precursor F.
Step 7, calcining the precursor F at 350 ℃ for 4h in air atmosphere to obtain β -Bi2O3And (3) powder.
Step 8, a certain amount of β -Bi2O3Putting the powder into a vacuum tube furnace, vacuumizing, and introducing N2Maintenance of N2Is 1 atm, and is heat-treated at 270 ℃ for 5 hours to obtain β -Bi having a strong visible light absorbing ability in black color2O3And (3) powder.
Example 3:
step 1, 5.145 g of Bi (NO) was charged through a glass container at normal temperature3)3•5H2Dissolving O in HNO with the concentration of 1 mol/L3And adding citric acid with the concentration of 0.5mol/L into the solution to form mixed solution, magnetically stirring in the dissolving process, continuously stirring for 50min after the chemical substances are completely dissolved, then adjusting the pH value by using NaOH solution with the concentration of 1 mol/L, controlling the dropping speed of the NaOH solution at 1.5mL/min, and gradually testing the pH value until the pH value of the mixed solution is 7.
Step 2, 2mmol of citric acid and 2mmol of Na [ Al (OH) ] were put through a glass vessel at ordinary temperature4]Adding the mixture into deionized water to enable the preparation concentration of the mixture to be 0.5mol/L, simultaneously stirring by magnetic force, and continuing stirring for 40min after the mixed solution is completely dissolved to generate a solution B.
And 3, dripping the solution A into the solution B through a new glass container at normal temperature, adjusting the pH value of the solution by using a NaOH solution with the concentration of 1 mol/L, controlling the dripping speed of the NaOH solution at 1mL/min, gradually testing the pH value until the pH value of the solution is 7, and then continuing stirring for 40min to obtain a solution C.
And 4, carrying out water bath on the solution C for 10h at the heating temperature of 90 ℃, and stirring by using an electric stirrer in the water bath process, wherein the rotating speed is controlled to be 40rpm, so as to obtain a precursor D.
And 5, drying the precursor D at the heating temperature of 125 ℃, controlling the drying time to be 13h, and grinding to obtain a precursor E.
Step 6, repeatedly cleaning the precursor E with deionized water for 3 times at normal temperature to remove Na in the precursor E+And Al3+And (4) ionizing, and drying at the heating temperature of 85 ℃ for 12h to obtain a precursor F.
Step 7, calcining the precursor F at 350 ℃ for 4h in air atmosphere to obtain β -Bi2O3And (3) powder.
Step 8, a certain amount of β -Bi2O3Putting the powder into a vacuum tube furnace, vacuumizing, and introducing N2Maintenance of N2Is 1 atm, and is heat-treated at 250 ℃ for 7 hours to obtain β -Bi having strong visible light absorption ability2O3And (3) powder.
Claims (1)
1. A preparation method of beta bismuth oxide with strong visible light absorption capacity is characterized by comprising the following steps:
step 1, 5.145 g of Bi (NO) was charged through a glass container at normal temperature3)35H2O dissolved in HNO at a concentration of 1.5mol/L3Adding citric acid with the concentration of 0.5mol/L into the solution to form a mixed solution, namely solution A, magnetically stirring in the dissolving process, continuously stirring for 30min after the chemical substances are completely dissolved, then adjusting the pH value by using NaOH solution with the concentration of 1.5mol/L, controlling the dropping speed of the NaOH solution at 2mL/min, and gradually testing the pH value until the pH value of the mixed solution is 7;
step 2, 2mmol of citric acid and 2mmol of Na [ Al (OH) ] were put through a glass vessel at ordinary temperature4]Adding the mixture into deionized water to enable the preparation concentration of the mixture to be 0.5mol/L, simultaneously stirring the mixture by magnetic force, and continuing stirring the mixture for 30min after the mixed solution is completely dissolved to generate a solution B;
step 3, dripping the solution A into the solution B through a new glass container at normal temperature, adjusting the pH value of the solution by using a NaOH solution with the concentration of 1.5mol/L, controlling the dripping speed of the NaOH solution at 2mL/min, gradually testing the pH value until the pH value of the solution is 7, and then continuing stirring for 30min to obtain a solution C;
step 4, carrying out water bath on the solution C for 14h at the heating temperature of 70 ℃, and stirring by using an electric stirrer in the water bath process, wherein the rotating speed is controlled to be 30rpm, so as to obtain a precursor D;
step 5, drying the precursor D at the heating temperature of 120 ℃, controlling the drying time to be 12h, and grinding to obtain a precursor E;
step 6, repeatedly cleaning the precursor E with deionized water for 3-5 times at normal temperature to remove Na in the precursor E+And Al3+Ionizing, and drying at 80 ℃ for 14h to obtain a precursor F;
step 7, calcining the precursor F at 355 ℃ for 3h in air atmosphere to obtain β -Bi2O3Powder;
step 8, putting a certain amount of β -Bi2O3 powder into a vacuum tube furnace, vacuumizing, introducing N2, maintaining the partial pressure of N2 at 1 atmosphere, and carrying out heat treatment at 260 ℃ for 6 hours to obtain black β -Bi with strong visible light absorption capacity2O3And (3) powder.
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N2气氛热处理对纳米TiO2可见光吸收性能的影响;高家诚等;《功能材料》;20091231;第31页第2节、第32-33页第3.4节 * |
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