CN112657520A - Preparation method of visible light catalyst - Google Patents
Preparation method of visible light catalyst Download PDFInfo
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- CN112657520A CN112657520A CN202011538203.8A CN202011538203A CN112657520A CN 112657520 A CN112657520 A CN 112657520A CN 202011538203 A CN202011538203 A CN 202011538203A CN 112657520 A CN112657520 A CN 112657520A
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- visible light
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- 239000003054 catalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 33
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000002244 precipitate Substances 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 10
- 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 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 5
- 239000011941 photocatalyst Substances 0.000 abstract description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 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 abstract 1
- 229940043267 rhodamine b Drugs 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000593 degrading effect Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 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 3
- 229940012189 methyl orange Drugs 0.000 description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a visible light catalyst, and a thermal sensitive catalyst Ag is prepared by a coprecipitation-hydrothermal method3PO4/α‑Bi2O3(ii) a Firstly, preparing alpha-Bi by a hydrothermal method2O3Then adding silver nitrate and disodium hydrogen phosphate in turn, and finally adding silver nitrate and disodium hydrogen phosphate into alpha-Bi2O3Surface coprecipitation to generate heat-sensitive catalyst Ag3PO4/α‑Bi2O3(ii) a Methylene blue and rhodamine B are used for simulating organic matters, and the highest degradation rate can reach 99.9%; the photocatalyst Ag is obtained by adopting the preparation method of the invention3PO4/α‑Bi2O3Has the advantages of high efficiency, stability, simplicity and easy obtainingAnd the photocatalytic degradation efficiency of organic pollutants can be improved.
Description
Technical Field
The invention relates to the technical field of preparation of photocatalysts, in particular to a preparation method of a visible light photocatalyst.
Background
Ag3PO4Due to the high oxidation activity of electron-hole pairs, strong photooxidation ability and high efficiency of photocatalytic degradation of organic pollutants, widely applied in the fields of materials, environment and energy. However, Ag3PO4Is unstable under visible light, can be photo-reduced or decomposed into a weakly active simple substance of silver, and consumes a large amount of the simple substanceSilver increases the cost of the photocatalyst, limiting its practical industrial application.
Disclosure of Invention
The present invention aims to provide a preparation method of a visible light photocatalyst to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a visible light catalyst comprises the following steps:
step one, sequentially adding a certain amount of polyethylene glycol and a certain amount of sodium hydroxide solution into bismuth nitrate, adding ammonia water into the bismuth nitrate, and uniformly stirring;
step two, heating the precipitate generated in the step one for a period of time, cooling, taking out the powder, roasting and drying to obtain alpha-Bi2O3；
Step three, mixing alpha-Bi2O3Uniformly dispersing in deionized water, and ultrasonic treating to obtain alpha-Bi2O3Uniformly dispersing in water;
step four, dropwise adding silver nitrate, stirring to dissolve the silver nitrate, and then dropwise adding a disodium hydrogen phosphate solution to obtain a precipitate; heating the precipitate, naturally cooling, cleaning, and drying to obtain the target product Ag3PO4/α-Bi2O3。
Preferably, ammonia water is used for adjusting the pH value of the solution in the first step to be within a range of 9-10.
Preferably, the sodium hydroxide solution in the first step is a sodium hydroxide solution without carbon dioxide.
Preferably, the Ag is3PO4And alpha-Bi2O3The molar ratio of (A) to (B) is 0.1:1 to 1: 1.
Preferably, the precipitate generated in the second step is transferred to a hydrothermal reaction kettle and is continuously heated for 2-3 hours at the temperature of 90-110 ℃; taking out the powder after cooling, and roasting for 5-8 h at the temperature of 400-430 ℃; and after natural cooling, respectively washing with ultrapure water and ethanol to remove impurities attached to the surface, and drying at 60-65 ℃.
Preferably, the third step is ultrasonic treatment for 4-6 h.
Preferably, the fourth step is to transfer the precipitate into a hydrothermal reaction kettle, keep the precipitate for 3-5 hours at 140-150 ℃, respectively wash the precipitate with ultrapure water and ethanol after natural cooling, and then dry the precipitate for 10-15 hours at 60-80 ℃ to finally obtain the target product.
Compared with the prior art, the invention has the beneficial effects that: the photocatalyst Ag is obtained by adopting the preparation method of the invention3PO4/α-Bi2O3Has the advantages of high efficiency, stability, simplicity and easy obtaining, and can improve the photocatalytic degradation efficiency of organic pollutants.
Drawings
FIG. 1 is a scanning electron micrograph of AB-x/1;
FIG. 2 is a transmission electron micrograph of AB-0.6/1;
FIG. 3 is an X-ray photoelectron spectrum of AB-0.6/1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-3, the present invention provides the following technical solutions: a preparation method of a visible light catalyst comprises the following steps:
step one, sequentially adding a certain amount of polyethylene glycol and a certain amount of sodium hydroxide solution into bismuth nitrate, adding ammonia water into the bismuth nitrate, and uniformly stirring;
step two, heating the precipitate generated in the step one for a period of time, cooling, taking out the powder, roasting and drying to obtain alpha-Bi2O3；
Step three, mixing alpha-Bi2O3Uniformly dispersing in deionized water, and ultrasonic treating to obtain alpha-Bi2O3In waterDispersing uniformly;
step four, dropwise adding silver nitrate, stirring to dissolve the silver nitrate, and then dropwise adding a disodium hydrogen phosphate solution to obtain a precipitate; heating the precipitate, naturally cooling, cleaning, and drying to obtain the target product Ag3PO4/α-Bi2O3。
Example 1
0.5mol of bismuth nitrate is firstly added into a 100ml beaker, then 2ml of polyethylene glycol and 0.4mol of sodium hydroxide solution are added, 5ml of ammonia water is added into the mixture, and the solution is stirred uniformly by a magnetic stirrer. Then transferring the generated precipitate into a hydrothermal reaction kettle of polytetrafluoroethylene, and continuously heating for 2h at 90 ℃. After cooling, the powder is taken out and roasted for 5h at the temperature of 400 ℃. After natural cooling, respectively washing with ultrapure water and ethanol for multiple times to remove impurities attached to the surface, and drying at 60 ℃ to obtain alpha-Bi2O3. Thirdly, 50mg of alpha-Bi2O3Uniformly dispersing in 40ml of deionized water, and then carrying out ultrasonic treatment for 4h to ensure that Bi is dispersed2O3The dispersion is uniform in water. Subsequently, 5mmol of silver nitrate was added dropwise and dissolved with stirring, and then a 0.2mol/L disodium hydrogenphosphate solution was added dropwise thereto to obtain a brown yellow precipitate. Transferring the precipitate into a hydrothermal reaction kettle of polytetrafluoroethylene, keeping the temperature at 140 ℃ for 3h, naturally cooling, washing with ultrapure water and ethanol for multiple times respectively, and drying at 60 ℃ for 10h to obtain a target product AB-1/1.
Example 2
0.5mol of bismuth nitrate is firstly added into a 100ml beaker, then 2ml of polyethylene glycol and 0.4mol of sodium hydroxide solution are added, 4ml of ammonia water is added into the mixture, and the solution is stirred uniformly by a magnetic stirrer. Then transferring the generated precipitate into a hydrothermal reaction kettle of polytetrafluoroethylene, and continuously heating for 3h at 100 ℃. After cooling, the powder is taken out and roasted for 5h at the temperature of 420 ℃. After natural cooling, respectively washing with ultrapure water and ethanol for multiple times to remove impurities attached to the surface, and drying at 70 ℃ to obtain alpha-Bi2O3. Thirdly, 50mg of alpha-Bi2O3Uniformly dispersing in 40ml of deionized water, and then carrying out ultrasonic treatment for 5 hours to ensure that Bi is dispersed2O3The dispersion is uniform in water. 4mmol of silver nitrate was added dropwise, and then dissolved with constant stirring, followed by dropwise addition of a 0.1mol/L disodium hydrogenphosphate solution thereto to give a brown-yellow precipitate. Transferring the precipitate into a hydrothermal reaction kettle of polytetrafluoroethylene, keeping the temperature at 150 ℃ for 4h, naturally cooling, washing with ultrapure water and ethanol for multiple times, and drying at 70 ℃ for 10h to obtain a target product AB-0.8/1.
Example 3
0.5mol of bismuth nitrate is firstly added into a 100ml beaker, then 2ml of polyethylene glycol and 0.5mol of sodium hydroxide solution are added, 6ml of ammonia water is added into the mixture, and the solution is stirred uniformly by a magnetic stirrer. Then transferring the generated precipitate into a hydrothermal reaction kettle of polytetrafluoroethylene, and continuously heating for 3h at 100 ℃. After cooling, the powder is taken out and roasted for 5h at the temperature of 420 ℃. After natural cooling, respectively washing with ultrapure water and ethanol for multiple times to remove impurities attached to the surface, and drying at 70 ℃ to obtain alpha-Bi2O3. Thirdly, 50mg of alpha-Bi2O3Uniformly dispersing in 40ml of deionized water, and then carrying out ultrasonic treatment for 5 hours to ensure that Bi is dispersed2O3The dispersion is uniform in water. 3mmol of silver nitrate was added dropwise, and then dissolved with constant stirring, followed by dropwise addition of a 0.1mol/L disodium hydrogenphosphate solution thereto to give a brown-yellow precipitate. Transferring the precipitate into a hydrothermal reaction kettle of polytetrafluoroethylene, keeping the temperature at 150 ℃ for 4h, naturally cooling, washing with ultrapure water and ethanol for multiple times, and drying at 70 ℃ for 12h to obtain a target product AB-0.6/1.
Example 4
Under the condition of visible light, the reaction temperature is controlled to be 40 ℃, and 5mg of Ag is taken as the thermosensitive catalyst in example 13PO4/α-Bi2O3Adding the mixture into 5mL of methyl orange solution with the concentration of 40mg/L, maintaining the rotating speed at 15 r/min, and degrading for 5min, wherein the degradation rate of the methyl orange reaches 99.2%.
Example 5
In visible light conditionsNext, the reaction temperature was controlled to 30 ℃ to obtain 6mg of Ag as the heat-sensitive catalyst in example 23PO4/α-Bi2O3Adding the mixture into 10mL of methyl orange solution with the concentration of 30mg/L, maintaining the rotating speed at 15 r/min, and degrading for 6min, wherein the degradation rate of the methyl orange reaches 99.4%.
Example 6
Under the condition of visible light, the reaction temperature is controlled to be 30 ℃, and 10mg of Ag is taken as the thermosensitive catalyst in example 33PO4/α-Bi2O3Adding 20mL of methylene blue solution with the concentration of 40mg/L, maintaining the rotating speed at 15 r/min, and degrading for 5min, wherein the degradation rate of the methylene blue reaches 99.5%.
Example 7
Under the condition of visible light, the reaction temperature is controlled to be 35 ℃, and 10mg of Ag is taken as the thermosensitive catalyst in example 13PO4/α-Bi2O3Adding 20mL of methylene blue solution with the concentration of 40mg/L, maintaining the rotating speed at 15 r/min, and degrading for 5min, wherein the degradation rate of the methylene blue reaches 99.9%.
Adjusting Ag by changing the amount of silver nitrate3PO4And alpha-Bi2O3And obtaining a series of products with different proportions. The products of different molar ratios are represented by AB-x/1, x/1(0.1/1, 0.2/1, 0.4/1, 0.6/1, 0.8/1, 1/1) representing Ag3PO4homo-alpha-Bi2O3The ratio of (a) to (b).
Under the condition of visible light, Ag is used at the temperature of 30-35 ℃, the catalyst concentration of 30mg/L, the rotation number of 40-50 rpm and the catalyst concentration of 3-5 mg/L3PO4/α-Bi2O3The methylene blue and the methyl orange are degraded, and the degradation rate reaches 99.9 percent.
In conclusion, the photocatalyst Ag is obtained by the preparation method3PO4/α-Bi2O3Has the advantages of high efficiency, stability, simplicity and easy obtaining, and can improve the photocatalytic degradation efficiency of organic pollutants.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. A preparation method of a visible light catalyst is characterized by comprising the following steps: the preparation method comprises the following steps:
step one, sequentially adding a certain amount of polyethylene glycol and a certain amount of sodium hydroxide solution into bismuth nitrate, adding ammonia water into the bismuth nitrate, and uniformly stirring;
step two, heating the precipitate generated in the step one for a period of time, cooling, taking out the powder, roasting and drying to obtain alpha-Bi2O3；
Step three, mixing alpha-Bi2O3Uniformly dispersing in deionized water, and ultrasonic treating to obtain alpha-Bi2O3Uniformly dispersing in water;
step four, dropwise adding silver nitrate, stirring to dissolve the silver nitrate, and then dropwise adding a disodium hydrogen phosphate solution to obtain a precipitate; heating the precipitate, naturally cooling, cleaning, and drying to obtain the target product Ag3PO4/α-Bi2O3。
2. The method for preparing a visible light catalyst according to claim 1, wherein: in the first step, ammonia water is used for adjusting the pH value of the solution to be within a range of 9-10.
3. The method for preparing a visible light catalyst according to claim 1, wherein: the sodium hydroxide solution in the first step is a sodium hydroxide solution without carbon dioxide.
4. According to claim1, the preparation method of the visible light catalyst is characterized by comprising the following steps: the Ag is3PO4And alpha-Bi2O3The molar ratio of (A) to (B) is 0.1:1 to 1: 1.
5. The method for preparing a visible light catalyst according to claim 1, wherein: transferring the generated precipitate into a hydrothermal reaction kettle, and continuously heating for 2-3 h at 90-110 ℃; taking out the powder after cooling, and roasting for 5-8 h at the temperature of 400-430 ℃; and after natural cooling, respectively washing with ultrapure water and ethanol to remove impurities attached to the surface, and drying at 60-65 ℃.
6. The method for preparing a visible light catalyst according to claim 1, wherein: and thirdly, carrying out ultrasonic treatment for 4-6 h.
7. The method for preparing a visible light catalyst according to claim 1, wherein: and step four, transferring the precipitate into a hydrothermal reaction kettle, keeping the hydrothermal reaction kettle at the temperature of 140-150 ℃ for 3-5 hours, naturally cooling, washing the precipitate with ultrapure water and ethanol respectively, and drying the precipitate at the temperature of 60-80 ℃ for 10-15 hours to obtain the target product.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549389A (en) * | 2014-12-09 | 2015-04-29 | 江苏大学 | Heterojunction nanosheet photocatalyst and preparation method and application of heterojunction nanosheet photocatalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549389A (en) * | 2014-12-09 | 2015-04-29 | 江苏大学 | Heterojunction nanosheet photocatalyst and preparation method and application of heterojunction nanosheet photocatalyst |
Non-Patent Citations (2)
| Title |
|---|
| FENG DING ET AL.: ""Fabrication of Ag3PO4/α-Bi2O3 composites with enhanced photocatalytic properties under visible light"", 《RSC ADVANCES》 * |
| 丁凤: ""近常温热催化降解亚甲基蓝/罗丹明B基础研究"", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
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