CN115646479A - Preparation method of organic matter modified BSO heterogeneous photocatalytic material - Google Patents
Preparation method of organic matter modified BSO heterogeneous photocatalytic material Download PDFInfo
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- CN115646479A CN115646479A CN202211296484.XA CN202211296484A CN115646479A CN 115646479 A CN115646479 A CN 115646479A CN 202211296484 A CN202211296484 A CN 202211296484A CN 115646479 A CN115646479 A CN 115646479A
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 38
- 239000005416 organic matter Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004475 Arginine Substances 0.000 claims abstract description 28
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 28
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008103 glucose Substances 0.000 claims abstract description 28
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims abstract description 17
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 39
- 239000008367 deionised water Substances 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 29
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 17
- 238000000502 dialysis Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 13
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 8
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000013543 active substance Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 9
- DQUIAMCJEJUUJC-UHFFFAOYSA-N dibismuth;dioxido(oxo)silane Chemical compound [Bi+3].[Bi+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O DQUIAMCJEJUUJC-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 5
- 238000007605 air drying Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of an organic matter modified BSO heterogeneous photocatalytic material. The BSO heterogeneous photocatalytic material is modified by the cooperation of glucose and arginine, the process of preferential growth of a specific crystal face is effectively inhibited, active substances in the degradation process are changed while the morphology of the BSO heterogeneous photocatalytic material is regulated, a seriously accumulated lamellar structure of the BSO heterogeneous photocatalytic material is effectively dispersed, the separation efficiency of a photon-generated carrier of the BSO heterogeneous photocatalytic material is accelerated, the light absorption range is expanded, the photocatalytic activity is enhanced, and the photocatalytic degradation efficiency of organic pollutants is improved.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a preparation method of an organic matter modified BSO heterogeneous photocatalytic material.
Background
Si 2 Bi 24 O 40 The (BSO) photocatalyst has a unique electronic structure, excellent visible light absorption capability and higher organic matter degradation capability. Bi 2 O 2 SiO 3 (BOS) is an important semiconductor functional material with unique [ Bi ] 2 O 2 ] 2+ -[SiO 3 ] 2- -[Bi 2 O 2 ] 2+ A layered structure. Because the single-phase photocatalyst often can not effectively realize the rapid separation of photon-generated carriers, the two materials can be compounded to form a heterojunction, thereby improving the photocatalytic performance of the photocatalyst. However, after the BSO is compounded with the BOS, the formed lamellar structure is seriously stacked, and agglomerated particles exist on the surface of the lamellar, which greatly blocks the adsorption channel of pollutants and reduces active sites on the surface of the material, thereby affecting the photocatalytic performance of the material.
In patent CN202110551331.4, a sol-gel method is used to prepare high-purity metastable phase Bi 2 O 2 SiO 3 Using metastable phases of Bi 2 O 2 SiO 3 The problem of agglomeration of part of block BSO materials is solved by easily generating a lamellar structure, but the problem of stacking the lamellar structure is still not overcome, and the catalytic material with high specific surface area cannot be effectively obtained, so that the photocatalytic performance of the catalytic material is limited.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of an organic matter modified BSO heterogeneous photocatalytic material, so as to obtain a photocatalytic composite material with perfect crystallization and excellent photocatalytic performance, and the preparation process has the characteristics of low cost, easy operation and short production period.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of an organic matter modified BSO heterogeneous photocatalytic material comprises the following steps:
weighing bismuth nitrate, dissolving the bismuth nitrate in deionized water, stirring, and adding ethylene glycol to form solution A;
weighing sodium metasilicate nonahydrate, dissolving in deionized water, and stirring to form a solution B;
slowly dripping the solution B into the solution A, and stirring to form a white emulsion-shaped BSO precursor;
step (4), weighing glucose and arginine, placing the glucose and the arginine in deionized water, and stirring the mixture at room temperature to form solution C;
step (5), putting the solution C into a polytetrafluoroethylene reaction kettle, reacting for 2-3 h at 160-200 ℃, and cooling to room temperature along with a furnace to obtain solution D;
step (6), centrifuging the solution D, filling the solution D into a dialysis bag for dialysis, and obtaining a mixed solution of glucose and arginine;
transferring the BSO precursor to a stainless steel reaction kettle lined with polytetrafluoroethylene, adding a mixed solution of glucose and arginine, sealing the reaction kettle, keeping the reaction kettle at a constant temperature of 160-200 ℃ for 8-14 h, and naturally cooling to room temperature; and washing and drying the obtained product to obtain the organic matter modified BSO heterogeneous photocatalytic material.
In one embodiment, in the step (1), 0.005-0.007 mol of bismuth nitrate, 3-5 mL of deionized water and 6-8 mL of ethylene glycol are added; in the step (2), 0.005-0.007 mol of sodium metasilicate nonahydrate and 7-10 mL of deionized water are added; in the step (4), 0.01 to 0.02mol of glucose, 0.005 to 0.01mol of arginine and 20 to 30mL of deionized water are added; and (7) mixing the glucose with the arginine by 2.5-15 mL.
In one embodiment, in the step (1), the stirring is continuously carried out for 25-40 min; the step (2) is to continuously stir for 25 to 40min; stirring for 20-30 min in the step (3); and (4) stirring for 30-40 min.
In one embodiment, in step (6), the centrifugation conditions are: centrifuging for 10-15 min under the centrifugal force of 12000 g; the molecular weight of the dialysis bag is 1000Da, and the dialysis conditions are as follows: dialyzing in 2000mL deionized water for 22-26 h.
In one embodiment, step (7), the stainless steel reactor fill volume is 80%.
In one embodiment, in the step (7), the washing conditions are: washing with deionized water and ethanol alternately for 2-3 times.
In one embodiment, in the step (7), the drying conditions are: drying for 8-12 h at 60-80 ℃.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the organic matter modified BSO heterogeneous photocatalytic material, the mixed solution of glucose and arginine subjected to hydrothermal pretreatment is used for effectively improving the photocatalytic performance of heterogeneous BSO, and the main reason is that active substances participating in a photocatalytic degradation process are converted while the morphology is regulated. Firstly, in the reaction of modifying BSO, the preferential growth of crystal faces (311) and (123) of the BSO is destroyed by glucose and arginine, a small and thin three-dimensional flower-shaped nano lamellar structure is formed, and the purpose of regulating and controlling the morphology is achieved; in addition, glucose and arginine are easy to form an intermediate product with reducibility in the reaction process, so that oxygen vacancies are obviously increased in the growth process of BSO, thereby forming an oxygen defect energy level, promoting the charge separation efficiency of a photon-generated carrier, accelerating the surface redox reaction and improving the photocatalytic performance of BSO.
Drawings
FIG. 1 is an SEM photograph of a sample obtained in example 1 of the present invention.
FIG. 2 is a graph showing the degradation of contaminants in a sample obtained in example 2 of the present invention.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
As described above, in the prior art, after BSO and BOS are compounded, a serious stacking phenomenon occurs, and a large amount of agglomerated particles exist on the surface of the sheet, which affects pollutant adsorption, and reduces surface active sites, so that the photocatalytic performance is affected. If a specific substance is found, the above problem can be solved by dispersing its lamellar structure.
Therefore, the invention provides the preparation method of the organic matter modified BSO heterogeneous photocatalytic material, which has the advantages of low cost, easy operation and short production period, the obtained composite material has good crystallization and excellent photocatalytic performance, and the specific operation steps are as follows:
weighing 0.005-0.007 mol of bismuth nitrate, dissolving the bismuth nitrate into 3-5 mL of deionized water, continuously stirring for 25-40 min, and adding 6-8 mL of ethylene glycol during stirring to form solution A;
step (2), weighing 0.005-0.007 mol of sodium metasilicate nonahydrate into 7-10 mL of deionized water, and continuously stirring for 25-40 min to form a solution B;
and (3) slowly dripping the solution B into the solution A, and stirring for 20-30 min to form a white emulsion-shaped BSO precursor.
Weighing 0.01-0.02 mol of glucose and 0.005-0.01 mol of arginine, placing the glucose and the arginine into 20-30 mL of deionized water, and fully stirring the mixture at room temperature for 30-40 min to form a transparent light yellow solution;
step (5), putting the transparent light yellow solution into a 30mL polytetrafluoroethylene reaction kettle, putting the reaction kettle into an electric heating air blowing drying oven, reacting for 2-3 h at 160-200 ℃, cooling to room temperature along with the oven, and changing the solution into brown;
and (6) centrifuging the brown liquid for 10-15 min under the centrifugal force of 12000g, then filling the liquid into a dialysis bag with the molecular weight of 1000Da, putting the dialysis bag into 2000mL of deionized water for dialysis for 22-26 h, wherein the dialyzed brown liquid is the mixed liquid of glucose and arginine.
Step (7), transferring the bismuth silicate precursor into a stainless steel reaction kettle lined with polytetrafluoroethylene (the filling volume is 80%); weighing 2.5-15 mL of glucose and arginine mixed solution, adding the mixed solution into a bismuth silicate precursor, sealing the reaction kettle, placing the reaction kettle in a forced air drying oven, keeping the temperature at 160-200 ℃ for 8-14 h, and naturally cooling to room temperature; and (3) washing the obtained product with deionized water and ethanol for 2-3 times in turn, and drying at 60-80 ℃ for 8-12 h to obtain the organic matter modified BSO heterogeneous photocatalytic material.
In the invention, the BSO heterogeneous photocatalytic material is synergistically modified by glucose and arginine, so that the process of preferential growth of a specific crystal face can be effectively inhibited, active substances in a degradation process are changed while the morphology of the BSO heterogeneous photocatalytic material is regulated, a seriously-stacked lamellar structure of the BSO heterogeneous photocatalytic material is effectively dispersed, the separation efficiency of a photon-generated carrier of the BSO heterogeneous photocatalytic material is accelerated, the light absorption range is expanded, the photocatalytic activity is enhanced, and the photocatalytic degradation efficiency of organic pollutants is improved.
Several embodiments of the invention are as follows.
Example 1:
a preparation method of an organic matter modified BSO heterogeneous photocatalytic material comprises the following steps:
(1) Weighing 0.006mol of bismuth nitrate, dissolving the bismuth nitrate in 4mL of deionized water, continuously stirring for 30min, and adding 7mL of ethylene glycol during stirring to form solution A;
(2) Weighing 0.006mol of sodium metasilicate nonahydrate into 8mL of deionized water, and continuously stirring for 30min to form a solution B;
(3) And slowly dripping the solution B into the solution A, and stirring for 20min to form a white emulsion-shaped bismuth silicate precursor.
(4) Weighing 0.017mol of glucose and 0.009mol of arginine, placing in 25mL of deionized water, and fully stirring at room temperature for 30min to form a transparent light yellow solution;
(5) Putting the transparent light yellow solution into a 30mL polytetrafluoroethylene reaction kettle, putting the reaction kettle into an electric heating forced air drying oven, reacting for 3 hours at 180 ℃, cooling the reaction kettle to room temperature along with the furnace, and changing the solution into brown;
(6) Centrifuging the brown liquid for 10min under 12000g centrifugal force, filling into a dialysis bag with molecular weight of 1000Da, and dialyzing the dialysis bag in 2000mL deionized water for 24h, wherein the dialyzed brown liquid is the mixed solution of glucose and arginine.
(7) Transferring the bismuth silicate precursor into a stainless steel reaction kettle lined with polytetrafluoroethylene (the filling volume is 80%); measuring 5mL of glucose and arginine mixed solution, adding the mixed solution into a bismuth silicate precursor, sealing the reaction kettle, placing the reaction kettle in an air-blast drying oven, keeping the temperature at 180 ℃ for 14h, and naturally cooling to room temperature; and (3) alternately washing the obtained product by using deionized water and ethanol in sequence for 3 times, and drying at 60 ℃ for 12 hours to obtain the organic matter modified BSO heterogeneous photocatalytic material.
Example 2:
a preparation method of an organic matter modified BSO heterogeneous photocatalytic material comprises the following steps:
(1) Weighing 0.007mol of bismuth nitrate, dissolving the bismuth nitrate in 5mL of deionized water, continuously stirring for 40min, and adding 8mL of ethylene glycol during stirring to form solution A;
(2) Weighing 0.007mol of sodium metasilicate nonahydrate in 10mL of deionized water, and continuously stirring for 40min to form a solution B;
(3) And slowly dripping the solution B into the solution A, and stirring for 30min to form a white emulsion-shaped bismuth silicate precursor.
(4) Weighing 0.02mol of glucose and 0.01mol of arginine, placing the glucose and the arginine into 30mL of deionized water, and fully stirring the mixture at room temperature for 40min to form a transparent light yellow solution;
(5) Putting the transparent light yellow solution into a 30mL polytetrafluoroethylene reaction kettle, putting the reaction kettle into an electric heating forced air drying oven, reacting for 2 hours at 200 ℃, cooling to room temperature along with the oven, and changing the solution into brown;
(6) Centrifuging the brown liquid for 15min under 12000g of centrifugal force, filling into a dialysis bag with the molecular weight of 1000Da, and putting the dialysis bag into 2000mL of deionized water for dialysis for 25h, wherein the dialyzed brown liquid is the mixed liquid of glucose and arginine.
(7) Transferring the bismuth silicate precursor into a stainless steel reaction kettle lined with polytetrafluoroethylene (the filling volume is 80%); weighing 2.5mL of glucose and arginine mixed solution, adding the mixed solution into a bismuth silicate precursor, sealing the reaction kettle, placing the reaction kettle in a forced air drying oven, keeping the reaction kettle at a constant temperature of 180 ℃ for 12 hours, and naturally cooling the reaction kettle to room temperature; and (3) alternately washing the obtained product by using deionized water and ethanol in sequence for 3 times, and drying at 80 ℃ for 10 hours to obtain the organic matter modified BSO heterogeneous photocatalytic material.
As can be seen from FIG. 1, the appearance of the product modified by the organic substance is a small and thin three-dimensional flower-like nanosheet structure, and the layer-by-layer stacking phenomenon is effectively improved. As can be seen from FIG. 2, after simulated visible light irradiation for 150min, the sample has a degradation rate of 99% for Rh B, and the photocatalytic performance is obviously improved.
Claims (7)
1. A preparation method of an organic matter modified BSO heterogeneous photocatalytic material is characterized by comprising the following steps:
weighing bismuth nitrate, dissolving the bismuth nitrate in deionized water, stirring, and adding ethylene glycol to form solution A;
weighing sodium metasilicate nonahydrate, dissolving in deionized water, and stirring to form a solution B;
slowly dripping the solution B into the solution A, and stirring to form a white emulsion-shaped BSO precursor;
step (4), weighing glucose and arginine, placing the glucose and the arginine in deionized water, and stirring the mixture at room temperature to form solution C;
step (5), putting the solution C into a polytetrafluoroethylene reaction kettle, reacting for 2-3 h at 160-200 ℃, and cooling to room temperature along with a furnace to obtain solution D;
step (6), centrifuging the solution D, and then putting the solution D into a dialysis bag for dialysis to obtain a mixed solution of glucose and arginine;
transferring the BSO precursor to a stainless steel reaction kettle lined with polytetrafluoroethylene, adding a mixed solution of glucose and arginine, sealing the reaction kettle, keeping the reaction kettle at a constant temperature of 160-200 ℃ for 8-14 h, and naturally cooling to room temperature; and washing and drying the obtained product to obtain the organic matter modified BSO heterogeneous photocatalytic material.
2. The preparation method of the organic matter modified BSO heterogeneous photocatalytic material according to claim 1, wherein in the step (1), 0.005-0.007 mol of bismuth nitrate, 3-5 mL of deionized water and 6-8 mL of ethylene glycol are added; in the step (2), 0.005-0.007 mol of sodium metasilicate nonahydrate and 7-10 mL of deionized water are added; in the step (4), 0.01 to 0.02mol of glucose, 0.005 to 0.01mol of arginine and 20 to 30mL of deionized water are added; and (7) mixing the glucose with the arginine by 2.5-15 mL.
3. The preparation method of the organic matter modified BSO heterogeneous photocatalytic material according to claim 1 or 2, wherein in the step (1), the stirring is continued for 25-40 min; the step (2) is to continuously stir for 25 to 40min; stirring for 20-30 min in the step (3); and (4) stirring for 30-40 min.
4. The method for preparing the organic matter modified BSO heterogeneous photocatalytic material according to claim 1 or 2, wherein in the step (6), the centrifugation conditions are as follows: centrifuging for 10-15 min under the centrifugal force of 12000 g; the molecular weight of the dialysis bag is 1000Da, and the dialysis conditions are as follows: dialyzing in 2000mL deionized water for 22-26 h.
5. The method for preparing organic matter modified BSO heterogeneous photocatalytic material according to claim 1 or 2, wherein in the step (7), the filling volume of the stainless steel reaction kettle is 80%.
6. The method for preparing organic matter modified BSO heterogeneous photocatalytic material according to claim 1 or 2, wherein in the step (7), the washing conditions are as follows: washing with deionized water and ethanol alternately for 2-3 times.
7. The method for preparing organic matter modified BSO heterogeneous photocatalytic material according to claim 1 or 2, wherein in the step (7), the drying conditions are as follows: drying for 8-12 h at 60-80 ℃.
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| 张培阳: "新型铋系光催化剂的制备及其光催化性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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