CN108479747A - The method that solvent-thermal method prepares stainless (steel) wire load bismuth oxide nanosheet photocatalyst - Google Patents
The method that solvent-thermal method prepares stainless (steel) wire load bismuth oxide nanosheet photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 43
- 239000002135 nanosheet Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 13
- 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 13
- 229910000831 Steel Inorganic materials 0.000 title abstract description 7
- 239000010959 steel Substances 0.000 title abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 78
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 34
- 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 abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 64
- 239000010935 stainless steel Substances 0.000 claims description 64
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 36
- 238000004729 solvothermal method Methods 0.000 claims description 22
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 20
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000012545 processing Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 3
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- 238000012986 modification Methods 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000011084 recovery Methods 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
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
- B01J35/39—Photocatalytic properties
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- 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
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Abstract
Description
技术领域technical field
本发明属于负载型光催化材料制备技术领域，具体涉及一种溶剂热法制备不锈钢网负载氧化铋纳米片光催化剂的方法。The invention belongs to the technical field of preparation of supported photocatalytic materials, and in particular relates to a method for preparing a stainless steel mesh-supported bismuth oxide nanosheet photocatalyst by a solvothermal method.
背景技术Background technique
TiO2等半导体材料可吸收太阳光中的紫外线，当辐射的能量大于或相当于半导体的禁带宽度时，半导体内电子受激发从价带跃迁到导带，而空穴则留在价带，使电子和空穴发生分离，分离的电子和空穴分别具有还原性和氧化性，电子可以还原H2O产生H2，空穴可以氧化H2O变为O2。在有机物存在下，空穴则可以将有机物氧化为CO2和H2O等，广泛应用于光催化降解水体和大气中的有机污染物，在催化领域具有广阔的应用前景，受到了广泛关注。Semiconductor materials such as TiO2 can absorb ultraviolet rays in sunlight. When the energy of the radiation is greater than or equal to the forbidden band width of the semiconductor, the electrons in the semiconductor are excited to jump from the valence band to the conduction band, while the holes stay in the valence band. The electrons and holes are separated, and the separated electrons and holes are respectively reductive and oxidative. The electrons can reduce H 2 O to produce H 2 , and the holes can oxidize H 2 O to O 2 . In the presence of organic matter, holes can oxidize organic matter into CO 2 and H 2 O, etc., and are widely used in photocatalytic degradation of organic pollutants in water and the atmosphere. They have broad application prospects in the field of catalysis and have attracted extensive attention.
目前，为了提高TiO2等半导体光催化剂光催化效率，提高其对太阳能的利用率，使之能够吸收可见光，进行光解水制氢和降解有机污染物，进行了广泛和深入的研究，相关研究概括起来主要包括两个方面：At present, in order to improve the photocatalytic efficiency of semiconductor photocatalysts such as TiO 2 , increase their utilization rate of solar energy, enable them to absorb visible light, carry out photolysis of water to produce hydrogen and degrade organic pollutants, extensive and in-depth research has been carried out. In summary, it mainly includes two aspects:
1、TiO2改性研究1. Research on modification of TiO 2
关于TiO2改性研究主要包括光催化剂纳米化、金属和非金属离子掺杂、半导体复合、染料光敏化、贵金属沉积、电子捕获剂、表面螯合及衍生作用和场外耦合等。这些改性研究提高了TiO2光催化效率，改性后的TiO2可以吸收太阳光中的可见光部分，进行光解水制氢和降解有机污染物。The research on TiO 2 modification mainly includes photocatalyst nanonization, metal and non-metal ion doping, semiconductor recombination, dye photosensitization, noble metal deposition, electron trapping agent, surface chelation and derivatization, and out-of-field coupling, etc. These modification studies have improved the photocatalytic efficiency of TiO 2 , and the modified TiO 2 can absorb the visible part of sunlight for photolysis of water to produce hydrogen and degrade organic pollutants.
2、寻找新的光催化剂2. Search for new photocatalysts
新的光催化体系包括钽酸盐[ATaO3(A＝Li,K),A2SrTa2O7·nH2O(A＝H,K,Rb)]、铌酸[Ba5LaTi2Nb3O18]、钛酸盐、多元硫化物和铋系光催化剂等。这些新的光催化体系丰富了光催化的研究内容，在提高光催化效率和太阳能利用方面取得了显著的进步。The new photocatalytic system includes tantalate [ATaO 3 (A=Li, K), A 2 SrTa 2 O 7 ·nH 2 O (A=H, K, Rb)], niobate [Ba 5 LaTi 2 Nb 3 O 18 ], titanates, polysulfides and bismuth-based photocatalysts, etc. These new photocatalytic systems have enriched the research content of photocatalysis, and have made remarkable progress in improving photocatalytic efficiency and solar energy utilization.
上述光催化剂均为纳米粉末状材料，虽然具有较高的光催化效率和可见光吸收效率，但是在流体中存在分离回收困难、纳米粒子易凝聚等缺点，限制和阻碍了这些纳米光催化剂的工业化应用。The above-mentioned photocatalysts are all nano-powder materials. Although they have high photocatalytic efficiency and visible light absorption efficiency, they have disadvantages such as difficult separation and recovery in fluids and easy aggregation of nanoparticles, which limit and hinder the industrial application of these nanophotocatalysts. .
为了解决上述问题，研究开发薄膜型TiO2是将光催化剂应用于流体净化的关键问题之一，目前国内外对TiO2薄膜光催化剂进行了很多研究，但大都局限于薄膜催化剂的晶相结构，并且薄膜型TiO2光催化剂的比表面积低，与反应物的接触面积有限，因而光催化效率不高。In order to solve the above problems, the research and development of thin-film TiO2 is one of the key issues in applying photocatalysts to fluid purification. At present, a lot of research has been done on TiO2 thin-film photocatalysts at home and abroad, but most of them are limited to the crystal phase structure of thin-film catalysts, and thin-film Type TiO2 photocatalyst has low specific surface area and limited contact area with reactants, so the photocatalytic efficiency is not high.
发明内容Contents of the invention
本发明所要解决的技术问题在于针对上述现有技术中的不足，提供一种溶剂热法制备不锈钢网负载氧化铋纳米片光催化剂的方法，将Bi2O3纳米片光催化剂负载在不锈钢网上，既解决了纳米光催化剂分离回收困难，又解决了薄膜型光催化剂光催化效率低的问题。The technical problem to be solved by the present invention is to provide a kind of solvothermal method for preparing stainless steel mesh-loaded bismuth oxide nanosheet photocatalyst for the above-mentioned deficiencies in the prior art, by loading Bi2O3 nanosheet photocatalyst on the stainless steel mesh, It not only solves the difficulty of separation and recovery of nano photocatalysts, but also solves the problem of low photocatalytic efficiency of thin film photocatalysts.
本发明采用以下技术方案：The present invention adopts following technical scheme:
溶剂热法制备不锈钢网负载氧化铋纳米片光催化剂的方法，以硝酸铋、乙二醇和丙酮为原料，不锈钢网为载体，控制水热反应温度和时间进行溶剂热反应，反应结束后取出不锈钢网，清洗后经烘干处理制得不锈钢网负载Bi2O3纳米片光催化剂。Solvothermal method for preparing stainless steel mesh-loaded bismuth oxide nanosheet photocatalyst, using bismuth nitrate, ethylene glycol and acetone as raw materials, stainless steel mesh as carrier, controlling the hydrothermal reaction temperature and time for solvothermal reaction, and taking out the stainless steel mesh after the reaction , washed and dried to prepare stainless steel mesh-loaded Bi 2 O 3 nanosheet photocatalysts.
具体的，将乙二醇加入丙酮中混合均匀得到溶液A；然后取硝酸铋加入到制备的溶液A中经完全溶解制得溶液B；然后将溶液B转移到水热反应釜中，将不锈钢网浸入溶液B，进行溶剂热反应。Specifically, ethylene glycol is added to acetone and mixed uniformly to obtain solution A; then bismuth nitrate is added to the prepared solution A and completely dissolved to obtain solution B; then solution B is transferred to a hydrothermal reaction kettle, and the stainless steel mesh Immerse in solution B for solvothermal reaction.
进一步的，乙二醇和丙酮按3:1～2:1的质量比混合制成溶液A。Further, ethylene glycol and acetone are mixed at a mass ratio of 3:1-2:1 to prepare solution A.
进一步的，硝酸铋加入量为乙二醇加入量的1/24～1/12，搅拌或超声促进硝酸铋溶解制得溶液B。Further, the amount of bismuth nitrate added is 1/24-1/12 of the amount of ethylene glycol added, stirring or ultrasonically promoting the dissolution of bismuth nitrate to prepare solution B.
进一步的，水热反应釜的填充度为70～80％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为150～170℃，水热反应时间为10～12h，水热反应完成后自然冷却至室温，取出不锈钢网备用。Further, the filling degree of the hydrothermal reaction kettle is 70-80%, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in solution B, the hydrothermal reaction temperature is 150-170°C, and the hydrothermal reaction time is 10-100°C. After 12 hours, after the completion of the hydrothermal reaction, it was naturally cooled to room temperature, and the stainless steel mesh was taken out for later use.
进一步的，采用超声波对制备的不锈钢网进行水洗5～10s。Further, the prepared stainless steel mesh is washed with water for 5-10 seconds by ultrasonic waves.
具体的，烘干处理的温度为80～90℃，处理时间为12～24h。Specifically, the drying treatment temperature is 80-90° C., and the treatment time is 12-24 hours.
与现有技术相比，本发明至少具有以下有益效果：Compared with the prior art, the present invention has at least the following beneficial effects:
本发明提供一种溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂的方法，采用溶剂热法，以硝酸铋、乙二醇和丙酮为原料制备不锈钢网负载Bi2O3纳米片光催化剂，优化了不锈钢网负载Bi2O3纳米片光催化剂制备工艺，工艺流程简单，产品性能优良，具有较好的可见光光催化性能，在80～90℃烘干既可以除去水分，又可以避免产物受热分解，干燥12～24h可以保证充分除去水分。The invention provides a method for preparing stainless steel mesh-loaded Bi2O3 nanosheet photocatalyst by solvothermal method, using bismuth nitrate, ethylene glycol and acetone as raw materials to prepare stainless steel mesh - loaded Bi2O3 nanosheet photocatalyst , optimized the preparation process of stainless steel mesh-loaded Bi 2 O 3 nanosheet photocatalyst, the process flow is simple, the product performance is excellent, and it has good visible light photocatalytic performance. Drying at 80-90°C can not only remove water, but also avoid Thermal decomposition, drying for 12 to 24 hours can ensure full removal of moisture.
进一步的，乙二醇和丙酮的质量比为3:1～2:1，在此范围内乙二醇浓度大于其临界胶束浓度，有利于获得片状Bi2O3，硝酸铋加入量为乙二醇加入量的1/24～1/12，有利于降低Bi2O3纳米片的厚度。Furthermore, the mass ratio of ethylene glycol to acetone is 3:1 to 2:1. Within this range, the concentration of ethylene glycol is greater than its critical micelle concentration, which is conducive to obtaining flaky Bi 2 O 3 . The amount of bismuth nitrate added is B 1/24-1/12 of the added amount of diol is beneficial to reduce the thickness of Bi 2 O 3 nanosheets.
进一步的，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，有利于Bi2O3纳米片在不锈钢网上的生长，提高二者的结合强度。Further, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in solution B, which is beneficial to the growth of Bi 2 O 3 nanosheets on the stainless steel mesh and improves the bonding strength of the two.
进一步的，水热反应的温度范围为150～170℃，填充度为70～80％，该条件下有利于形成高压条件，反应时间为12～18h，有利于反应充分进行。Further, the temperature range of the hydrothermal reaction is 150-170° C., and the filling degree is 70-80%, which is conducive to the formation of high-pressure conditions, and the reaction time is 12-18 hours, which is conducive to the full progress of the reaction.
进一步的，反应结束后不锈钢网用超声波水洗5～10s，有利于获得纯净的Bi2O3纳米片。Further, after the reaction, the stainless steel mesh is washed with ultrasonic water for 5-10 s, which is beneficial to obtain pure Bi 2 O 3 nanosheets.
综上所述，本发明工艺简单，有效优化不锈钢网负载Bi2O3纳米片光催化剂制备工艺，制备的产品性能优良，能作为光催化材料使用。In summary, the process of the present invention is simple, and the preparation process of Bi 2 O 3 nanosheet photocatalyst supported by stainless steel mesh is effectively optimized. The prepared product has excellent performance and can be used as a photocatalytic material.
下面通过附图和实施例，对本发明的技术方案做进一步的详细描述。The technical solutions of the present invention will be described in further detail below with reference to the accompanying drawings and embodiments.
附图说明Description of drawings
图1为本发明不锈钢网负载Bi2O3纳米片光催化剂的XRD谱图；Fig. 1 is the XRD spectrogram of the stainless steel mesh of the present invention supporting Bi 2 O 3 nanosheet photocatalysts;
图2为本发明不锈钢网负载Bi2O3纳米片光催化剂的SEM照片，其中，(a)为锈钢网负载Bi2O3纳米片光催化材料放大500倍SEM照片，(b)为不锈钢网负载Bi2O3纳米片光催化材料放大10万倍SEM照片；Fig. 2 is the SEM photograph of the stainless steel net supporting Bi2O3 nanosheet photocatalyst of the present invention, wherein, (a) is the SEM photo of the stainless steel net supporting Bi2O3 nanosheet photocatalytic material enlarged 500 times, (b) is the stainless steel net supporting Bi2O3 Nanosheet photocatalytic material magnified 100,000 times SEM photo;
图3本发明制备不锈钢网负载Bi2O3纳米片光催化剂对罗丹明B的可见光光催化效果。Fig. 3 Visible light photocatalytic effect of rhodamine B on stainless steel mesh supported Bi 2 O 3 nanosheet photocatalyst prepared by the present invention.
具体实施方式Detailed ways
本发明一种溶剂热法制备不锈钢网负载氧化铋纳米片光催化剂的方法，以硝酸铋(Bi(NO3)3·5H2O)、乙二醇和丙酮为原料，不锈钢网为载体，采用溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂，具体步骤如下：The invention discloses a method for preparing stainless steel net-loaded bismuth oxide nanosheet photocatalyst by solvothermal method, using bismuth nitrate (Bi(NO 3 ) 3 5H 2 O), ethylene glycol and acetone as raw materials, stainless steel net as carrier, and solvent Thermal preparation of stainless steel mesh supported Bi 2 O 3 nanosheet photocatalyst, the specific steps are as follows:
S1、取乙二醇加入到丙酮中，混合均匀得到溶液A；S1, take ethylene glycol and join in acetone, mix uniformly to obtain solution A;
乙二醇和丙酮按3:1～2:1的质量比混合。Ethylene glycol and acetone are mixed at a mass ratio of 3:1 to 2:1.
S2、取硝酸铋加入到溶液A中，完全溶解得溶液B；S2, get bismuth nitrate and join in solution A, dissolve completely and obtain solution B;
硝酸铋加入量为乙二醇加入量的1/24～1/12，搅拌或超声促进硝酸铋溶解。The amount of bismuth nitrate added is 1/24 to 1/12 of the amount of ethylene glycol added, and stirring or ultrasonication promotes the dissolution of bismuth nitrate.
S3、溶液B转移到反应釜中，将不锈钢网浸入溶液B，进行溶剂热反应；S3, the solution B is transferred to the reaction kettle, the stainless steel mesh is immersed in the solution B, and the solvothermal reaction is carried out;
水热反应釜的填充度为70～80％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为150～170℃，水热反应时间为10～12h，水热反应完成后需自然冷却至室温。The filling degree of the hydrothermal reaction kettle is 70-80%. The stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in solution B. The hydrothermal reaction temperature is 150-170°C, and the hydrothermal reaction time is 10-12h. After the thermal reaction is completed, it needs to be naturally cooled to room temperature.
S4、反应结束取出不锈钢网，超声清洗后烘干，制得不锈钢网负载Bi2O3纳米片光催化剂；S4, the stainless steel net is taken out after the reaction is completed, dried after ultrasonic cleaning, and the stainless steel net-loaded Bi 2 O 3 nanosheet photocatalyst is obtained;
反应结束后不锈钢网用超声波水洗5～10s，烘干温度为80～90℃，烘干时间为12～24h。After the reaction, the stainless steel mesh is washed with ultrasonic water for 5-10s, the drying temperature is 80-90°C, and the drying time is 12-24h.
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。通常在此处附图中的描述和所示的本发明实施例的组件可以通过各种不同的配置来布置和设计。因此，以下对在附图中提供的本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments It is a part of embodiments of the present invention, but not all embodiments. The components of the embodiments of the invention generally described and illustrated in the drawings herein may be arranged and designed in a variety of different configurations. Accordingly, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.
实施例1Example 1
一种溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂的方法，包括以下步骤：A kind of solvothermal method prepares the stainless steel net load Bi 2 O 3 the method for the nano sheet photocatalyst, comprises the following steps:
1)将乙二醇和丙酮按3:1的质量比混合均匀得到溶液A；1) Ethylene glycol and acetone are mixed uniformly at a mass ratio of 3:1 to obtain solution A;
2)取硝酸铋加入到溶液A中，硝酸铋加入量为乙二醇加入量的1/24，搅拌促进硝酸铋溶解，完全溶解得溶液B；2) Add bismuth nitrate to solution A, the amount of bismuth nitrate added is 1/24 of the amount of ethylene glycol added, stirring promotes the dissolution of bismuth nitrate, and completely dissolves to obtain solution B;
3)溶液B转移到反应釜中，水热反应釜的填充度为70％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为150℃，水热反应时间为12h，水热反应完成后需自然冷却至室温。3) Solution B is transferred to the reaction kettle, the filling degree of the hydrothermal reaction kettle is 70%, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in the solution B, the hydrothermal reaction temperature is 150°C, and the hydrothermal reaction time is After 12 hours, the hydrothermal reaction needs to be naturally cooled to room temperature.
4)反应结束取出不锈钢网，超声清洗5s，烘干温度为80℃，烘干时间为24h。4) After the reaction, take out the stainless steel mesh, ultrasonically clean it for 5 seconds, and dry it at 80°C for 24 hours.
实施例2Example 2
一种溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂的方法，包括以下步骤：A kind of solvothermal method prepares the stainless steel net load Bi 2 O 3 the method for the nano sheet photocatalyst, comprises the following steps:
1)将乙二醇和丙酮按2:1的质量比混合均匀得到溶液A；1) Ethylene glycol and acetone are mixed uniformly at a mass ratio of 2:1 to obtain solution A;
2)取硝酸铋加入到溶液A中，硝酸铋加入量为乙二醇加入量的1/20，超声促进硝酸铋溶解，完全溶解得溶液B；2) Take bismuth nitrate and add it to solution A, the amount of bismuth nitrate added is 1/20 of the amount of ethylene glycol added, ultrasonically promotes the dissolution of bismuth nitrate, and completely dissolves to obtain solution B;
3)溶液B转移到反应釜中，水热反应釜的填充度为75％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为155℃，水热反应时间为11.5h，水热反应完成后需自然冷却至室温。3) Solution B is transferred to the reaction kettle, the filling degree of the hydrothermal reaction kettle is 75%, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in the solution B, the hydrothermal reaction temperature is 155 °C, and the hydrothermal reaction time is After 11.5h, the hydrothermal reaction needs to be naturally cooled to room temperature.
4)反应结束取出不锈钢网，超声清洗6s，烘干温度为85℃，烘干时间为20h。4) After the reaction, the stainless steel mesh was taken out, ultrasonically cleaned for 6 seconds, and the drying temperature was 85° C., and the drying time was 20 hours.
实施例3Example 3
一种溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂的方法，包括以下步骤：A kind of solvothermal method prepares the stainless steel net load Bi 2 O 3 the method for the nano sheet photocatalyst, comprises the following steps:
1)将乙二醇和丙酮按2.5:1的质量比混合均匀得到溶液A；1) Ethylene glycol and acetone are mixed uniformly at a mass ratio of 2.5:1 to obtain solution A;
2)取硝酸铋加入到溶液A中，硝酸铋加入量为乙二醇加入量的1/18，搅拌促进硝酸铋溶解，完全溶解得溶液B；2) Add bismuth nitrate to solution A, the amount of bismuth nitrate added is 1/18 of the amount of ethylene glycol added, stirring promotes the dissolution of bismuth nitrate, and completely dissolves to obtain solution B;
3)溶液B转移到反应釜中，水热反应釜的填充度为80％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为160℃，水热反应时间为11h，水热反应完成后需自然冷却至室温。3) Solution B is transferred to the reaction kettle, the filling degree of the hydrothermal reaction kettle is 80%, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in solution B, the hydrothermal reaction temperature is 160 °C, and the hydrothermal reaction time is After the completion of the hydrothermal reaction, it needs to be naturally cooled to room temperature.
4)反应结束取出不锈钢网，超声清洗7s，烘干温度为85℃，烘干时间为18h。4) After the reaction, the stainless steel mesh was taken out, ultrasonically cleaned for 7 seconds, and the drying temperature was 85°C for 18 hours.
实施例4Example 4
一种溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂的方法，包括以下步骤：A kind of solvothermal method prepares the stainless steel net load Bi 2 O 3 the method for the nano sheet photocatalyst, comprises the following steps:
1)将乙二醇和丙酮按2:1的质量比混合均匀得到溶液A；1) Ethylene glycol and acetone are mixed uniformly at a mass ratio of 2:1 to obtain solution A;
2)取硝酸铋加入到溶液A中，硝酸铋加入量为乙二醇加入量的1/15，搅拌促进硝酸铋溶解，完全溶解得溶液B；2) Take bismuth nitrate and add it to solution A, the amount of bismuth nitrate added is 1/15 of the amount of ethylene glycol added, stirring promotes the dissolution of bismuth nitrate, and completely dissolves to obtain solution B;
3)溶液B转移到反应釜中，水热反应釜的填充度为78％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为165℃，水热反应时间为10.5h，水热反应完成后需自然冷却至室温。3) Solution B is transferred to the reaction kettle, the filling degree of the hydrothermal reaction kettle is 78%, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in the solution B, the hydrothermal reaction temperature is 165 °C, and the hydrothermal reaction time After 10.5h, the hydrothermal reaction needs to be naturally cooled to room temperature.
4)反应结束取出不锈钢网，超声清洗9s，烘干温度为90℃，烘干时间为12h。4) After the reaction, the stainless steel mesh was taken out, ultrasonically cleaned for 9s, and the drying temperature was 90°C for 12 hours.
实施例5Example 5
一种溶剂热法制备不锈钢网负载Bi2O3纳米片光催化剂的方法，包括以下步骤：A kind of solvothermal method prepares the stainless steel net load Bi 2 O 3 the method for the nano sheet photocatalyst, comprises the following steps:
1)将乙二醇和丙酮按2.5:1的质量比混合均匀得到溶液A；1) Ethylene glycol and acetone are mixed uniformly at a mass ratio of 2.5:1 to obtain solution A;
2)取硝酸铋加入到溶液A中，硝酸铋加入量为乙二醇加入量的1/12，搅拌或超声促进硝酸铋溶解，完全溶解得溶液B；2) Take bismuth nitrate and add it to solution A. The amount of bismuth nitrate added is 1/12 of the amount of ethylene glycol added. Stir or ultrasonically promote the dissolution of bismuth nitrate, and completely dissolve to obtain solution B;
3)溶液B转移到反应釜中，水热反应釜的填充度为80％，不锈钢网用去离子水和乙醇清洗干净并完全浸入溶液B中，水热反应温度为170℃，水热反应时间为10h，水热反应完成后需自然冷却至室温。3) Solution B is transferred to the reaction kettle, the filling degree of the hydrothermal reaction kettle is 80%, the stainless steel mesh is cleaned with deionized water and ethanol and completely immersed in the solution B, the hydrothermal reaction temperature is 170 °C, and the hydrothermal reaction time is After 10 hours, the hydrothermal reaction needs to be naturally cooled to room temperature.
4)反应结束取出不锈钢网，超声清洗10s，烘干温度为90℃，烘干时间为1h。4) After the reaction, the stainless steel mesh was taken out, ultrasonically cleaned for 10 s, and dried at 90° C. for 1 h.
采用实施例1制备的不锈钢网负载Bi2O3纳米片光催化剂的XRD谱图如图1所示，采用实施例2制备的不锈钢网负载Bi2O3纳米片光催化剂的SEM照片如图2所示，其中，(a)为锈钢网负载Bi2O3纳米片光催化材料放大500倍SEM照片，(b)为不锈钢网负载Bi2O3纳米片光催化材料放大10万倍SEM照片，在罗丹明B浓度为20mg/L，在可见光照射下光催化反应12min，罗丹明B降解率为100％，实验结果如图3所示，采用以上所述实验方案，均可获得具有较高光催化活性的不锈钢网负载Bi2O3纳米片光催化剂，在上述条件范围之内，产品的纯度和性能不受影响。Adopt the stainless steel mesh prepared by embodiment 1 to load Bi 2 O The XRD spectrogram of nanosheet photocatalyst is shown in Figure 1, adopt the stainless steel mesh prepared in Example 2 to load Bi 2 O The SEM photo of O nanosheet photocatalyst is shown in Figure 2 As shown, among them, (a) is a 500-fold SEM photo of the photocatalytic material loaded on rusty steel mesh, and (b) is a 100,000-fold SEM photo of the photocatalytic material loaded on stainless steel mesh. The photocatalytic reaction was 12 minutes under visible light irradiation, and the degradation rate of Rhodamine B was 100%. The experimental results are shown in Figure 3. Using the above-mentioned experimental scheme, stainless steel mesh loads with high photocatalytic activity can be obtained. Bi 2 O 3 nanosheet photocatalyst, within the range of the above conditions, the purity and performance of the product will not be affected.
以上内容仅为说明本发明的技术思想，不能以此限定本发明的保护范围，凡是按照本发明提出的技术思想，在技术方案基础上所做的任何改动，均落入本发明权利要求书的保护范围之内。The above content is only to illustrate the technical ideas of the present invention, and cannot limit the protection scope of the present invention. Any changes made on the basis of the technical solutions according to the technical ideas proposed in the present invention shall fall within the scope of the claims of the present invention. within the scope of protection.
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