CN110038552A - With visible light-responded bismuth stannate photochemical catalyst and preparation method thereof - Google Patents
With visible light-responded bismuth stannate photochemical catalyst and preparation method thereof Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 41
- 229940071182 stannate Drugs 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 title claims description 13
- 239000000243 solution Substances 0.000 claims abstract description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 5
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000003643 water by type Substances 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 31
- 230000004298 light response Effects 0.000 abstract description 17
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229960001229 ciprofloxacin hydrochloride Drugs 0.000 description 4
- DIOIOSKKIYDRIQ-UHFFFAOYSA-N ciprofloxacin hydrochloride Chemical compound Cl.C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 DIOIOSKKIYDRIQ-UHFFFAOYSA-N 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- -1 BiFeO3 Chemical class 0.000 description 1
- 229910002902 BiFeO3 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100001240 inorganic pollutant Toxicity 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
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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
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
本发明属于光催化材料技术领域，公开了一种具有可见光响应的锡酸铋光催化剂的制备方法，包括如下步骤：将SnCl4·5H2O溶解于20 mL去离子水中，并搅拌至完全溶解；将Bi(NO3)3·5H2O溶于30 mL 2 M的稀硝酸溶液中；在搅拌过程中将上述两种溶液混合，继续搅拌30分钟；用一定浓度的NaOH溶液调节该混合溶液的pH，调节至适宜pH后，在搅拌下继续反应60 min；将所得溶液置于100 mL水热釜中，180ºC条件下反应24个小时，室温下冷却，将沉淀物离心、水洗后置于干燥箱中烘干；研钵中研磨得到锡酸铋光催化剂；还公开了由上述制备方法所制得的具有可见光响应的锡酸铋光催化剂。本发明，采用锅水热法制备出具有可见光响应的锡酸铋材料，在模拟光照射下对有机污染物降解效率较高的特性。
The invention belongs to the technical field of photocatalytic materials, and discloses a preparation method of a bismuth stannate photocatalyst with visible light response . ; Dissolve Bi(NO 3 ) 3 .5H 2 O in 30 mL of 2 M dilute nitric acid solution; mix the above two solutions during stirring, and continue stirring for 30 minutes; adjust the mixed solution with a certain concentration of NaOH solution After adjusting to a suitable pH, the reaction was continued for 60 min under stirring; the obtained solution was placed in a 100 mL hydrothermal kettle, reacted at 180ºC for 24 hours, cooled at room temperature, and the precipitate was centrifuged, washed with water and placed in a Drying in a drying oven; grinding in a mortar to obtain a bismuth stannate photocatalyst; and a bismuth stannate photocatalyst with visible light response prepared by the above preparation method is also disclosed. The invention adopts the pot hydrothermal method to prepare the bismuth stannate material with visible light response, and has the characteristics of high degradation efficiency of organic pollutants under simulated light irradiation.
Description
技术领域technical field
本发明涉及光催化材料技术领域，具体是一种具有可见光响应的锡酸铋光催化剂及其制备方法。The invention relates to the technical field of photocatalytic materials, in particular to a bismuth stannate photocatalyst with visible light response and a preparation method thereof.
背景技术Background technique
目前，能源危机和环境污染已成为吸引全球研究人员关注的两大问题。半导体光催化被认为是开发新能源和治理环境污染的有效途径之一。这种方法具有设备简单、氧化性能强、高效节能、操作条件容易控制等特点，并且不会对环境造成二次污染。当光催化剂吸收一个能量（hυ）与其带隙能（Eg）相匹配或超过Eg的光子，价带上的电子（e-）将会向导带跃迁，同时在价带上留下带正电的空穴（h+），从而形成光生e--h+对。h+是一种强氧化剂，导带e-是一种强还原剂，它们可以将大多数的有机和无机污染物无选择性的直接、间接氧化或还原，且不需要添加其它化学试剂，从而实现污染物的减量化和无害化。二氧化钛被认为是最有前途的光催化剂之一，在紫外光照射下具有高光催化活性，优异的化学稳定性，以及低成本和无毒性。然而，由于相对较大的能带隙（Eg）约为3.2 eV，TiO2对可见光没有响应，这限制了其在实际应用中的使用。因此，有必要开发新的可见光响应光催化剂。At present, energy crisis and environmental pollution have become two major issues that attract the attention of researchers around the world. Semiconductor photocatalysis is considered to be one of the effective ways to develop new energy and control environmental pollution. This method has the characteristics of simple equipment, strong oxidation performance, high efficiency and energy saving, easy control of operating conditions, etc., and will not cause secondary pollution to the environment. When a photocatalyst absorbs a photon with an energy (hυ) that matches or exceeds its band gap energy (Eg), an electron (e-) in the valence band will transition to the conduction band, leaving a positively charged electron in the valence band. holes (h+), thereby forming photogenerated e--h+ pairs. h+ is a strong oxidant, conduction band e- is a strong reducing agent, they can directly and indirectly oxidize or reduce most organic and inorganic pollutants without selectivity, and do not need to add other chemical reagents, so as to achieve Reduction and harmlessness of pollutants. Titanium dioxide is considered to be one of the most promising photocatalysts with high photocatalytic activity under UV light irradiation, excellent chemical stability, and low cost and non-toxicity. However, due to the relatively large energy band gap (Eg) of about 3.2 eV, TiO2 does not respond to visible light, which limits its use in practical applications. Therefore, it is necessary to develop new visible-light-responsive photocatalysts.
众所周知，可见光响应光催化剂因其在可见光照射下分解水或降解有机污染物的潜在应用而引起越来越多的关注。近年来，许多研究者致力于含Bi化合物的开发研究，如BiFeO3、BiVO4和Bi2WO6等。这些Bi系化合物在可见光范围内都显示出一定的光催化能力，归因于O 2p和Bi 6s的杂化价带使其带隙变窄。作为Bi基氧化物的一员，典型的烧绿石结构Bi2Sn2O7因其特殊的离子电导率、催化作用和气体传感性能而得到广泛研究。然而，关于在可见光照射下改善Bi2Sn2O7的光催化降解性能的研究仍然很少。Bi2Sn2O7作为一种具有可见光响应的新型光催化材料，它将为光催化去除和降解有机污染物开辟一条新的途径，在环境净化和新能源开发方面具有非常良好的应用前景。因此，研究开发高活性、高稳定性和良好循环利用性能的可见光催化剂，是国内外水处理领域的重要前沿课题。It is well known that visible light-responsive photocatalysts have attracted increasing attention due to their potential applications in water splitting or degradation of organic pollutants under visible light irradiation. In recent years, many researchers have devoted themselves to the development of Bi-containing compounds, such as BiFeO3, BiVO4 and Bi2WO6. These Bi-based compounds all show a certain photocatalytic ability in the visible light range, which is attributed to the narrowing of the band gap due to the hybrid valence bands of O 2p and Bi 6s. As a member of Bi-based oxides, the typical pyrochlore structure Bi2Sn2O7 has been widely studied for its special ionic conductivity, catalytic effect, and gas sensing properties. However, there are still few studies on improving the photocatalytic degradation performance of Bi2Sn2O7 under visible light irradiation. As a novel photocatalytic material with visible light response, Bi2Sn2O7 will open up a new way for photocatalytic removal and degradation of organic pollutants, and has very good application prospects in environmental purification and new energy development. Therefore, the research and development of visible light catalysts with high activity, high stability and good recycling performance is an important frontier topic in the field of water treatment at home and abroad.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种具有可见光响应的锡酸铋光催化剂及其制备方法，以解决上述背景技术中提出的问题。The purpose of the present invention is to provide a bismuth stannate photocatalyst with visible light response and a preparation method thereof, so as to solve the problems raised in the above background technology.
为实现上述目的，本发明提供如下技术方案：To achieve the above object, the present invention provides the following technical solutions:
一种具有可见光响应的锡酸铋光催化剂及其制备方法，包括如下步骤：A bismuth stannate photocatalyst with visible light response and a preparation method thereof, comprising the following steps:
（1）将SnCl4·5H2O溶解于20 mL 去离子水中，并搅拌至完全溶解；(1) Dissolve SnCl 4 ·5H 2 O in 20 mL of deionized water, and stir until completely dissolved;
（2）将Bi(NO3)3·5H2O溶于30 mL 2 M的稀硝酸溶液中；(2) Dissolve Bi(NO 3 ) 3 ·5H 2 O in 30 mL of 2 M dilute nitric acid solution;
（3）在搅拌过程中将上述两种溶液混合，继续搅拌30分钟；(3) Mix the above two solutions during the stirring process and continue stirring for 30 minutes;
（4）用一定浓度的NaOH溶液调节该混合溶液的pH，调节至适宜pH后，在搅拌下继续反应60 min；(4) Adjust the pH of the mixed solution with a certain concentration of NaOH solution, and after adjusting to an appropriate pH, continue the reaction for 60 min under stirring;
（5）将所得溶液置于100 mL水热釜中，180ºC条件下反应24个小时，室温下冷却，将沉淀物离心、水洗后置于干燥箱中烘干；(5) The obtained solution was placed in a 100 mL hydrothermal kettle, reacted at 180ºC for 24 hours, cooled at room temperature, and the precipitate was centrifuged, washed with water, and then dried in a drying oven;
（6）研钵中研磨得到锡酸铋光催化剂。(6) Grinding in a mortar to obtain a bismuth stannate photocatalyst.
作为本发明进一步的方案：步骤（1）中，SnCl4·5H2O的摩尔质量为0.01mol。As a further solution of the present invention: in step (1), the molar mass of SnCl 4 ·5H 2 O is 0.01 mol.
作为本发明进一步的方案：步骤（2）中，Bi(NO3)3·5H2O的摩尔质量为0.01mol。As a further solution of the present invention: in step (2), the molar mass of Bi(NO 3 ) 3 ·5H 2 O is 0.01 mol.
作为本发明进一步的方案：步骤（3）中，NaOH溶液的浓度为4 M。As a further scheme of the present invention: in step (3), the concentration of the NaOH solution is 4 M.
作为本发明进一步的方案：步骤（3）中，调节pH至pH=7。As a further solution of the present invention: in step (3), the pH is adjusted to pH=7.
作为本发明进一步的方案：步骤（3）中，调节pH至pH=9。As a further solution of the present invention: in step (3), the pH is adjusted to pH=9.
作为本发明进一步的方案：步骤（3）中，调节pH至pH=11。As a further solution of the present invention: in step (3), the pH is adjusted to pH=11.
作为本发明再进一步的方案：步骤（3）中，调节pH至pH=13。As a further solution of the present invention: in step (3), the pH is adjusted to pH=13.
一种具有可见光响应的锡酸铋光催化剂，由上述的具有可见光响应的锡酸铋光催化剂的制备方法制备得到。A bismuth stannate photocatalyst with visible light response is prepared by the above-mentioned preparation method of the bismuth stannate photocatalyst with visible light response.
与现有技术相比，本发明的有益效果是：Compared with the prior art, the beneficial effects of the present invention are:
所述一种具有可见光响应的锡酸铋光催化剂及其制备方法，工艺简单且成本低廉，采用锅水热法制备出具有可见光响应的锡酸铋材料，在模拟光照射下对有机污染物降解效率较高的特性。The bismuth stannate photocatalyst with visible light response and a preparation method thereof have the advantages of simple process and low cost. The bismuth stannate material with visible light response is prepared by a pot hydrothermal method, and the organic pollutants are degraded under simulated light irradiation. Features with higher efficiency.
附图说明Description of drawings
图1为具有可见光响应的锡酸铋光催化剂的XRD图。FIG. 1 is an XRD pattern of a bismuth stannate photocatalyst with visible light response.
图2为具有可见光响应的锡酸铋光催化剂的SEM图。FIG. 2 is an SEM image of a bismuth stannate photocatalyst with visible light response.
具体实施方式Detailed ways
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，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做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。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
实施例1Example 1
本发明实施例1中，一种具有可见光响应的锡酸铋光催化剂的制备方法，包括如下步骤：将0.01mol SnCl4·5H2O溶解于20 mL 去离子水中，并搅拌至完全溶解，将0.01mol Bi(NO3)3·5H2O溶于30 mL 2 M的稀硝酸溶液中。在搅拌过程中将上述两种溶液混合，继续搅拌30分钟。之后向该混合溶液中逐滴滴加4 M的NaOH溶液，调节pH至pH=7，在搅拌下继续反应60 min。将所得溶液置于100 mL水热釜中，180ºC条件下反应24个小时，室温下冷却，将沉淀物离心、水洗后置于干燥箱中烘干，研钵中研磨得到锡酸铋光催化剂。In Example 1 of the present invention, a method for preparing a bismuth stannate photocatalyst with visible light response includes the following steps: dissolving 0.01 mol of SnCl 4 ·5H 2 O in 20 mL of deionized water, stirring until completely dissolved, 0.01 mol Bi(NO 3 ) 3 ·5H 2 O was dissolved in 30 mL of 2 M dilute nitric acid solution. The above two solutions were mixed during stirring, and stirring was continued for 30 minutes. Then, 4 M NaOH solution was added dropwise to the mixed solution, the pH was adjusted to pH=7, and the reaction was continued for 60 min under stirring. The obtained solution was placed in a 100 mL hydrothermal kettle, reacted at 180ºC for 24 hours, cooled at room temperature, the precipitate was centrifuged, washed with water, dried in a drying oven, and ground in a mortar to obtain a bismuth stannate photocatalyst.
上述制备方法所得到的锡酸铋光催化剂，经过模拟光照射120 min，对10 mg/L的盐酸环丙沙星废水的去除率为40.15%。The bismuth stannate photocatalyst obtained by the above preparation method was irradiated with simulated light for 120 min, and the removal rate of 10 mg/L ciprofloxacin hydrochloride wastewater was 40.15%.
实施例2Example 2
本发明实施例2中，一种具有可见光响应的锡酸铋光催化剂的制备方法，包括如下步骤：将0.01mol SnCl4·5H2O溶解于20 mL 去离子水中，并搅拌至完全溶解，将0.01mol Bi(NO3)3·5H2O溶于30 mL 2 M的稀硝酸溶液中。在搅拌过程中将上述两种溶液混合，继续搅拌30分钟，之后向该混合溶液中逐滴滴加4 M的NaOH溶液，调节pH至pH=9，在搅拌下继续反应60 min。将所得溶液置于100 mL水热釜中，180ºC条件下反应24个小时。室温下冷却，将沉淀物离心、水洗后置于干燥箱中烘干，研钵中研磨得到锡酸铋光催化剂。In Example 2 of the present invention, a method for preparing a bismuth stannate photocatalyst with visible light response includes the following steps: dissolving 0.01 mol of SnCl 4 ·5H 2 O in 20 mL of deionized water, stirring until completely dissolved, 0.01 mol Bi(NO 3 ) 3 ·5H 2 O was dissolved in 30 mL of 2 M dilute nitric acid solution. During the stirring process, the above two solutions were mixed, and the stirring was continued for 30 minutes. Then, 4 M NaOH solution was added dropwise to the mixed solution to adjust the pH to pH=9, and the reaction was continued for 60 minutes under stirring. The resulting solution was placed in a 100 mL hydrothermal kettle and reacted at 180ºC for 24 hours. Cooling at room temperature, the precipitate is centrifuged, washed with water, dried in a drying oven, and ground in a mortar to obtain a bismuth stannate photocatalyst.
上述制备方法所得到的锡酸铋光催化剂，经过模拟光照射120 min，对10 mg/L的盐酸环丙沙星废水的去除率为39.9%。The bismuth stannate photocatalyst obtained by the above preparation method was irradiated with simulated light for 120 min, and the removal rate of 10 mg/L ciprofloxacin hydrochloride wastewater was 39.9%.
实施例3Example 3
本发明实施例3中，一种具有可见光响应的锡酸铋光催化剂的制备方法，包括如下步骤：将0.01mol SnCl4·5H2O溶解于20 mL 去离子水中，并搅拌至完全溶解，将0.01mol Bi(NO3)3·5H2O溶于30 mL 2 M的稀硝酸溶液中。在搅拌过程中将上述两种溶液混合，继续搅拌30分钟，之后向该混合溶液中逐滴滴加4 M的NaOH溶液，调节pH至pH=11，在搅拌下继续反应60 min。将所得溶液置于100 mL水热釜中，180ºC条件下反应24个小时，室温下冷却，将沉淀物离心、水洗后置于干燥箱中烘干，研钵中研磨得到锡酸铋光催化剂。In Example 3 of the present invention, a method for preparing a bismuth stannate photocatalyst with visible light response includes the following steps: dissolving 0.01 mol of SnCl 4 ·5H 2 O in 20 mL of deionized water, stirring until completely dissolved, 0.01 mol Bi(NO 3 ) 3 ·5H 2 O was dissolved in 30 mL of 2 M dilute nitric acid solution. During the stirring process, the above two solutions were mixed, and the stirring was continued for 30 minutes. Then, 4 M NaOH solution was added dropwise to the mixed solution to adjust the pH to pH=11, and the reaction was continued for 60 minutes under stirring. The obtained solution was placed in a 100 mL hydrothermal kettle, reacted at 180ºC for 24 hours, cooled at room temperature, the precipitate was centrifuged, washed with water, dried in a drying oven, and ground in a mortar to obtain a bismuth stannate photocatalyst.
上述制备方法所得到的锡酸铋光催化剂，经过模拟光照射120 min，对10 mg/L的盐酸环丙沙星废水的去除率为68.5%。The bismuth stannate photocatalyst obtained by the above preparation method was irradiated with simulated light for 120 min, and the removal rate of 10 mg/L ciprofloxacin hydrochloride wastewater was 68.5%.
实施例4Example 4
本发明实施例4中，一种具有可见光响应的锡酸铋光催化剂的制备方法，包括如下步骤：将0.01mol SnCl4·5H2O溶解于20 mL 去离子水中，并搅拌至完全溶解，将0.01mol Bi(NO3)3·5H2O溶于30 mL 2 M的稀硝酸溶液中。在搅拌过程中将上述两种溶液混合，继续搅拌30分钟。之后向该混合溶液中逐滴滴加4 M的NaOH溶液，调节pH至pH=13，在搅拌下继续反应60 min，将所得溶液置于100 mL水热釜中，180ºC条件下反应24个小时。室温下冷却，将沉淀物离心、水洗后置于干燥箱中烘干，研钵中研磨得到锡酸铋光催化剂。In Example 4 of the present invention, a method for preparing a bismuth stannate photocatalyst with visible light response includes the following steps: dissolving 0.01 mol of SnCl 4 ·5H 2 O in 20 mL of deionized water, stirring until completely dissolved, 0.01 mol Bi(NO 3 ) 3 ·5H 2 O was dissolved in 30 mL of 2 M dilute nitric acid solution. The above two solutions were mixed during stirring, and stirring was continued for 30 minutes. Then, 4 M NaOH solution was added dropwise to the mixed solution, pH was adjusted to pH=13, and the reaction was continued for 60 min under stirring. The obtained solution was placed in a 100 mL hydrothermal kettle and reacted at 180ºC for 24 hours. . Cooling at room temperature, the precipitate is centrifuged, washed with water, dried in a drying oven, and ground in a mortar to obtain a bismuth stannate photocatalyst.
上述制备方法所得到的锡酸铋光催化剂，经过模拟光照射120 min，对10 mg/L的盐酸环丙沙星废水的去除率为42.6%。The bismuth stannate photocatalyst obtained by the above preparation method was irradiated with simulated light for 120 min, and the removal rate of 10 mg/L ciprofloxacin hydrochloride wastewater was 42.6%.
参阅图1和图2，基于以上实施例，选取pH=11时制备的锡酸铋光催化剂的性能较优，即实施例3，通过进一步的表征研究，该条件下制备的锡酸铋光催化剂属于球形纳米片，相比于传统的光催化材料，本发明制得的锡酸铋光催化剂能够响应模拟光，具有可见光催化活性，且制备方法简单快速，无二次污染。Referring to FIG. 1 and FIG. 2, based on the above examples, the performance of the bismuth stannate photocatalyst prepared when pH=11 is selected is better, that is, Example 3, through further characterization research, the bismuth stannate photocatalyst prepared under this condition It belongs to spherical nanosheets. Compared with traditional photocatalytic materials, the bismuth stannate photocatalyst prepared by the invention can respond to simulated light, has visible light catalytic activity, and the preparation method is simple and fast without secondary pollution.
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。It will be apparent to those skilled in the art that the present invention is not limited to the details of the above-described exemplary embodiments, but that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments are to be regarded in all respects as illustrative and not restrictive, and the scope of the invention is to be defined by the appended claims rather than the foregoing description, which are therefore intended to fall within the scope of the claims. All changes within the meaning and scope of the equivalents of , are included in the present invention.
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。In addition, it should be understood that although this specification is described in terms of embodiments, not each embodiment only includes an independent technical solution, and this description in the specification is only for the sake of clarity, and those skilled in the art should take the specification as a whole , the technical solutions in each embodiment can also be appropriately combined to form other implementations that can be understood by those skilled in the art.
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