CN104998671A - A kind of supported Bi2O2CO3 photocatalyst and preparation method thereof - Google Patents
A kind of supported Bi2O2CO3 photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 32
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 32
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims description 37
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 23
- 239000011572 manganese Substances 0.000 claims description 23
- 239000011701 zinc Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 11
- 239000011240 wet gel Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 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 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000120 microwave digestion Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims 2
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000000725 suspension Substances 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 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
- 230000005284 excitation Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000012784 weak cation exchange Methods 0.000 description 1
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Abstract
本发明公开了一种负载型Bi2O2CO3光催化剂及其制备方法，属于无机环保光催化材料技术领域。本发明的技术方案要点是通过将Bi2O2CO3与负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土复合而形成的。本发明还公开了该负载型Bi2O2CO3光催化剂的制备方法。本发明的高岭土较强的吸附吸性能可以维持Bi2O2CO3悬浮体系较高的光催化效率，利用磁性技术来回收光催化剂，简化分离过程，降低操作费用，制备方法简单，易于控制且成本低廉。The invention discloses a loaded Bi 2 O 2 CO 3 photocatalyst and a preparation method thereof, belonging to the technical field of inorganic environment-friendly photocatalytic materials. The gist of the technical solution of the present invention is formed by compounding Bi 2 O 2 CO 3 with kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 . The invention also discloses a preparation method of the supported Bi 2 O 2 CO 3 photocatalyst. The kaolin of the present invention has strong adsorption and absorption properties, can maintain the high photocatalytic efficiency of the Bi 2 O 2 CO 3 suspension system, uses magnetic technology to recover the photocatalyst, simplifies the separation process, reduces operating costs, and has a simple preparation method, easy control and low cost.
Description
技术领域 technical field
本发明属于无机环保光催化材料技术领域，具体涉及一种负载型Bi2O2CO3光催化剂及其制备方法。 The invention belongs to the technical field of inorganic environment - friendly photocatalytic materials, and in particular relates to a loaded Bi2O2CO3 photocatalyst and a preparation method thereof.
背景技术 Background technique
近年来，利用半导体光催化技术降解染料废水及空气中有机污染物的研究十分活跃。光催化技术的核心内容为选择合适的光催化剂，半导体光催化剂不同，其带隙不同，对光源的选择性不同，带隙激发需要的光能也不同，导致不同半导体光催化性能的差异。例如某些窄带隙半导体光催化剂如CdS等在可见光照射下有光催化活性，但是由于其本身的光化学不稳定性，使其在光线照射下会发生光腐蚀，因而不是良好的光催化剂。因此，开发新型具有光化学稳定性及具有较高光催化活性的光催化剂显得尤为迫切。 In recent years, the use of semiconductor photocatalytic technology to degrade dye wastewater and organic pollutants in the air has been very active. The core content of photocatalytic technology is to choose a suitable photocatalyst. Different semiconductor photocatalysts have different band gaps, different selectivity to light sources, and different light energy required for band gap excitation, resulting in differences in photocatalytic performance of different semiconductors. For example, some narrow-bandgap semiconductor photocatalysts such as CdS have photocatalytic activity under visible light irradiation, but due to their own photochemical instability, they will undergo photocorrosion under light irradiation, so they are not good photocatalysts. Therefore, it is particularly urgent to develop new photocatalysts with photochemical stability and high photocatalytic activity.
Bi2O2CO3是一种新型的光催化材料，其禁带宽度为3.4eV，当受到能量不低于其带隙的光照射时，会产生导带电子和价带空穴，具有较强的还原性和氧化性，能直接将有机污染物降解成无毒无害的水和二氧化碳。但是纳米Bi2O2CO3光催化剂在使用过程中一方面容易团聚致使光催化活性降低，另一方面由于其粒径太小导致其分离及回收再生困难。所以，用于废水处理时，必须将Bi2O2CO3负载于一定的载体上才能使用。高岭土是储量丰富的非金属矿物，是以高岭石族矿物为主要成分的土质岩石，具有强的离子吸附性和弱的阳离子交换性、强吸水性、易于分散悬浮于水中等特点，非常适合用来作为Bi2O2CO3光催化剂的载体。以天然矿物高岭土作为Bi2O2CO3光催化剂载体，可以使Bi2O2CO3光催化剂牢固地与矿物结合，进而使光催化性能更稳定持久；另外，在废水处理应用中，还可以利用高岭土的离子交换和吸附性能将废水中的有机物有效地吸附到Bi2O2CO3光催化剂的表面，增加催化剂与污染物的接触几率，达到提高光降解效率和降解速率的目的，同时还可以大大降低催化剂的制备成本。尽管将Bi2O2CO3负载在高岭土上可以提高其光催化活性，然而在工程应用上，悬浮体系光催化剂粉末使用后需要过滤将其分离回收，在分离过程中相当一部分光催化剂流失，同时回收的光催化剂活性也有所降低。近年来，一种高效、快速且经济的磁分离技术已被广泛应用于环境保护等领域。如果将一种磁性组分负载在Bi2O2CO3光催化剂表面，不但可以避免催化剂颗粒间的团聚，提高其光催化活性，还可以增加Bi2O2CO3光催化剂的沉降速率，并利用磁分离技术将其从废水处理体系中快速分离出，解决了光催化技术在实际应用中的关键问题。 Bi 2 O 2 CO 3 is a new type of photocatalytic material with a forbidden band width of 3.4eV. When irradiated with light whose energy is not lower than its band gap, it will generate conduction band electrons and valence band holes, which have a relatively With strong reducing and oxidizing properties, it can directly degrade organic pollutants into non-toxic and harmless water and carbon dioxide. However, the nano-Bi 2 O 2 CO 3 photocatalyst is easy to agglomerate during use, resulting in a decrease in photocatalytic activity, and on the other hand, it is difficult to separate, recycle and regenerate due to its small particle size. Therefore, when used for wastewater treatment, Bi 2 O 2 CO 3 must be loaded on a certain carrier before it can be used. Kaolin is a non-metallic mineral with abundant reserves. It is an earthy rock mainly composed of kaolinite minerals. It has strong ion adsorption, weak cation exchange, strong water absorption, and is easy to disperse and suspend in water. It is very suitable for Used as the carrier of Bi 2 O 2 CO 3 photocatalyst. Using the natural mineral kaolin as the Bi 2 O 2 CO 3 photocatalyst carrier can make the Bi 2 O 2 CO 3 photocatalyst firmly bond with the mineral, thereby making the photocatalytic performance more stable and durable; in addition, in wastewater treatment applications, it can also Utilize the ion exchange and adsorption properties of kaolin to effectively adsorb the organic matter in the wastewater to the surface of the Bi 2 O 2 CO 3 photocatalyst, increase the contact probability between the catalyst and pollutants, achieve the purpose of improving the photodegradation efficiency and degradation rate, and at the same time The preparation cost of the catalyst can be greatly reduced. Although loading Bi 2 O 2 CO 3 on kaolin can improve its photocatalytic activity, however, in engineering applications, the photocatalyst powder in the suspension system needs to be separated and recovered by filtration after use. During the separation process, a considerable part of the photocatalyst is lost, and at the same time The recovered photocatalyst activity was also reduced. In recent years, an efficient, fast and economical magnetic separation technology has been widely used in environmental protection and other fields. If a magnetic component is loaded on the surface of the Bi 2 O 2 CO 3 photocatalyst, it can not only avoid the agglomeration of the catalyst particles, improve its photocatalytic activity, but also increase the sedimentation rate of the Bi 2 O 2 CO 3 photocatalyst, and It is quickly separated from the wastewater treatment system by using magnetic separation technology, which solves the key problem in the practical application of photocatalytic technology.
发明内容 Contents of the invention
本发明解决的技术问题是提供了一种光催化活性高且易于分离回收并重复使用的负载型Bi2O2CO3光催化剂。 The technical problem solved by the invention is to provide a supported Bi 2 O 2 CO 3 photocatalyst with high photocatalytic activity and easy separation, recovery and reuse.
本发明解决的另一个技术问题是提供了一种操作简单、易于控制且成本低廉的负载型Bi2O2CO3光催化剂的制备方法。 Another technical problem solved by the present invention is to provide a preparation method of a supported Bi 2 O 2 CO 3 photocatalyst with simple operation, easy control and low cost.
本发明为解决上述技术问题采用如下技术方案，一种负载型Bi2O2CO3光催化剂，其特征在于是通过将Bi2O2CO3与负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土复合而形成的，其中高岭土与软磁性Mn0.5Zn0.5Fe2O4的质量比为5-15:1，负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土与Bi2O2CO3的质量比为1-3:1。 In order to solve the above technical problems, the present invention adopts the following technical scheme, a supported Bi 2 O 2 CO 3 photocatalyst, which is characterized in that Bi 2 O 2 CO 3 and loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 It is formed by compounding kaolin, wherein the mass ratio of kaolin and soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 is 5-15:1, and the kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 and Bi 2 O 2 CO The mass ratio of 3 is 1-3:1.
本发明所述的负载型Bi2O2CO3光催化剂的制备方法，其特征在于包括以下步骤：（1）将硝酸锰、硝酸锌和硝酸铁按摩尔比1:1:4的比例与去离子水混合均匀得到混合溶液，再向混合溶液中加入高岭土，然后向混合体系中加入乙二胺四乙酸二钠（EDTA），其中EDTA的加入量与硝酸锌的摩尔比为3:1，将所得的混合体系在80℃的水浴中保持12h得到湿凝胶，湿凝胶经110℃干燥得到干凝胶，然后将干凝胶于500℃煅烧2h后得到负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土；（2）在搅拌条件下将五水硝酸铋和尿素按摩尔比1:3的比例与去离子水混合均匀得到混合溶液，向混合溶液中加入氨水调节混合溶液的pH值为4，在搅拌条件下将步骤（1）制得的负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土加入到上述混合溶液中，将所得的混合体系转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于180-200℃微波反应10-30min，经冷却、过滤、洗涤、干燥后得到具有高催化活性的负载型Bi2O2CO3光催化剂。 The preparation method of the supported Bi 2 O 2 CO 3 photocatalyst of the present invention is characterized in that it comprises the following steps: (1) mixing manganese nitrate, zinc nitrate and iron nitrate in a molar ratio of 1:1:4 with the removed Ionized water is mixed evenly to obtain a mixed solution, then kaolin is added to the mixed solution, and then disodium ethylenediaminetetraacetic acid (EDTA) is added to the mixed system, wherein the molar ratio of EDTA to zinc nitrate is 3:1. The resulting mixed system was kept in a water bath at 80°C for 12 hours to obtain a wet gel, and the wet gel was dried at 110°C to obtain a xerogel, and then the xerogel was calcined at 500°C for 2 hours to obtain a soft magnetic Mn 0.5 Zn 0.5 Fe loaded 2 O 4 kaolin; (2) Mix bismuth nitrate pentahydrate and urea with deionized water at a molar ratio of 1:3 under stirring conditions to obtain a mixed solution, and add ammonia water to the mixed solution to adjust the pH value of the mixed solution For 4, add the kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 prepared in step (1) to the above mixed solution under stirring conditions, transfer the resulting mixed system to a hydrothermal reactor, and then Put the hydrothermal reaction kettle into a microwave digestion apparatus and react with microwave at 180-200°C for 10-30min, after cooling, filtering, washing and drying, a loaded Bi 2 O 2 CO 3 photocatalyst with high catalytic activity is obtained.
进一步限定，步骤（1）的混合溶液中硝酸锌的摩尔浓度为0.01mol/L。 Further defined, the molar concentration of zinc nitrate in the mixed solution in step (1) is 0.01mol/L.
进一步限定，步骤（1）中加入高岭土的量为软磁性Mn0.5Zn0.5Fe2O4质量的5-15倍。 It is further defined that the amount of kaolin added in step (1) is 5-15 times the mass of the soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 .
进一步限定，步骤（2）的混合溶液中硝酸铋的摩尔浓度为0.05mol/L。 Further defined, the molar concentration of bismuth nitrate in the mixed solution in step (2) is 0.05mol/L.
进一步限定，步骤（2）中加入负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土的量为Bi2O2CO3质量的1-3倍。 It is further defined that the amount of kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 added in step (2) is 1-3 times the mass of Bi 2 O 2 CO 3 .
本发明与现有技术相比具有以下显著优点：1、高岭土较强的吸附吸性能可以维持Bi2O2CO3悬浮体系较高的光催化效率；2、利用磁性技术来回收光催化剂，简化分离过程，降低操作费用；3、本发明方法简单，易于控制且成本低廉。 Compared with the prior art, the present invention has the following significant advantages: 1. The strong adsorption and absorption performance of kaolin can maintain the higher photocatalytic efficiency of the Bi 2 O 2 CO 3 suspension system; 2. Use magnetic technology to recover photocatalysts, simplifying The separation process reduces operating costs; 3. The method of the present invention is simple, easy to control and low in cost.
具体实施方式 Detailed ways
以下结合实施例进一步描述本发明，应该指出，本发明并非局限于下述各实施例。 The present invention is further described below in conjunction with the examples. It should be noted that the present invention is not limited to the following examples.
实施例1 Example 1
（1）将物质的量分别为0.1×10-2mol、0.1×10-2mol和0.4×10-2mol的硝酸锰、硝酸锌和硝酸铁用去离子水配成混合溶液，混合溶液中硝酸锌的摩尔浓度为0.01mol/L，再向混合溶液中加入相当于上述体系软磁性Mn0.5Zn0.5Fe2O4质量5倍的高岭土，然后向混合体系中加入0.3×10-2mol EDTA，将所得的混合体系在80℃的水浴中保持12h得到湿凝胶，湿凝胶经110℃干燥得到干凝胶，然后将干凝胶于500℃煅烧2h后得到负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土； (1) Mix manganese nitrate, zinc nitrate and ferric nitrate with the amount of 0.1×10 -2 mol, 0.1×10 -2 mol and 0.4×10 -2 mol respectively with deionized water to form a mixed solution. The molar concentration of zinc nitrate is 0.01mol/L, and kaolin equivalent to 5 times the mass of the soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 of the above system is added to the mixed solution, and then 0.3×10 -2 mol EDTA is added to the mixed solution , keep the resulting mixed system in a water bath at 80°C for 12h to obtain a wet gel, dry the wet gel at 110°C to obtain a xerogel, and then calcinate the xerogel at 500°C for 2h to obtain a soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 kaolin;
（2）在搅拌条件下将物质的量分别为0.55×10-2mol和1.65×10-2mol的硝酸铋和尿素用去离子水配成混合溶液，混合溶液中硝酸铋的摩尔浓度为0.05mol/L，向混合溶液中加入氨水调节混合溶液的pH值为4，然后加入1.415g步骤（1）制得的负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土，将所得的混合体系转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于180℃微波反应30min，经冷却、过滤、洗涤、干燥后得到具有高催化活性的负载型Bi2O2CO3光催化剂。 (2) Mix bismuth nitrate and urea with deionized water in amounts of 0.55×10 -2 mol and 1.65×10 -2 mol respectively under stirring conditions to form a mixed solution, and the molar concentration of bismuth nitrate in the mixed solution is 0.05 mol/L, add ammonia water to the mixed solution to adjust the pH value of the mixed solution to 4, then add 1.415g of kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 prepared in step (1), and mix the resulting mixed system Transfer to a hydrothermal reaction kettle, then put the hydrothermal reaction kettle into a microwave digestion apparatus and react with microwave at 180°C for 30 minutes, after cooling, filtering, washing and drying, the supported Bi 2 O 2 CO 3 with high catalytic activity was obtained catalyst of light.
实施例2 Example 2
（1）将物质的量分别为0.1×10-2mol、0.1×10-2mol和0.4×10-2mol的硝酸锰、硝酸锌和硝酸铁用去离子水配成混合溶液，混合溶液中硝酸锌的摩尔浓度为0.01mol/L，再向混合溶液中加入相当于上述体系软磁性Mn0.5Zn0.5Fe2O4质量10倍的高岭土，然后向混合体系中加入0.3×10-2mol EDTA，将所得的混合体系在80℃的水浴中保持12h得到湿凝胶，湿凝胶经110℃干燥得到干凝胶，然后将干凝胶于500℃煅烧2h后得到负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土； (1) Mix manganese nitrate, zinc nitrate and ferric nitrate with the amount of 0.1×10 -2 mol, 0.1×10 -2 mol and 0.4×10 -2 mol respectively with deionized water to form a mixed solution. The molar concentration of zinc nitrate is 0.01mol/L, and kaolin equivalent to 10 times the mass of the soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 of the above system is added to the mixed solution, and then 0.3×10 -2 mol EDTA is added to the mixed solution , keep the resulting mixed system in a water bath at 80°C for 12h to obtain a wet gel, dry the wet gel at 110°C to obtain a xerogel, and then calcinate the xerogel at 500°C for 2h to obtain a soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 kaolin;
（2）在搅拌条件下将物质的量分别为0.55×10-2mol和1.65×10-2mol的硝酸铋和尿素用去离子水配成混合溶液，混合溶液中硝酸铋的摩尔浓度为0.05mol/L，向混合溶液中加入氨水调节混合溶液的pH值为4，然后加入2.594g步骤（1）制得的负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土，将所得的混合体系转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于180℃微波反应20min，经冷却、过滤、洗涤、干燥后得到具有高催化活性的负载型Bi2O2CO3光催化剂。 (2) Mix bismuth nitrate and urea with deionized water in amounts of 0.55×10 -2 mol and 1.65×10 -2 mol respectively under stirring conditions to form a mixed solution, and the molar concentration of bismuth nitrate in the mixed solution is 0.05 mol/L, add ammonia water to the mixed solution to adjust the pH value of the mixed solution to 4, then add 2.594g of kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 prepared in step (1), and mix the resulting mixed system Transfer to a hydrothermal reaction kettle, then put the hydrothermal reaction kettle into a microwave digestion apparatus and react with microwave at 180°C for 20 minutes, after cooling, filtering, washing and drying, the supported Bi 2 O 2 CO 3 with high catalytic activity is obtained catalyst of light.
实施例3 Example 3
（1）将物质的量分别为0.1×10-2mol、0.1×10-2mol和0.4×10-2mol的硝酸锰、硝酸锌和硝酸铁用去离子水配成混合溶液，混合溶液中硝酸锌的摩尔浓度为0.01mol/L，再向混合溶液中加入相当于上述体系软磁性Mn0.5Zn0.5Fe2O4质量15倍的高岭土，然后向混合体系中加入0.3×10-2mol EDTA，将所得的混合体系在80℃的水浴中保持12h得到湿凝胶，湿凝胶经110℃干燥得到干凝胶，然后将干凝胶在500℃煅烧2h后得到负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土； (1) Mix manganese nitrate, zinc nitrate and ferric nitrate with the amount of 0.1×10 -2 mol, 0.1×10 -2 mol and 0.4×10 -2 mol respectively with deionized water to form a mixed solution. The molar concentration of zinc nitrate is 0.01mol/L, and kaolin equivalent to 15 times the mass of the soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 of the above system is added to the mixed solution, and then 0.3×10 -2 mol EDTA is added to the mixed solution , the resulting mixed system was kept in a water bath at 80°C for 12h to obtain a wet gel, and the wet gel was dried at 110°C to obtain a xerogel, and then the xerogel was calcined at 500°C for 2h to obtain a soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 kaolin;
（2）在搅拌条件下将物质的量分别为0.55×10-2mol和1.65×10-2mol的硝酸铋和尿素用去离子水配成混合溶液，混合溶液中硝酸铋的摩尔浓度为0.05mol/L，向混合溶液中加入氨水调节混合溶液的pH值为4，然后加入3.82g步骤（2）制得的负载有软磁性Mn0.5Zn0.5Fe2O4的高岭土，将所得的混合体系转移至水热反应釜中，然后将水热反应釜放入微波消解仪中于200℃微波反应10min，经冷却、过滤、洗涤、干燥后得到具有高催化活性的负载型Bi2O2CO3光催化剂。 (2) Mix bismuth nitrate and urea with deionized water in amounts of 0.55×10 -2 mol and 1.65×10 -2 mol respectively under stirring conditions to form a mixed solution, and the molar concentration of bismuth nitrate in the mixed solution is 0.05 mol/L, add ammonia water to the mixed solution to adjust the pH value of the mixed solution to 4, then add 3.82g of kaolin loaded with soft magnetic Mn 0.5 Zn 0.5 Fe 2 O 4 prepared in step (2), and mix the resulting mixed system Transfer to a hydrothermal reaction kettle, then put the hydrothermal reaction kettle into a microwave digestion apparatus and react with microwave at 200°C for 10 minutes, after cooling, filtering, washing and drying, the supported Bi 2 O 2 CO 3 with high catalytic activity is obtained catalyst of light.
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。 The above embodiments have described the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. What are described in the above embodiments and description are only to illustrate the principles of the present invention. Without departing from the scope of the principle of the present invention, there will be various changes and improvements in the present invention, and these changes and improvements all fall within the protection scope of the present invention.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105749945A (en) * | 2016-03-16 | 2016-07-13 | 湖北文理学院 | A Preparation Method of Fe(Ш)/Bi2O2CO3 Photocatalyst |
| CN105772051A (en) * | 2016-04-18 | 2016-07-20 | 河南师范大学 | A kind of Bi2O2CO3-BiFeO3 composite photocatalyst and preparation method thereof |
| CN105797760A (en) * | 2016-04-18 | 2016-07-27 | 河南师范大学 | A kind of Bi2O2CO3-WO3 composite photocatalyst and preparation method thereof |
| CN106186061A (en) * | 2016-06-09 | 2016-12-07 | 辽宁石油化工大学 | A method for stabilizing Bi2O2CO3 at high temperature |
| CN106423180A (en) * | 2016-10-12 | 2017-02-22 | 洛阳鼎威材料科技有限公司 | Kaoline and perovskite composite material and preparing method thereof |
| CN109331836A (en) * | 2018-10-10 | 2019-02-15 | 重庆大学 | A new method for preparing β-Bi2O3/MnxZn1-xFe2O4 composite magnetic photocatalytic material |
| CN110745879A (en) * | 2018-07-23 | 2020-02-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of Mg2+ doped basic nickel carbonate microspheres |
| CN112808287A (en) * | 2021-01-31 | 2021-05-18 | 湖南科技大学 | Magnetic core-shell type bismuth oxycarbonate/sepiolite composite photocatalyst and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4914392A (en) * | 1972-05-23 | 1974-02-07 |
-
2015
- 2015-06-03 CN CN201510298200.4A patent/CN104998671A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4914392A (en) * | 1972-05-23 | 1974-02-07 |
Non-Patent Citations (6)
| Title |
|---|
| GANGQIANG ZHU等: "Heterostructured Fe3O4/Bi2O2CO3 photocatalyst: Synthesis, characterization and application in recyclable photodegradation of organic dyes under visible light irradiation", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| PUTTASWAMY MADHUSUDAN等: "Novel urea assisted hydrothermal synthesis of hierarchical BiVO4/Bi2O2CO3 nanocomposites with enhanced visible-light photocatalytic activity", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
| 姚仲鹏 著: "《空气净化原理、设计与应用》", 30 September 2014, 中国科学技术出版社 * |
| 席国喜等: "EDTA络合溶胶-凝胶法制备Mn-Zn铁氧体", 《硅酸盐通报》 * |
| 杨保祥 编著: "《钛基材料制造》", 31 January 2015, 冶金工业出版社 * |
| 马惠言 等: "载体对负载型催化剂的光催化活性影响研究", 《内蒙古工业大学学报》 * |
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| CN105797760A (en) * | 2016-04-18 | 2016-07-27 | 河南师范大学 | A kind of Bi2O2CO3-WO3 composite photocatalyst and preparation method thereof |
| CN106186061A (en) * | 2016-06-09 | 2016-12-07 | 辽宁石油化工大学 | A method for stabilizing Bi2O2CO3 at high temperature |
| CN106423180A (en) * | 2016-10-12 | 2017-02-22 | 洛阳鼎威材料科技有限公司 | Kaoline and perovskite composite material and preparing method thereof |
| CN110745879A (en) * | 2018-07-23 | 2020-02-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of Mg2+ doped basic nickel carbonate microspheres |
| CN109331836A (en) * | 2018-10-10 | 2019-02-15 | 重庆大学 | A new method for preparing β-Bi2O3/MnxZn1-xFe2O4 composite magnetic photocatalytic material |
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