CN106238050A - Copper oxide/Red copper oxide composite photocatalyst material and preparation method thereof - Google Patents
Copper oxide/Red copper oxide composite photocatalyst material and preparation method thereof Download PDFInfo
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 72
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 34
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 23
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 title abstract description 5
- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 title 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 229940112669 cuprous oxide Drugs 0.000 claims abstract description 71
- 230000001699 photocatalysis Effects 0.000 claims abstract description 34
- 239000012266 salt solution Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- 229960004643 cupric oxide Drugs 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 14
- 235000002639 sodium chloride Nutrition 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 239000010949 copper Substances 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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Abstract
本发明公开了一种氧化铜/氧化亚铜复合光催化材料及其制备方法。在一较佳实施案例之中，该制备方法包括：将氧化亚铜粉体分散于盐溶液中，并在0℃～95℃持续搅拌反应0.01～240h，之后分离出反应产物，再洗涤、干燥，获得所述氧化铜/氧化亚铜复合光催化材料。本发明通过利用环保廉价的盐溶液对氧化亚铜表面进行轻微氧化处理来制备氧化铜/氧化亚铜复合光催化剂，制备过程简单，反应过程温和容易控制，反应物廉价环保，不仅可完整的保持氧化亚铜原有形貌，还能精确控制氧化铜含量，确保氧化亚铜活性面的暴露，光催化活性高，循环稳定性好，在光催化领域具有广泛应用前景。
The invention discloses a copper oxide/cuprous oxide composite photocatalytic material and a preparation method thereof. In a preferred embodiment, the preparation method includes: dispersing the cuprous oxide powder in the salt solution, and continuously stirring and reacting at 0°C-95°C for 0.01-240h, and then separating the reaction product, washing and drying , to obtain the copper oxide/cuprous oxide composite photocatalytic material. The present invention prepares a cuprous oxide/cuprous oxide composite photocatalyst by slightly oxidizing the surface of cuprous oxide with an environmentally friendly and cheap salt solution. The preparation process is simple, the reaction process is mild and easy to control, and the reactants are cheap and environmentally friendly. The original shape of cuprous oxide can also precisely control the content of copper oxide to ensure the exposure of the active surface of cuprous oxide. It has high photocatalytic activity and good cycle stability, and has broad application prospects in the field of photocatalysis.
Description
技术领域technical field
本发明具体涉及一种氧化铜/氧化亚铜复合光催化材料及其制备方法，属于纳米材料科学领域。The invention specifically relates to a copper oxide/cuprous oxide composite photocatalytic material and a preparation method thereof, which belong to the field of nanometer material science.
背景技术Background technique
氧化亚铜是一种重要的P型半导体，禁带宽度为2.0～2.2eV，在可将光区有很强的吸收，并且无毒、价廉和制备简单，因而在光催化、气敏传感器和太阳能电池等领域有着很好的应用前景。但是，单一的氧化亚铜作为光催化剂仍然难以满足实际应用的要求，复合光催化剂能够解决单一组分催化剂诸多不足。在不同类型的氧化亚铜复合光催化材料中，氧化铜/氧化亚铜(CuO/Cu2O)复合光催化材料是制备相对简单，反应最容易控制的。Cuprous oxide is an important P-type semiconductor with a forbidden band width of 2.0-2.2eV. It has strong absorption in the light-absorbing region, and is non-toxic, cheap and easy to prepare. Therefore, it is used in photocatalysis and gas sensors. And solar cells and other fields have good application prospects. However, single cuprous oxide as a photocatalyst is still difficult to meet the requirements of practical applications, and composite photocatalysts can solve many shortcomings of single-component catalysts. Among different types of cuprous oxide composite photocatalytic materials, cuprous oxide/cuprous oxide (CuO/Cu 2 O) composite photocatalytic materials are relatively simple to prepare and the reaction is most easily controlled.
目前，制备CuO/Cu2O复合材料通常在水热条件下，通过控制还原剂与铜盐的比例一步得到(如CN103466682A和CN102180509A)。这种方法虽然步骤少，但是通常需要较高的反应温度，而且水热条件下很难对产物组分，以及氧化铜和氧化亚铜形貌同时进行精确的调控。另外，可通过对预先合成氧化亚铜进行氧化的两步法得到CuO/Cu2O复合材料，如氧化亚铜与NaOH溶液反应(Cryst.Eng.Comm.,2013,15,p7462-7467)或空气中氧化煅烧(J.Mater.Chem.A.2015,3,p5294-5298)。现有的这些两步法，虽然可以预先制备特定形貌的氧化亚铜，但是反应通常较为剧烈，大量的氧化亚铜表面被氧化铜覆盖，不利于氧化亚铜活性点位暴露，光催化性能提高受到影响。At present, the preparation of CuO/Cu 2 O composite materials is usually obtained in one step by controlling the ratio of reducing agent and copper salt under hydrothermal conditions (such as CN103466682A and CN102180509A). Although this method has fewer steps, it usually requires a higher reaction temperature, and it is difficult to precisely control the product components and the morphology of cupric oxide and cuprous oxide under hydrothermal conditions. In addition, CuO/Cu 2 O composites can be obtained by a two-step method of oxidizing pre-synthesized cuprous oxide, such as the reaction of cuprous oxide with NaOH solution (Cryst. Eng. Comm., 2013, 15, p7462-7467) or Oxidative calcination in air (J. Mater. Chem. A. 2015, 3, p5294-5298). Although these existing two-step methods can prepare cuprous oxide with specific morphology in advance, the reaction is usually more violent, and a large amount of cuprous oxide surface is covered by copper oxide, which is not conducive to the exposure of cuprous oxide active sites, and the photocatalytic performance Improvement is affected.
发明内容Contents of the invention
本发明的目的在于提供一种氧化铜/氧化亚铜复合光催化材料及其制备方法，以克服现有技术中的不足。The object of the present invention is to provide a cupric oxide/cuprous oxide composite photocatalytic material and a preparation method thereof, so as to overcome the deficiencies in the prior art.
为实现前述发明目的，本发明的一实施案例之中提供了一种氧化铜/氧化亚铜复合光催化材料的制备方法，其包括：将氧化亚铜浸渍于盐溶液中，并在0℃～95℃反应0.01～240h，获得所述氧化铜/氧化亚铜复合光催化材料。In order to achieve the purpose of the aforementioned invention, an embodiment of the present invention provides a method for preparing a copper oxide/cuprous oxide composite photocatalytic material, which includes: immersing cuprous oxide in a salt solution, and React at 95° C. for 0.01 to 240 hours to obtain the copper oxide/cuprous oxide composite photocatalytic material.
作为较为优选的实施方案之一，该制备方法包括：将氧化亚铜粉体分散于盐溶液中，并在0℃～95℃持续搅拌反应0.01～240h，获得所述氧化铜/氧化亚铜复合光催化材料。As one of the more preferred embodiments, the preparation method includes: dispersing cuprous oxide powder in a salt solution, and continuously stirring and reacting at 0°C to 95°C for 0.01 to 240h to obtain the cuprous oxide/cuprous oxide composite photocatalytic material.
进一步的，所述盐溶液包含盐的水溶液，所述盐可优选自但不限于氯化钠、硫酸钠、硝酸钠、氯化钾、硫酸钾、硝酸钾中的任意一种或两种以上的组合。Further, the salt solution includes an aqueous solution of salt, and the salt may be preferably selected from any one or more than two of sodium chloride, sodium sulfate, sodium nitrate, potassium chloride, potassium sulfate, and potassium nitrate. combination.
更为优选的，所述盐溶液的浓度为0.1mM～5M。More preferably, the concentration of the salt solution is 0.1mM-5M.
更为优选的，所述盐溶液中所含盐与氧化亚铜的摩尔比为1000～0.001：1。More preferably, the molar ratio of salt to cuprous oxide contained in the salt solution is 1000-0.001:1.
在一更为具体的实施方案之中，该制备方法可以包括：将氧化亚铜粉体分散于盐溶液中，并在0℃～95℃持续搅拌反应0.01～240h，之后分离出反应产物，再洗涤、干燥，获得所述氧化铜/氧化亚铜复合光催化材料。In a more specific embodiment, the preparation method may include: dispersing the cuprous oxide powder in the salt solution, and continuously stirring and reacting at 0°C to 95°C for 0.01 to 240h, then separating the reaction product, and then washing and drying to obtain the copper oxide/cuprous oxide composite photocatalytic material.
在本发明中所采用的氧化亚铜可以是任何合适形态的，例如片层状、块体、粉体，优选为粉体。另外，本发明可采用纯氧化亚铜材料，亦可以采用氧化亚铜与其它材料复合形成的材料，例如表层包覆有氧化亚铜的颗粒材料、片层材料、块状材料等。The cuprous oxide used in the present invention can be in any suitable form, such as lamellar, block, powder, preferably powder. In addition, the present invention can use pure cuprous oxide material, and can also use cuprous oxide and other materials compounded, such as granular materials, sheet materials, block materials and the like coated with cuprous oxide on the surface.
本发明的另一实施案例之中还提供了由前述任一种方法制备的氧化铜/氧化亚铜复合光催化材料。Another embodiment of the present invention also provides a copper oxide/cuprous oxide composite photocatalytic material prepared by any one of the aforementioned methods.
与现有技术相比，本发明的优点包括：通过利用环保廉价的盐溶液对氧化亚铜表面进行轻微氧化(或认为是刻蚀)处理来制备氧化铜/氧化亚铜复合光催化剂，制备过程简单，反应过程温和容易控制，反应物廉价环保，不仅可完整的保持氧化亚铜原有形貌，还能精确控制氧化铜含量，确保氧化亚铜活性面的暴露，催化活性高，循环稳定性好。Compared with the prior art, the advantages of the present invention include: preparing a cuprous oxide/cuprous oxide composite photocatalyst by utilizing an environmentally friendly and cheap salt solution to slightly oxidize (or consider etching) the surface of cuprous oxide. It is simple, the reaction process is mild and easy to control, and the reactants are cheap and environmentally friendly. It can not only completely maintain the original shape of cuprous oxide, but also accurately control the content of cuprous oxide to ensure the exposure of the active surface of cuprous oxide. High catalytic activity and cycle stability it is good.
附图说明Description of drawings
图1为实施例1制备的氧化铜/氧化亚铜复合光催化材料的扫描电镜图；Fig. 1 is the scanning electron micrograph of the cupric oxide/cuprous oxide composite photocatalytic material that embodiment 1 prepares;
图2为实施例1制备的氧化铜/氧化亚铜复合光催化材料的XRD图；Fig. 2 is the XRD pattern of the cupric oxide/cuprous oxide composite photocatalytic material prepared in embodiment 1;
图3为实施例1制备的氧化铜/氧化亚铜复合光催化材料的对甲基橙的光催化降解图；Fig. 3 is the photocatalytic degradation figure to methyl orange of the cupric oxide/cuprous oxide composite photocatalytic material that embodiment 1 prepares;
图4为实施例1制备的氧化铜/氧化亚铜复合光催化材料的对甲基橙的光催化循环降解图。4 is a photocatalytic cycle degradation diagram of methyl orange of the copper oxide/cuprous oxide composite photocatalytic material prepared in Example 1.
具体实施方式detailed description
本发明的一典型实施案例之中提供了一种氧化铜/氧化亚铜复合光催化材料的制备方法，其可以包括以下步骤：A typical implementation of the present invention provides a method for preparing a copper oxide/cuprous oxide composite photocatalytic material, which may include the following steps:
(1)将一定量的氧化亚铜分散在盐溶液中，在0℃～95℃搅拌反应0.01～120h；(1) Disperse a certain amount of cuprous oxide in the salt solution, and stir and react at 0°C-95°C for 0.01-120h;
(2)将反应产物离心、洗涤和干燥后，即得到氧化铜/氧化亚铜复合光催化材料；(2) After the reaction product is centrifuged, washed and dried, the copper oxide/cuprous oxide composite photocatalytic material is obtained;
前述的“一定量”是指：盐溶液与氧化亚铜的摩尔比为1000～0.001：1。The aforementioned "a certain amount" means that the molar ratio of salt solution to cuprous oxide is 1000-0.001:1.
较为优选的，所述盐溶液可以选自：摩尔浓度为0.1mM～5M的氯化钠、硫酸钠、硝酸钠、氯化钾、硫酸钾或硝酸钾水溶液。More preferably, the salt solution can be selected from: aqueous solutions of sodium chloride, sodium sulfate, sodium nitrate, potassium chloride, potassium sulfate or potassium nitrate with a molar concentration of 0.1 mM-5M.
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。The following is a detailed description of the embodiments of the present invention. This embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to the following implementation example.
实施例1Example 1
43.3mg氧化亚铜立方体加入到5ml，0.2M氯化钠水溶液中超声分散，室温下搅拌反应12h。产物离心清洗后真空干燥。经扫描电镜(请参阅图1所示)和XRD(请参阅图2所示)分析：氧化亚铜仍然保持完整的立方体形貌，光滑的表面生成片状或逐渐长大成三角锥状产物，而且没有完全覆盖氧化亚铜表面，经XRD分析，生成的产物是氧化铜，即，获得了氧化铜/氧化亚铜复合光催化材料(CuO/Cu2O，如下简称样品)。请参阅图3所示，本实施例的样品在120分钟内能够将甲基橙几乎完全降解，而且样品暗吸附实验也表明在120分钟内样品几乎无吸附，说光照下的降解完全是由光催化引起的。另外，请参阅图4，本实施例的样品经过四次循环后催化活性没有降低，证明其具有良好的光催化稳定性。Add 43.3 mg of cuprous oxide cubes into 5 ml of 0.2 M sodium chloride aqueous solution for ultrasonic dispersion, and stir at room temperature for 12 h. The product was cleaned by centrifugation and dried in vacuum. Analyzed by scanning electron microscopy (see Figure 1) and XRD (see Figure 2): cuprous oxide still maintains a complete cubic shape, and the smooth surface generates flakes or gradually grows into triangular pyramid-shaped products, and The surface of the cuprous oxide is not completely covered, and the product formed is copper oxide according to XRD analysis, that is, a copper oxide/cuprous oxide composite photocatalytic material (CuO/Cu 2 O, hereinafter referred to as the sample) is obtained. Please refer to Figure 3, the sample of this embodiment can degrade methyl orange almost completely within 120 minutes, and the dark adsorption experiment of the sample also shows that the sample has almost no adsorption within 120 minutes, which means that the degradation under light is completely caused by light. caused by catalysis. In addition, please refer to FIG. 4 , the catalytic activity of the sample in this example did not decrease after four cycles, which proves that it has good photocatalytic stability.
实施例2Example 2
43.3mg氧化亚铜立方体加入到5ml，0.1mM氯化钾水溶液中超声分散，70℃下搅拌反应8h，产物离心清洗后真空干燥。Add 43.3mg of cuprous oxide cubes into 5ml, 0.1mM potassium chloride aqueous solution for ultrasonic dispersion, stir and react at 70°C for 8h, and vacuum-dry the product after centrifugal cleaning.
实施例3Example 3
43.3mg氧化亚铜八面体加入到5ml，50mM氯化钠水溶液中超声分散，0℃下搅拌反应240h，产物离心清洗后真空干燥。Add 43.3mg cuprous oxide octahedron into 5ml, 50mM sodium chloride aqueous solution for ultrasonic dispersion, stir and react at 0°C for 240h, and vacuum-dry the product after centrifugal washing.
实施例4Example 4
43.3mg氧化亚铜八面体加入到5ml，1M硫酸钠水溶液中超声分散，95℃下搅拌反应0.01h，产物离心清洗后真空干燥。Add 43.3mg cuprous oxide octahedron into 5ml, 1M sodium sulfate aqueous solution, ultrasonically disperse, stir and react at 95°C for 0.01h, and vacuum-dry the product after centrifugal cleaning.
实施例5Example 5
43.3mg氧化亚铜截角八面体加入到5ml，5M硝酸钠水溶液中超声分散，50℃下搅拌反应6h。产物离心清洗后真空干燥。Add 43.3mg cuprous oxide truncated octahedron into 5ml, 5M sodium nitrate aqueous solution for ultrasonic dispersion, and stir at 50°C for 6h. The product was cleaned by centrifugation and dried in vacuum.
需要说明的是，在本说明书之中，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。It should be noted that, in this specification, the terms "comprising", "comprising" or any other variant thereof are intended to cover a non-exclusive inclusion, so that a process, method, article or device comprising a series of elements not only includes those elements, but also other elements not expressly listed, or elements inherent in the process, method, article, or apparatus.
应当理解，以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。It should be understood that the above description is only a preferred embodiment of the present invention. It should be pointed out that for those skilled in the art, some improvements and modifications can be made without departing from the principle of the present invention. These improvements And retouching should also be regarded as the protection scope of the present invention.
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