CN110560096B - A kind of graphene oxide photocatalytic material supporting bismuth heterojunction and its preparation method and application - Google Patents
A kind of graphene oxide photocatalytic material supporting bismuth heterojunction and its preparation method and application Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 title claims abstract description 23
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 16
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011941 photocatalyst Substances 0.000 claims abstract description 20
- 239000002135 nanosheet Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 150000001621 bismuth Chemical class 0.000 claims abstract description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
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Abstract
本发明公开了一种负载铋系异质结的氧化石墨烯光催化材料的制备方法，包括以下步骤：首先制备BiOI/BixNbOy光催化剂和氧化石墨烯，将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上，以负载后的石墨烯纳米片为前驱体，对预冷冻处理后的化合物进行真空干燥处理，得到具有高强度的负载铋系异质结的氧化石墨烯光催化材料。本发明负载铋系异质结的氧化石墨烯光催化材料具有高强度、高比表面积和强吸附等特点，可以有效解决粉末状光催化剂在使用后难以分离和回收利用的难题，避免了纳米材料对环境造成的二次污染等问题；有利于提高光催化反应速率；提高了催化剂光生载流子的分离率，增加了光催化剂的的稳定性，拓宽了光谱响应范围。
The invention discloses a preparation method of a graphene oxide photocatalytic material supported with a bismuth series heterojunction, comprising the following steps: firstly preparing a BiOI/BixNbOy photocatalyst and graphene oxide, and loading the synthesized BiOI/BixNbOy heterojunction catalyst On graphene oxide nanosheets, the loaded graphene nanosheets are used as precursors, and the pre-freezing compound is subjected to vacuum drying to obtain graphene oxide photocatalytic materials with high-strength supported bismuth heterojunctions. The graphene oxide photocatalytic material loaded with bismuth series heterojunction has the characteristics of high strength, high specific surface area, strong adsorption, etc., can effectively solve the problem that the powder photocatalyst is difficult to separate and recycle after use, and avoids nanomaterials It is beneficial to improve the photocatalytic reaction rate, improve the separation rate of photogenerated carriers of the catalyst, increase the stability of the photocatalyst, and broaden the spectral response range.
Description
技术领域technical field
本发明涉及一种光催化材料的制备方法，具体为一种负载铋系异质结的氧化石墨烯光催化材料的制备与应用。The invention relates to a preparation method of a photocatalytic material, in particular to the preparation and application of a graphene oxide photocatalytic material supported with a bismuth series heterojunction.
背景技术Background technique
持久性有机污染物(persistent organic pollutants，简称POPs)是对具有长期残留性和大范围迁移性、生物蓄积性、半挥发性及对生物体有高毒性的一类天然的或人工合成的有机物及其衍生物的统称，POPs污染逐渐成为目前国际上备受关注的新的全球性环境问题。随着国内工农业经济的高速发展,有关水体中POPs经各种途径的排放量不断上升，污染状况呈现恶化趋势，造成的健康问题日趋严重，调查研究表明，地表水环境普遍受到持久性有机物的污染，水源水、地下水水质也面临严峻的考验。Persistent organic pollutants (POPs) are a class of natural or artificially synthesized organic compounds with long-term residual and large-scale migration, bioaccumulation, semi-volatile and high toxicity to living organisms. The general term for its derivatives, POPs pollution has gradually become a new global environmental problem that has attracted international attention. With the rapid development of domestic industrial and agricultural economy, the discharge of POPs in relevant water bodies through various channels continues to rise, the pollution situation is showing a worsening trend, and the resulting health problems are becoming more and more serious. Investigations show that the surface water environment is generally affected by persistent organic compounds Pollution, source water and groundwater quality are also facing severe challenges.
光催化降解是POPs在环境中的重要转化途径，也是最常用的化学降解方法。现有的常规光催化剂、铌系、铋系复合氧化物或异质结，氧化石墨烯基复合催化剂等，但都具有一定的不足。因此，制备具有无毒稳定、催化活性高、绿色能源利用率高及循环利用性能好的新型光催化剂，对于实现水中POPs的高效降解具有重要意义。本发明旨在制备一种具有高效催化性能的负载铋系异质结的氧化石墨烯光催化材料。Photocatalytic degradation is an important transformation pathway of POPs in the environment, and it is also the most commonly used chemical degradation method. Existing conventional photocatalysts, niobium-based, bismuth-based composite oxides or heterojunctions, graphene oxide-based composite catalysts, etc., all have certain deficiencies. Therefore, the preparation of novel photocatalysts with non-toxic and stable properties, high catalytic activity, high green energy utilization rate, and good recycling performance is of great significance for realizing the efficient degradation of POPs in water. The present invention aims to prepare a graphene oxide photocatalytic material supported by bismuth series heterojunction with high catalytic performance.
发明内容SUMMARY OF THE INVENTION
本发明的目的是为了克服现有光催化材料的光谱响应范围较窄、循环利用性差、产生水体二次污染、载流子分离效率低等不足，提供了一种高效的负载铋系异质结的氧化石墨烯光催化材料的制备方法。The purpose of the present invention is to overcome the shortcomings of the existing photocatalytic materials such as narrow spectral response range, poor recyclability, secondary water pollution, and low carrier separation efficiency, and provides a highly efficient supported bismuth-based heterojunction. The preparation method of the graphene oxide photocatalytic material.
本发明通过以下技术方案实现。The present invention is realized by the following technical solutions.
一种负载铋系异质结的氧化石墨烯光催化材料的制备方法，包括以下步骤：A preparation method of a graphene oxide photocatalytic material supporting a bismuth-based heterojunction, comprising the following steps:
首先制备BiOI/BixNbOy光催化剂和氧化石墨烯，将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上，以负载后的石墨烯纳米片为前驱体，借助定向真空冷冻干燥技术，对预冷冻处理后的化合物进行真空干燥处理，即可得到具有高强度的负载铋系异质结的氧化石墨烯光催化材料。Firstly, BiOI / BixNbOy photocatalyst and graphene oxide were prepared, and the synthesized BiOI/BixNbOy heterojunction catalyst was loaded on graphene oxide nanosheets, and the loaded graphene nanosheets were used as precursors, and the directional vacuum freeze-drying was carried out. technology, vacuum drying the pre-freezing compound to obtain a graphene oxide photocatalytic material with high-strength supported bismuth heterojunction.
优选地，采用Nb2O5和Bi(NO3)3·5H2O制备BiOI/BixNbOy光催化剂。Preferably, the BiOI / BixNbOy photocatalyst is prepared using Nb 2 O 5 and Bi(NO 3 ) 3 .5H 2 O.
优选地，BiOI/BixNbOy光催化剂的制备过程中分别添加不同的表面活性剂或者分别控制不同的反应条件(如反应温度，时间，反应物配比等)合成具有不同晶型的BiOI/BixNbOy异质结光催化剂。Preferably, in the preparation process of BiOI / BixNbOy photocatalyst, different surfactants are respectively added or different reaction conditions (such as reaction temperature, time, ratio of reactants, etc.) are respectively controlled to synthesize BiOI/BiOI/BiOI with different crystal forms. Bi x NbO y heterojunction photocatalysts.
优选地，所述表面活性剂为柠檬酸钠、十二烷基苯磺酸钠或溴化十六烷基三甲胺。Preferably, the surfactant is sodium citrate, sodium dodecylbenzenesulfonate or cetyltrimethylamine bromide.
优选地，在真空冷冻干燥的过程中，真空度为3.3～13pa。Preferably, in the process of vacuum freeze-drying, the degree of vacuum is 3.3-13 Pa.
一种上述方法制备的负载铋系异质结的氧化石墨烯光催化材料。A graphene oxide photocatalytic material supporting bismuth-based heterojunction prepared by the above method.
上述负载铋系异质结的氧化石墨烯光催化材料主要应用于对水体POPs的降解。The above-mentioned bismuth-based heterojunction-loaded graphene oxide photocatalytic material is mainly used for the degradation of POPs in water.
本发明制备方法中BiOI/BixNbOy的负载结合定向真空冷冻干燥技术，可大幅度提高石墨烯基催化剂的机械强度。In the preparation method of the present invention, the loading of BiOI / BixNbOy combined with the directional vacuum freeze-drying technology can greatly improve the mechanical strength of the graphene-based catalyst.
上述制备方法中氧化石墨烯基负载可以提高BiOI/BixNbOy催化剂的分散程度和分散均匀性。The graphene oxide-based loading in the above preparation method can improve the dispersion degree and dispersion uniformity of the BiOI / BixNbOy catalyst.
与现有技术相比，本发明所提供的技术方案的优点在于：Compared with the prior art, the advantages of the technical solution provided by the present invention are:
(1)构筑的负载铋系异质结的氧化石墨烯光催化材料具有高强度、高比表面积和强吸附等特点，可以有效解决粉末状光催化剂在使用后难以分离和回收利用的难题，避免了纳米材料对环境造成的二次污染等问题。(1) The constructed graphene oxide photocatalytic material supported by bismuth heterojunction has the characteristics of high strength, high specific surface area and strong adsorption, which can effectively solve the problem that the powder photocatalyst is difficult to separate and recycle after use. The problem of secondary pollution caused by nanomaterials to the environment has been solved.
(2)氧化石墨烯负载体比传统光催化剂载体(如活性炭)更易于传质，有利于提高光催化反应速率。(2) Graphene oxide supports are easier to transfer mass than traditional photocatalyst supports (such as activated carbon), which is beneficial to improve the photocatalytic reaction rate.
(3)利用高强度的氧化石墨烯作为BiOI/BixNbOy的载体，结合了两者优异的光电性质和结构特质，提高了催化剂光生载流子的分离率，增加了光催化剂的的稳定性，拓宽了光谱响应范围。(3) Using high-strength graphene oxide as the carrier of BiOI / BixNbOy , which combines the excellent optoelectronic properties and structural characteristics of the two, improves the separation rate of photogenerated carriers of the catalyst, and increases the stability of the photocatalyst. , broadening the spectral response range.
附图说明Description of drawings
图1为GO-BiOI/BixNbOy光催化剂的合成及其对POPs的降解机理图。Figure 1 shows the synthesis of GO- BiOI / BixNbOy photocatalyst and its degradation mechanism for POPs.
具体实施方式Detailed ways
实施例1Example 1
首先，采用溶剂热法制备BiOI/BixNbOy光催化剂(制备过程中添加表面活性剂柠檬酸钠)，然后，采用改进的Hummers法制备氧化石墨烯。将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上。再次，以负载后的石墨烯纳米片为前驱体，借助定向真空冷冻干燥技术，在真空度为3.3Pa下，进行真空干燥，即可得到高强度的负载铋系异质结的石墨烯光催化材料。First, BiOI / BixNbOy photocatalysts were prepared by solvothermal method (surfactant sodium citrate was added during preparation), and then graphene oxide was prepared by modified Hummers method. The synthesized BiOI / BixNbOy heterojunction catalysts were supported on graphene oxide nanosheets. Thirdly, using the loaded graphene nanosheets as the precursor, with the help of the directional vacuum freeze-drying technology, under the vacuum degree of 3.3Pa, vacuum drying can be obtained to obtain high-strength supported bismuth heterojunction graphene photocatalysis Material.
以氙灯为模拟太阳光源，构建负载BiOI/BixNbOy异质结的氧化石墨烯连续流反应器。分别以含POPs的模型污水和实际污水为处理对象，在污染物和光催化达到吸附平衡后，每隔一定时间取样测定POPs浓度和COD、TOC的含量，分析POPs的降解率和矿化度。Using a xenon lamp as a simulated solar light source, a graphene oxide continuous flow reactor loaded with BiOI/Bi x NbO y heterojunction was constructed. Model sewage containing POPs and actual sewage were taken as treatment objects. After the pollutants and photocatalysis reached the adsorption equilibrium, samples were taken at regular intervals to measure the POPs concentration and the content of COD and TOC, and the degradation rate and salinity of POPs were analyzed.
本发明公开了一种负载铋系异质结的氧化石墨烯光催化材料的制备与应用。通过在氧化石墨烯上负载BiOI/BixNbOy异质结，再进行真空冷冻干燥，即得到高强度的负载铋系异质结的氧化石墨烯光催化材料。The invention discloses the preparation and application of a graphene oxide photocatalytic material supporting a bismuth series heterojunction. By loading BiOI/Bix NbO y heterojunction on graphene oxide, and then vacuum freeze-drying, a graphene oxide photocatalytic material with high strength supporting bismuth heterojunction is obtained.
实施例2Example 2
首先，采用溶剂热法制备BiOI/BixNbOy光催化剂(制备过程中添加表面活性剂十二烷基苯磺酸钠)，然后，采用改进的Hummers法制备氧化石墨烯。将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上。再次，以负载后的石墨烯纳米片为前驱体，借助定向真空冷冻干燥技术，在真空度为5.0Pa下，进行真空干燥，即可得到高强度的负载铋系异质结的石墨烯光催化材料。First, BiOI / BixNbOy photocatalysts were prepared by solvothermal method (surfactant sodium dodecylbenzenesulfonate was added during preparation), and then graphene oxide was prepared by modified Hummers method. The synthesized BiOI / BixNbOy heterojunction catalysts were supported on graphene oxide nanosheets. Thirdly, using the loaded graphene nanosheets as the precursor, with the help of directional vacuum freeze-drying technology, vacuum drying is carried out under the vacuum degree of 5.0Pa, and high-strength graphene photocatalysis with bismuth-based heterojunction can be obtained. Material.
实施例3Example 3
首先，采用溶剂热法制备BiOI/BixNbOy光催化剂(制备过程中添加表面活性剂溴化十六烷基三甲铵)，然后，采用改进的Hummers法制备氧化石墨烯。将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上。再次，以负载后的石墨烯纳米片为前驱体，借助定向真空冷冻干燥技术，在真空度为6.0Pa下，进行真空干燥，即可得到高强度的负载铋系异质结的石墨烯光催化材料。First, the BiOI / BixNbOy photocatalyst was prepared by a solvothermal method (the surfactant cetyltrimethylammonium bromide was added during the preparation process), and then, graphene oxide was prepared by a modified Hummers method. The synthesized BiOI / BixNbOy heterojunction catalysts were supported on graphene oxide nanosheets. Thirdly, using the loaded graphene nanosheets as the precursor, with the help of directional vacuum freeze-drying technology, under the vacuum degree of 6.0Pa, vacuum drying can obtain high-strength supported bismuth heterojunction graphene photocatalysis Material.
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。Finally, it should be noted that the above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, the The technical solutions described in the foregoing embodiments may be modified, or some technical features thereof may be equivalently replaced. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
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