WO2023246646A1 - 具有疏水中空微纳米结构的光催化材料及制备方法和应用 - Google Patents

具有疏水中空微纳米结构的光催化材料及制备方法和应用 Download PDF

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WO2023246646A1
WO2023246646A1 PCT/CN2023/100718 CN2023100718W WO2023246646A1 WO 2023246646 A1 WO2023246646 A1 WO 2023246646A1 CN 2023100718 W CN2023100718 W CN 2023100718W WO 2023246646 A1 WO2023246646 A1 WO 2023246646A1
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nano structure
photocatalytic material
hollow micro
photocatalytic
hydrophobic hollow
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French (fr)
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张程蕾
谢陈鑫
滕厚开
钱光磊
雷太平
赵慧
任春燕
李旗
荆燕琴
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天津正达科技有限责任公司
中海油天津化工研究设计院有限公司
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
    • B01J35/23—
    • B01J35/39—
    • 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
    • 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
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • 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
    • C02F2101/34—Organic compounds containing oxygen
    • 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
    • C02F2101/36—Organic compounds containing halogen
    • 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
    • C02F2101/40—Organic compounds containing sulfur
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the invention relates to the technical field of sewage treatment, and in particular to a photocatalytic material with a hydrophobic hollow micro-nano structure, its preparation method and application.
  • Photocatalytic wastewater is a new type of wastewater treatment technology.
  • photocatalysis can use solar energy to reduce O 2 to produce superoxide radicals ( ⁇ O 2 ), which indirectly oxidizes pollutants; or it can generate photogenerated holes under photocatalytic conditions and directly mineralize pollutants.
  • ⁇ O 2 superoxide radicals
  • current photocatalysts have problems such as poor light energy absorption ability, low migration and separation rate of photogenerated carriers, and few carriers reaching the surface of the catalyst without recombination, resulting in low light energy utilization.
  • most of the current photocatalysts are nanostructured. Although they can increase the reaction area, they will lead to catalyst agglomeration. How to solve the low light utilization rate and catalyst agglomeration is the current research focus.
  • Graphite phase carbon nitride (gC 3 N 4 ) is one of the most common optical materials. It has the advantages of narrow band gap (2.7eV), high photochemical stability and low cost, and can absorb visible light. However, traditional gC 3 N 4 still suffers from low absorption efficiency of visible light, low surface area and complex carrier fluid. high rate problem.
  • the present invention provides a photocatalytic material with a hydrophobic hollow micro-nano structure, a preparation method and an application.
  • the photocatalytic material has stable structural performance and many active sites. , has good photocatalytic effect.
  • the present invention provides a photocatalytic material with a hydrophobic hollow micro-nano structure, which is achieved using the following technical solutions.
  • a photocatalytic material with a hydrophobic hollow micro-nano structure uses hollow tubular gC 3 N 4 as a carrier and supports tin dioxide quantum dots (SnQDs) and nitrogen-doped graphene quantum dots (NGQDs). (Sn-NG) QDs/gC 3 N 4 photocatalytic material with hydrophobic hollow micro-nano structure.
  • the present invention provides a method for preparing a photocatalytic material with a hydrophobic hollow micro-nano structure, which is achieved by adopting the following technical solutions.
  • a method for preparing the above-mentioned photocatalytic material with a hydrophobic hollow micro-nano structure including the following steps:
  • the mass ratio of NGQDs, SnQDs and gC 3 N 4 is 1: (1-5): (10-20).
  • step S2 the solvent is a mixed solution of isopropyl alcohol and deionized water, and the volume ratio of isopropyl alcohol and deionized water is (1-3):1.
  • the surfactant is sodium dodecylbenzene sulfonate or OP-10, and the concentration of the surfactant is 0.01-0.05 mol/L.
  • the present invention prepares hollow tubular gC 3 N 4 through a high-temperature solid phase method, constructs a micron-scale photocatalyst carrier, and loads SnQDs and NGQDs nanoparticles onto the surface and pores of gC 3 N 4 through a one-step solvothermal method to construct (Sn- NG)QDs/gC 3 N 4 photocatalytic material improves the oxidation ability of the photocatalyst and prevents the agglomeration of NGQDs nanoparticles.
  • the conductivity and light conversion function of the photocatalyst are improved to provide energy for the composite catalyst and prevent the agglomeration of NGQDs nanoparticles.
  • the photocatalytic material obtained by the invention has stable structural performance, many active sites, and good photocatalytic effect.
  • the method is simple and can be produced on a large scale.
  • Figure 1 is an SEM image of the (Sn-NG) QDs/gC 3 N 4 photocatalytic material prepared in Example 1 of the present invention
  • Figure 2 is a diagram showing the test results of (Sn-NG) QDs/gC 3 N 4 prepared in Examples 1-3 and Comparative Examples 1-3 of the present invention for degrading methylene blue wastewater;
  • Figure 3 is an SEM image of the (Sn-NG) QDs/gC 3 N 4 photocatalytic material prepared in Example 2 of the present invention
  • Figure 4 is an SEM image of the (Sn-NG) QDs/gC 3 N 4 photocatalytic material prepared in Example 3 of the present invention
  • Figure 5 is a diagram showing the cycle test results of (Sn-NG) QDs/gC 3 N 4 prepared in Example 1 of the present invention for degrading methylene blue wastewater.
  • a method for preparing a photocatalytic material with a hydrophobic hollow micro-nano structure including the following steps:
  • a method for preparing a photocatalytic material with a hydrophobic hollow micro-nano structure including the following steps:
  • a method for preparing a photocatalytic material with a hydrophobic hollow micro-nano structure including the following steps:
  • the (Sn-NG) QDs/gC 3 N 4 photocatalyst was prepared according to the method of Example 1, except that no surfactant was added when preparing the mixed solution.
  • NGQDs/gC 3 N 4 photocatalyst was prepared according to the method of Example 1, except that SnCl 4 ⁇ 5H 2 O was not added when preparing the mixed solution.
  • SnQDs/gC 3 N 4 photocatalyst was prepared according to the method of Example 1, except that urea and citric acid were not added when preparing the mixed solution.
  • SnQDs/gC 3 N 4 is used as the photocatalyst to photocatalytically degrade dye wastewater (methylene blue is 15 mg/L). Avoid light adsorption for the first 30 minutes. After the adsorption is saturated, turn on the light source (visible light) for photocatalytic degradation of dye wastewater. The test results are shown in Figure 2. The removal rate of COD from dye wastewater is 53.7%, which is 38.9% lower than that in Example 1.

Abstract

一种具有疏水中空微纳米结构的光催化材料及制备方法和应用。制备方法包括高温固相法制备中空管状g-C 3N 4，构造微米级光催化剂载体；采用一步溶剂热法，将SnQDs和NGQDs负载到g-C 3N 4表面和孔道内，得到以中空管状g-C 3N 4为载体，负载SnQDs和NGQDs的疏水中空微纳米结构的光催化材料，该结构能够有效阻止纳米结构的团聚。另外，SnQDs和NGQDs的引入可有效提高光吸收能力和光生载流子的分离率，使(Sn-NG)QDs/g-C 3N 4具有较强的氧化能力，能够有效对污水进行处理。

Description

具有疏水中空微纳米结构的光催化材料及制备方法和应用
相关申请的交叉引用
本申请要求2022年06月22日提交的中国专利申请202210739845.7的权益，该申请的内容通过引用被合并于本文。
技术领域
本发明涉及污水处理技术领域，特别涉及一种具有疏水中空微纳米结构的光催化材料及制备方法和应用。
背景技术
光催化污水是一种新型污水处理技术。在有O2的条件下，光催化可利用太阳能将O2还原产生超氧自由基(·O2)，间接将污染物氧化；或者在光催化条件下产生光生空穴，直接矿化污染物，具有绿色、易操作的优点。但当前光催化剂存在光能吸收能力差、光生载流子发生迁移并分离率低，到达催化剂表面且没有发生复合的载流子少等问题，导致光能利用率低。此外，目前大多光催化剂是纳米结构的，虽然能增加反应面积，但会导致催化剂团聚，如何解决光利用率低和催化剂团聚是当前的研究重点。
石墨相氮化碳(g-C3N4)是最常见的光材料之一，具有带隙窄(2.7eV)、光化学稳定性高和成本低的优点，能够吸收可见光。但传统的g-C3N4仍存在对可见光的吸收效率低、表面积低和载流体的复合 率高的问题。
发明内容
本发明为了解决现有g-C3N4光催化材料存在的上述技术问题，提供一种具有疏水中空微纳米结构的光催化材料及制备方法和应用，该光催化材料结构性能稳定、活性位点多，具有良好的光催化效果。
第一方面，本发明提供了一种具有疏水中空微纳米结构的光催化材料，是采用以下技术方案得以实现的。
一种具有疏水中空微纳米结构的光催化材料，所述光催化材料为以中空管状g-C3N4为载体，负载二氧化锡量子点(SnQDs)和氮掺杂石墨烯量子点(NGQDs)的具有疏水中空微纳米结构的(Sn-NG)QDs/g-C3N4光催化材料。
第二方面，本发明提供了一种具有疏水中空微纳米结构的光催化材料的制备方法，是采用以下技术方案得以实现的。
一种上述具有疏水中空微纳米结构的光催化材料的制备方法，包括以下步骤：
S1.中空管状g-C3N4的制备：将三聚氰胺在惰性气体气氛下，以2-10℃/min的速率升温至400-600℃，恒温反应4-12h，得到中空管状g-C3N4；
S2.(Sn-NG)QDs/g-C3N4的制备：将尿素、柠檬酸、SnCl4·5H2O和表面活性剂搅拌分散在溶剂中，得到混合溶液，调节pH至8-10；然后加入步骤S1的中空管状g-C3N4材料，超声分散20-40min；转移 至不锈钢反应釜中，在200-350℃下，反应6-12h得到固体材料，经洗涤干燥后，得到(Sn-NG)QDs/g-C3N4光催化材料。
进一步的，(Sn-NG)QDs/g-C3N4光催化材料中，NGQDs、SnQDs与g-C3N4的质量比为1：(1-5)：(10-20)。
进一步的，步骤S2中，调节pH的试剂为30％-50％的氨水。
进一步的，步骤S2中，所述溶剂为异丙醇和去离子水的混合溶液，异丙醇和去离子水的体积比为(1-3)：1。
进一步的，步骤S2中，所述表面活性剂为十二烷基苯磺酸钠或OP-10，表面活性剂的浓度为0.01-0.05mol/L。
第三方面，本申请提供了一种具有疏水中空微纳米结构的光催化材料的用途，是采用以下技术方案得以实现的。
一种上述具有疏水中空微纳米结构的光催化材料作为光催化剂在污水处理中的应用。
本申请具有以下有益效果。
本发明通过高温固相法制备中空管状g-C3N4，构造微米级光催化剂载体，并通过一步溶剂热法将SnQDs和NGQDs纳米颗粒负载到g-C3N4表面和孔道内，构建得到(Sn-NG)QDs/g-C3N4光催化材料，提高了光催化剂的氧化能力，阻止了NGQDs纳米颗粒的团聚。通过负载NGQDs提高光催化剂的导电性和光转换功能为复合催化剂提供能量，并阻止NGQDs纳米颗粒团聚。通过活性剂的作用和构建微纳米结构得到疏水表面，以提高活性自由基的扩散能力。本发明所得光催化材料结构性能稳定、活性位点多，具有良好的光催化效果，制备 方法简单，可规模生产。
附图说明
图1是本发明实施例1制备的(Sn-NG)QDs/g-C3N4光催化材料的SEM图；
图2是本发明实施例1-3和对比例1-3制备的(Sn-NG)QDs/g-C3N4用于降解亚甲基蓝废水的试验结果图；
图3是本发明实施例2制备的(Sn-NG)QDs/g-C3N4光催化材料的SEM图；
图4是本发明实施例3制备的(Sn-NG)QDs/g-C3N4光催化材料的SEM图；
图5是本发明实施例1制备的(Sn-NG)QDs/g-C3N4用于降解亚甲基蓝废水的循环试验结果图。
具体实施方式
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开。
实施例1
一种具有疏水中空微纳米结构的光催化材料的制备方法，包括以下步骤：
S1.将三聚氰胺在惰性气体气氛下，以8℃/min的速率升温至500℃，恒温反应12h，得到中空管状g-C3N4材料；
S2.以异丙醇和去离子水体积比1：1的溶液作为反应溶剂；将0.25g尿素、0.27g柠檬酸、0.87g SnCl4·5H2O和0.12g十二烷基苯磺酸钠搅拌溶解在反应溶剂中，得到混合溶液，用30％氨水调节溶液pH至8；然后加入15mg中空g-C3N4材料，超声分散30min；转移至不锈钢反应釜中，在200℃下，反应10h得到固体材料；经多次洗涤干燥并后得到(Sn-NG)QDs/g-C3N4光催化材料。其SEM图如图1所示。
以(Sn-NG)QDs/g-C3N4作为光催化剂光催化降解染料废水(亚甲基蓝为15mg/L)。前30min避光吸附，待吸附饱和后打开光源(可见光)进行光催化降解处理染料废水。试验结果如图2所示，光催化处理5.5h时，对亚甲基蓝的去除率为92.6％。
实施例2
一种具有疏水中空微纳米结构的光催化材料的制备方法，包括以下步骤：
S1.将三聚氰胺在惰性气体气氛下，以8℃/min的速率升温至600℃，恒温反应6h，得到中空管状g-C3N4材料；
S2.以异丙醇和去离子水体积比3：1的溶液作为反应溶剂；将0.25g尿素、0.27g柠檬酸、0.58g SnCl4·5H2O和0.15g十二烷基苯磺酸钠分散在反应溶剂中，得到混合溶液，用50％氨水调节溶液pH至10；然后加入中空20mg g-C3N4材料，超声分散30min；转移至不锈钢反应釜中，在350℃下，反应10h得到固体材料；经多次洗涤干燥并后得到(Sn-NG)QDs/g-C3N4光催化材料。其SEM图如图3所示。
以(Sn-NG)QDs/g-C3N4作为光催化剂光催化降解染料废水(亚甲基蓝为15mg/L)。前30min避光吸附，待吸附饱和后打开光源(可见光)进行光催化降解处理染料废水。试验结果如图2所示，光催化处理5.5h时，对染料废水COD的去除率为85.3％。
实施例3
一种具有疏水中空微纳米结构的光催化材料的制备方法，包括以下步骤：
S1.将三聚氰胺在惰性气体气氛下，以6℃/min的速率升温至500℃，恒温反应12h，得到中空管状g-C3N4材料；
S2.以异丙醇和去离子水体积比3：1的溶液作为反应溶剂。将0.25g尿素、0.27g柠檬酸、0.87g SnCl4·5H2O和20μL OP-10搅拌分散在反应溶剂中，得到混合溶液，用25％氨水调节溶液pH至9；然后加入中空18mg中空g-C3N4材料，超声分散30min；转移至不锈钢反应釜中，在300℃下，反应10h得到固体材料；经多次洗涤干燥并后得到(Sn-NG)QDs/g-C3N4光催化材料。其SEM图如图4所示。
以(Sn-NG)QDs/g-C3N4作为光催化剂光催化降解染料废水(亚甲基蓝为15mg/L)。前30min避光吸附，待吸附饱和后打开光源(可见光)进行光催化降解处理染料废水。试验结果如图2所示，光催化处理5.5h时，对染料废水COD的去除率为82.0％。
对比例1
根据实施例1的方法制备(Sn-NG)QDs/g-C3N4光催化剂，不同之处在于，配置混合溶液时中不添加表面活性剂。
以(Sn-NG)QDs/g-C3N4作为光催化剂光催化降解染料废水(亚甲基蓝为15mg/L)。前30min避光吸附，待吸附饱和后打开光源(可见光)进行光催化降解处理染料废水。试验结果如图2所示，对染料废水COD的去除率为62.6％，比实施例1低32.0％。
对比例2
根据实施例1的方法制备NGQDs/g-C3N4光催化剂，不同之处在于，配制混合溶液时中不添加SnCl4·5H2O。
以NGQDs/g-C3N4作为光催化剂光催化降解染料废水(亚甲基蓝为15mg/L)。前30min避光吸附，待吸附饱和后打开光源(可见光)进行光催化降解处理染料废水。试验结果如图2所示，对染料废水COD的去除率为46.8％，比实施例1低45.8％。
对比例3
根据实施例1的方法制备SnQDs/g-C3N4光催化剂，不同之处在于，配制混合溶液时中不添加尿素和柠檬酸。
以SnQDs/g-C3N4作为光催化剂光催化降解染料废水(亚甲基蓝为15mg/L)。前30min避光吸附，待吸附饱和后打开光源(可见光)进行光催化降解处理染料废水。试验结果如图2所示，对染料废水COD的去除率为53.7％，比实施例1低38.9％。
性能检测
根据实施例1的方法制备(Sn-NG)QDs/g-C3N4光催化剂，重复进行10次实验，考察光催化剂的稳定性。如图5所示，第10次试验较第1次仅降低11.8％，说明该催化剂较稳定。
以上详细描述了本发明的优选实施方式，但是，本发明并不限于此。在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，包括各个技术特征以任何其它的合适方式进行组合，这些简单变型和组合同样应当视为本发明所公开的内容，均属于本发明的保护范围。

Claims (7)

  1. 一种具有疏水中空微纳米结构的光催化材料，其特征在于：所述光催化材料为以中空管状g-C3N4为载体，负载SnQDs和NGQDs的具有疏水中空微纳米结构的(Sn-NG)QDs/g-C3N4光催化材料。
  2. 一种权利要求1所述具有疏水中空微纳米结构的光催化材料的制备方法，其特征在于：包括以下步骤：
    S1.中空管状g-C3N4的制备：将三聚氰胺在惰性气体气氛下，以2-10℃/min的速率升温至400-600℃，恒温反应4-12h，得到中空管状g-C3N4；
    S2.(Sn-NG)QDs/g-C3N4的制备：将尿素、柠檬酸、SnCl4·5H2O和表面活性剂搅拌分散在溶剂中，得到混合溶液，调节pH至8-10；然后加入步骤S1的中空管状g-C3N4材料，超声分散20-40min；在200-350℃下，反应6-12h得到固体材料，经洗涤干燥后，得到(Sn-NG)QDs/g-C3N4光催化材料。
  3. 根据权利要求2所述的一种具有疏水中空微纳米结构的光催化材料的制备方法，其特征在于：(Sn-NG)QDs/g-C3N4光催化材料中，NGQDs、SnQDs与g-C3N4的质量比为1：(1-5)：(10-20)。
  4. 根据权利要求2所述的一种具有疏水中空微纳米结构的光催化材料的制备方法，其特征在于：步骤S2中，调节pH的试剂为30％-50％ 的氨水。
  5. 根据权利要求2所述的一种具有疏水中空微纳米结构的光催化材料的制备方法，其特征在于：步骤S2中，所述溶剂为异丙醇和去离子水的混合溶液，异丙醇和去离子水的体积比为(1-3)：1。
  6. 根据权利要求2所述的一种具有疏水中空微纳米结构的光催化材料的制备方法，其特征在于：步骤S2中，所述表面活性剂为十二烷基苯磺酸钠或OP-10，表面活性剂的浓度为0.01-0.05mol/L。
  7. 一种权利要求1所述具有疏水中空微纳米结构的光催化材料作为光催化剂在污水处理中的应用。
PCT/CN2023/100718 2022-06-22 2023-06-16 具有疏水中空微纳米结构的光催化材料及制备方法和应用 WO2023246646A1 (zh)

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