CN105964250B - It is a kind of with visible light-responded Ag10Si4O13Photochemical catalyst and its preparation method and application - Google Patents
It is a kind of with visible light-responded Ag10Si4O13Photochemical catalyst and its preparation method and application Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000003054 catalyst Substances 0.000 title abstract description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 15
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 6
- 239000011941 photocatalyst Substances 0.000 claims description 28
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- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
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- 238000002156 mixing Methods 0.000 abstract 1
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- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 9
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
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- 238000012360 testing method Methods 0.000 description 6
- 230000004298 light response Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 150000004760 silicates Chemical class 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
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- 238000003746 solid phase reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- QUZPNFFHZPRKJD-UHFFFAOYSA-N germane Chemical compound [GeH4] QUZPNFFHZPRKJD-UHFFFAOYSA-N 0.000 description 1
- 229910052986 germanium hydride Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
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- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种具有可见光响应的Ag10Si4O13光催化剂及其制备方法和应用，属于半导体光催化剂技术领域。The invention relates to an Ag 10 Si 4 O 13 photocatalyst with visible light response, a preparation method and application thereof, and belongs to the technical field of semiconductor photocatalysts.
背景技术Background technique
利用半导体光催化剂将难以收集的低密度的太阳能光能转化成高密度易利用的电能和化学能已成为近年国际上最活跃的研究领域之一。尤其是在光催化分解水以及利用光氧化降解污染物治理环境方面展现出的独特的优势，已引起世界各国科学家的广泛关注，因此对半导体光催化剂进行广泛的理论以及实验研究将具有非常重要的战略和现实意义。The use of semiconductor photocatalysts to convert the difficult-to-collect low-density solar energy into high-density and easy-to-use electrical and chemical energy has become one of the most active research fields in the world in recent years. Especially in photocatalytic water splitting and the use of photooxidative degradation of pollutants to control the environment, it has attracted widespread attention from scientists all over the world. Therefore, it will be very important to conduct extensive theoretical and experimental research on semiconductor photocatalysts. Strategic and practical significance.
目前制约光催化技术实际应用的所有问题中，最重要的是如何提高光催化剂对光能的利用效率。在太阳光谱中，紫外光约占所有能量3～4％，而可见光却占比却超过40％，因此，研究开发可见光响应的光催化剂是提高太阳能利用效率的一项研究重点，具有很重要的理论和实际意义。Among all the problems currently restricting the practical application of photocatalytic technology, the most important is how to improve the utilization efficiency of light energy by photocatalysts. In the solar spectrum, ultraviolet light accounts for about 3-4% of all energy, while visible light accounts for more than 40%. Therefore, the research and development of photocatalysts that respond to visible light is a research focus to improve solar energy utilization efficiency and is of great importance. Theoretical and practical implications.
硅酸盐化合物常作为催化材料被广泛应用在工业催化中，但目前关于硅酸盐化合物作为光催化剂材料的报道较少。尤其是银基硅酸盐类化合物，由于其合成反应条件严苛，通常需要极高的氧压条件，这极大制约了银基硅酸盐类化合物的***研究。因此，从硅酸盐化合物中发现并合成具有高效光催化活性的银基硅酸盐材料，对于扩大光催化剂的实际应用具有十分重要的意义。Silicate compounds are often used as catalytic materials in industrial catalysis, but there are few reports on silicate compounds as photocatalyst materials. Especially silver-based silicate compounds, due to the harsh conditions of their synthesis reaction, usually require extremely high oxygen pressure conditions, which greatly restricts the systematic research of silver-based silicate compounds. Therefore, the discovery and synthesis of silver-based silicate materials with high photocatalytic activity from silicate compounds is of great significance for expanding the practical application of photocatalysts.
发明内容Contents of the invention
针对上述现有技术的，本发明的目的提供一种具有可见光响应的Ag10Si4O13光催化剂及其制备方法。In view of the aforementioned prior art, the object of the present invention is to provide an Ag 10 Si 4 O 13 photocatalyst with visible light response and a preparation method thereof.
本发明的另一目的是提供该Ag10Si4O13光催化剂在降解有机污染物以及分解水产氧中的应用。Another object of the present invention is to provide the application of the Ag 10 Si 4 O 13 photocatalyst in degrading organic pollutants and decomposing water to generate oxygen.
为实现上述目的，本发明采用如下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
本发明的第一方面，提供一种具有可见光响应的Ag10Si4O13光催化剂的制备方法，步骤如下：The first aspect of the present invention provides a preparation method of Ag 10 Si 4 O 13 photocatalyst with visible light response, the steps are as follows:
(1)将偏硅酸钠和硝酸银按摩尔比1：(2-4)混合，研磨至均匀；(1) Mix sodium metasilicate and silver nitrate in a molar ratio of 1: (2-4), and grind until uniform;
(2)将研磨得到的混合物加入到去离子水中，搅拌，分离沉淀，洗涤，干燥，得前驱体；(2) adding the mixture obtained by grinding into deionized water, stirring, separating the precipitate, washing, and drying to obtain the precursor;
(3)将前驱体在常压下加热至300-500℃，并保持3-5小时，即得Ag10Si4O13光催化剂。(3) Heating the precursor to 300-500° C. under normal pressure and maintaining it for 3-5 hours to obtain the Ag 10 Si 4 O 13 photocatalyst.
优选的，步骤(1)中，偏硅酸纳和硝酸银的摩尔比为1：3。偏硅酸纳和硝酸银的加入量会影响制备的Ag10Si4O13光催化剂的结构组成，本发明对偏硅酸纳和硝酸银加入的量进行了考察，结果发现，偏硅酸纳和硝酸银按摩尔比1：(2-4)加入为宜，能够最大程度的生成目标产物；当偏硅酸纳和硝酸银按摩尔比1：3加入时，Ag10Si4O13的产率最高。Preferably, in step (1), the molar ratio of sodium metasilicate to silver nitrate is 1:3. The addition amount of sodium metasilicate and silver nitrate can influence the structural composition of the Ag 10 Si 4 O 13 photocatalyst of preparation, the present invention has investigated the amount that sodium metasilicate and silver nitrate add, the result finds that sodium metasilicate It is advisable to add silver nitrate and silver nitrate at a molar ratio of 1: (2-4) to maximize the formation of the target product; when sodium metasilicate and silver nitrate are added at a molar ratio of 1:3, the production of Ag 10 Si 4 O 13 highest rate.
优选的，步骤(1)中，研磨时间为15-25min，进一步的，优选为20min。通过研磨可以改善本发明的固相反应中反应物的接触情况，以增加有利于反应的缺陷浓度，改善了反应的热力学和动力学条件，使固相反应能够顺利进行。本发明对研磨时间进行了优化，结果发现，若研磨时间过短，则反应物的接触不充分；若研磨时间过长，则一方面延长了合成时间，增加了生产成本，另一方面可能还会影响反应产物的晶体构型。经多次对比试验发现，研磨时间以15-25min为宜。Preferably, in step (1), the grinding time is 15-25 minutes, further, preferably 20 minutes. Grinding can improve the contact condition of the reactants in the solid phase reaction of the present invention, so as to increase the concentration of defects that are beneficial to the reaction, improve the thermodynamic and kinetic conditions of the reaction, and enable the solid phase reaction to proceed smoothly. The present invention optimizes the grinding time. As a result, it is found that if the grinding time is too short, the contact of the reactants will not be sufficient; Can affect the crystal configuration of the reaction product. After many comparison tests, it is found that the grinding time is 15-25min.
优选的，步骤(2)中，研磨得到的混合物与去离子水加入量的比为(0.5-1.5)mmol：10ml。Preferably, in step (2), the ratio of the mixture obtained by grinding to the added amount of deionized water is (0.5-1.5) mmol: 10 ml.
优选的，步骤(2)中，洗涤采用的是去离子水和无水乙醇清洗。Preferably, in step (2), deionized water and absolute ethanol are used for washing.
优选的，步骤(3)中，将前驱体在常压下加热至400℃。对前驱体进行热处理可以改变产物的晶相结构，而产物的晶相结构与其光催化活性密切相关，本发明对热处理温度进行了考察，结果发现，热处理的温度高于500℃或低于300℃都无法生成本发明的结晶Ag10Si4O13。Preferably, in step (3), the precursor is heated to 400° C. under normal pressure. Heat treatment of the precursor can change the crystal phase structure of the product, and the crystal phase structure of the product is closely related to its photocatalytic activity. The present invention investigated the heat treatment temperature and found that the heat treatment temperature is higher than 500°C or lower than 300°C None of them can produce the crystalline Ag 10 Si 4 O 13 of the present invention.
优选的，步骤(3)中，以5℃/min的速率进行升温至加热温度。Preferably, in step (3), the temperature is raised to the heating temperature at a rate of 5° C./min.
上述方法制备的Ag10Si4O13光催化剂，由无规则的纳米颗粒组成，在过渡金属离子(Ag+) 的存在下，硅酸盐中的SiO4四面体容易畸变而产生极化，通过控制这些极性四面体的排列会在材料内部构建一个内部极化电场；另外，复杂的过渡金属的配位环境为光生电子在相连多面体之间的转移提供了可能性。因此，上述方法制备的Ag10Si4O13具有高效光催化活性。The Ag 10 Si 4 O 13 photocatalyst prepared by the above method is composed of random nanoparticles. In the presence of transition metal ions (Ag + ), the SiO 4 tetrahedron in the silicate is easily distorted and polarized. Controlling the arrangement of these polar tetrahedrons will build an internal polarizing electric field inside the material; in addition, the complex coordination environment of transition metals provides the possibility for the transfer of photogenerated electrons between connected polyhedra. Therefore, the Ag 10 Si 4 O 13 prepared by the above method has high photocatalytic activity.
本发明的第二方面，提供上述Ag10Si4O13光催化剂在分解水产氧和降解有机污染物中的应用。The second aspect of the present invention provides the application of the above-mentioned Ag 10 Si 4 O 13 photocatalyst in decomposing water to generate oxygen and degrade organic pollutants.
本发明的有益效果：Beneficial effects of the present invention:
(1)本发明制备的Ag10Si4O13光催化剂具有可见光响应，经实验研究发现，Ag10Si4O13显示出较好的光催化活性，在可见光照下在2.5小时分解水产氧110umol，50分钟内降解98％的亚甲基蓝有机染料。在全光(300nm-1100nm)下其光氧化降解亚甲基蓝效率要比商品TiO2 (P25)要更加优秀。因此，本发明制备的Ag10Si4O13光催化剂同时具有分解水产氧和降解空气、废水、地表水或饮用水中有机污染物的双重效果，这是现有报道的银基硅酸盐化合物所不具备的。(1) The Ag 10 Si 4 O 13 photocatalyst prepared by the present invention has a visible light response. It is found through experimental research that Ag 10 Si 4 O 13 shows better photocatalytic activity, and it decomposes water to produce 110umol of oxygen in 2.5 hours under visible light , Degrade 98% of methylene blue organic dye within 50 minutes. Under full light (300nm-1100nm), its photooxidative degradation efficiency of methylene blue is better than commercial TiO 2 (P25). Therefore, the Ag 10 Si 4 O 13 photocatalyst prepared by the present invention has dual effects of decomposing water to generate oxygen and degrading organic pollutants in air, waste water, surface water or drinking water. This is the silver-based silicate compound reported do not have.
(2)本发明Ag10Si4O13光催化剂采用固相反应合成，首先形成前驱体，然后经常温、高温固相反应结晶，形成热力学稳定的Ag10Si4O13晶体。制备合成方法条件简单，无需极高的氧压条件，无需添加有机溶剂，反应条件温和，更适合大规模生产和实际应用，具有较高的商业化应用前景。(2) The Ag 10 Si 4 O 13 photocatalyst of the present invention is synthesized by solid-state reaction. First, a precursor is formed, and then crystallized by solid-state reaction at normal or high temperature to form a thermodynamically stable Ag 10 Si 4 O 13 crystal. The preparation and synthesis method has simple conditions, does not require extremely high oxygen pressure conditions, does not need to add organic solvents, has mild reaction conditions, is more suitable for large-scale production and practical application, and has high commercial application prospects.
附图说明Description of drawings
图1为本发明前驱体，结晶Ag10Si4O13标准卡片的X射线图；Fig. 1 is the precursor of the present invention, the X-ray diagram of crystal Ag 10 Si 4 O 13 standard card;
图2为本发明产物的光吸收图谱；Fig. 2 is the optical absorption spectrum of product of the present invention;
图3为本发明产物的SEM图；Fig. 3 is the SEM figure of product of the present invention;
图4为本发明实施例产物形成的光催化剂与氮掺杂P25用于可见光光催化降解有机染料亚甲基蓝对比；Fig. 4 is the photocatalyst that the product of the embodiment of the present invention forms and nitrogen-doped P25 is used for visible light photocatalytic degradation organic dye methylene blue comparison;
图5为光催化剂可见光光催化降解有机染料亚甲基蓝前后溶液中总碳含量(TC)，有机碳含量(TOC)和无机碳量(IC)变化图；Fig. 5 is the total carbon content (TC) in the solution before and after photocatalyst visible light photocatalytic degradation organic dye methylene blue, organic carbon content (TOC) and inorganic carbon content (IC) change figure;
图6为本发明实施例产物形成的光催化剂用于光催化分解水产氧产量图。Fig. 6 is a photocatalyst photocatalytic water splitting oxygen production diagram formed by the product of the embodiment of the present invention.
具体实施方式Detailed ways
结合实施例对本发明作进一步的说明，应该说明的是，下述实施例仅是为了解释本发明，并不对其内容进行限定。The present invention will be further described in conjunction with the examples. It should be noted that the following examples are only for explaining the present invention, and do not limit its content.
实施例1：Example 1:
称取3mmol偏硅酸钠和9mmol硝酸银放入玛瑙研钵中，研磨20分钟直至颜色均匀。然后将研磨均匀的混合物全部倒入100mL烧杯中，加入100mL去离子水搅拌十分钟。最后将沉淀分离并用去离子水和无水乙醇清洗，最后在在室温下干燥，即可得到前驱体。Weigh 3 mmol of sodium metasilicate and 9 mmol of silver nitrate into an agate mortar and grind for 20 minutes until the color is uniform. Then pour the uniformly ground mixture into a 100mL beaker, add 100mL deionized water and stir for ten minutes. Finally, the precipitate is separated and washed with deionized water and absolute ethanol, and finally dried at room temperature to obtain the precursor.
将所得的前驱体粉末置于坩埚内，然后以每分钟5摄氏度的速率加热到400摄氏度并保持4小时，进行二次固相热处理，即得到结晶性良好的Ag10Si4O13。The obtained precursor powder was placed in a crucible, and then heated to 400 degrees Celsius at a rate of 5 degrees Celsius per minute and kept for 4 hours for a second solid phase heat treatment to obtain Ag 10 Si 4 O 13 with good crystallinity.
对制备的前驱体和结晶Ag10Si4O13进行结构表征和性能测试，其中，前驱体和结晶Ag10Si4O13的X射线衍射图如图1所示；结晶Ag10Si4O13的光吸收图谱如图2所示；结晶Ag10Si4O13的SEM图如图3所示。Structural characterization and performance tests were carried out on the prepared precursor and crystalline Ag 10 Si 4 O 13 , where the X-ray diffraction patterns of the precursor and crystalline Ag 10 Si 4 O 13 are shown in Figure 1; the crystalline Ag 10 Si 4 O 13 The optical absorption spectrum of the crystal is shown in Figure 2; the SEM image of crystal Ag 10 Si 4 O 13 is shown in Figure 3.
由图1可以看出，未经过热处理的前驱体基本为非晶相，经过4个小时热处理后，产物表现出较好的结晶性，成分为Ag10Si4O13，并未出现明显的杂峰。由图2可以看出，结晶Ag10Si4O13在可见光领域有很强的吸收。由图3可以看出，本实施例得到的Ag10Si4O13产物为2微米左右的颗粒，并没有特殊的形貌。It can be seen from Figure 1 that the precursor without heat treatment is basically an amorphous phase. After 4 hours of heat treatment, the product shows good crystallinity, the composition is Ag 10 Si 4 O 13 , and no obvious impurities appear. peak. It can be seen from Figure 2 that the crystalline Ag 10 Si 4 O 13 has strong absorption in the visible light field. It can be seen from FIG. 3 that the Ag 10 Si 4 O 13 product obtained in this example is a particle of about 2 microns, and has no special shape.
实施例2：Example 2:
称取3mmol偏硅酸钠和6mmol硝酸银放入玛瑙研钵中，研磨20分钟直至颜色均匀。然后将研磨均匀的混合物全部倒入100mL烧杯中，加入100mL去离子水搅拌十分钟。最后将沉淀分离并用去离子水和无水乙醇清洗，最后在在室温下干燥，即可得到前驱体。Weigh 3 mmol of sodium metasilicate and 6 mmol of silver nitrate into an agate mortar and grind for 20 minutes until the color is uniform. Then pour the uniformly ground mixture into a 100mL beaker, add 100mL deionized water and stir for ten minutes. Finally, the precipitate is separated and washed with deionized water and absolute ethanol, and finally dried at room temperature to obtain the precursor.
将所得的前驱体粉末置于坩埚内，然后以每分钟5摄氏度的速率加热到300摄氏度并保持3小时，进行二次固相热处理，即得到结晶性良好的Ag10Si4O13。The obtained precursor powder was placed in a crucible, and then heated to 300 degrees Celsius at a rate of 5 degrees Celsius per minute and kept for 3 hours for a second solid phase heat treatment to obtain Ag 10 Si 4 O 13 with good crystallinity.
实施例3：Example 3:
称取3mmol偏硅酸钠和12mmol硝酸银放入玛瑙研钵中，研磨20分钟直至颜色均匀。然后将研磨均匀的混合物全部倒入100mL烧杯中，加入100mL去离子水搅拌十分钟。最后将沉淀分离并用去离子水和无水乙醇清洗，最后在在室温下干燥，即可得到前驱体。Weigh 3mmol sodium metasilicate and 12mmol silver nitrate into an agate mortar and grind for 20 minutes until the color is uniform. Then pour the uniformly ground mixture into a 100mL beaker, add 100mL deionized water and stir for ten minutes. Finally, the precipitate is separated and washed with deionized water and absolute ethanol, and finally dried at room temperature to obtain the precursor.
将所得的前驱体粉末置于坩埚内，然后以每分钟5摄氏度的速率加热到500摄氏度并保持5小时，进行二次固相热处理，即得到结晶性良好的Ag10Si4O13。The obtained precursor powder was placed in a crucible, and then heated to 500 degrees Celsius at a rate of 5 degrees Celsius per minute and kept for 5 hours for a second solid-phase heat treatment to obtain Ag 10 Si 4 O 13 with good crystallinity.
性能测试：Performance Testing:
1.光催化降解有机染料测试1. Photocatalytic degradation of organic dyes
在普通的100mL玻璃烧杯中常温常压下进行。光源选用装有滤光片的300W氙灯，使得光源波长大于420nm。用亚甲基蓝来评价样品的光催化活性。称取50mg氢化锗样品分散在50 ml亚甲基蓝B溶液中(20mg/L)。光催化反应测试前，避光磁力搅拌30min使亚甲基蓝在催化剂表面达到吸附平衡，通光后每隔10min取样3ml，离心分离，取上清液用紫外可见分光光度计测量吸光度。Carry out in ordinary 100mL glass beaker under normal temperature and pressure. The light source is a 300W xenon lamp equipped with a filter, so that the wavelength of the light source is greater than 420nm. The photocatalytic activity of the samples was evaluated with methylene blue. Weigh 50 mg of germanium hydride sample and disperse in 50 ml of methylene blue B solution (20 mg/L). Before the photocatalytic reaction test, magnetically stir for 30 minutes in the dark to make the methylene blue reach adsorption equilibrium on the catalyst surface. After passing the light, take 3ml samples every 10 minutes, centrifuge and take the supernatant to measure the absorbance with a UV-Vis spectrophotometer.
实施例1制备的结晶Ag10Si4O13的光催化降解有机染料测试结果如图4-5所示，由图可知，在可见光下光催化剂经光催化降解有机染料亚甲基蓝测试，光催化剂可在50分钟将亚甲基蓝降解98％，其光催化活性要高于氮掺杂P25。The photocatalytic degradation organic dye test results of the crystalline Ag 10 Si 4 O 13 prepared in Example 1 are shown in Figure 4-5. It can be seen from the figure that the photocatalyst can be tested by photocatalytic degradation of the organic dye methylene blue under visible light. 98% of methylene blue was degraded in 50 minutes, and its photocatalytic activity was higher than that of nitrogen-doped P25.
2.光催化分解水产氧测试2. Photocatalytic water splitting oxygen production test
在连接有循环冷却水(5℃)封闭的玻璃容器***进行并进行，真空条件为-97KPa。在顶部照射的光源选用装有滤光片的300W氙灯，使得光源波长大于420nm。通光后每隔0.5h进行测试，由气相色谱仪测得的峰面积值转化为氧气的产量。It is carried out in a closed glass container system connected with circulating cooling water (5°C), and the vacuum condition is -97KPa. The light source illuminated on the top is a 300W xenon lamp equipped with a filter, so that the wavelength of the light source is greater than 420nm. Test every 0.5h after passing through the light, and convert the peak area value measured by the gas chromatograph into the output of oxygen.
实施例1制备的结晶Ag10Si4O13的光催化分解水产氧的结果如图6所示，由图6可以看出，在可见光下光催化剂可在2.5h内分解水产生约110umol氧气。The results of photocatalytic water splitting and oxygen generation of crystalline Ag 10 Si 4 O 13 prepared in Example 1 are shown in Fig. 6. It can be seen from Fig. 6 that the photocatalyst can split water and generate about 110umol oxygen within 2.5 hours under visible light.
以上的检测和分析综合的证明了本发明得到的产物是具有可见光响应用于光催化产氢的光催化剂。并在光降解有机污染物及分解水产氧方面具有较好的应用价值。The above detection and analysis comprehensively prove that the product obtained in the present invention is a photocatalyst with visible light response for photocatalytic hydrogen production. And it has good application value in photodegradation of organic pollutants and decomposition of water to produce oxygen.
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