CN109382102B - 用于室内甲醛和苯完全快速降解的可见光催化材料的制备方法 - Google Patents
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Abstract
本发明属于环境工程领域的实用技术，提供一种光催化材料（Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69）在可见光下可将室内甲醛和苯完全快速降解，达到净化空气的目的。本发明采用乙醇、五氧化二钽、五氧化二铌、硝酸银、聚乙烯吡咯烷酮通过简单的乙醇回流法、固热法以及原位还原制备出在可见光下高效氧化室内甲醛和苯的三相光催化剂。只需将少量的催化剂平铺于固体表面上，在可见光照射下就可以将甲醛和苯氧化为二氧化碳和水，无二次污染，而且催化剂可重复使用稳定性极高，选择性极好。所制得的催化剂无毒无害便于回收、原材料成本低。符合环境净化的要求，有望应用于室内空气净化如空气净化器、内墙涂料等领域。
Description
技术领域
本发明涉及一种三相催化剂的合成方法及其在可见光下对室内甲醛和苯净化方面的应用，工程上涉及室内污染处理技术领域，技术上涉及材料合成及光催化领域。
背景技术
室内甲醛和苯主要来自于木质家具、木质地板、以及各类板材，粘合剂，涂料等，随着时间的推移逐渐挥发排放到比较封闭的室内，长时间以来由于长时间在室内活动对人类的健康造成严重的影响，引起人类免疫力低下、过敏、哮喘等呼吸道疾病甚至导致癌症的发生。对于室内环境的净化人们提出了各种方法来实现，有吸附，生物降解，热降解，以及光催化降解等技术，其中光催化降解技术被认为是一种高效绿色环保无次生污染的技术而被广泛研究。
钽酸银（Ag2Ta4O11）是一种银基材料，晶体具有独特片状结构，可以有效的促进电子与空穴的分离与转移，而且高度重叠的杂化轨道有助于提高催化剂的稳定性。作为银基材料的一种对光比较敏感，在光的长时间照射下银纳米颗粒可以很容易的还原出来并均匀的分布于催化剂表面。而银纳米颗粒可以作为一种电子接受体，将催化剂上的电子转移到银纳米颗粒，提高电子与空穴的分离效率，同时作为活性位点提高催化剂的催化活性。然而不幸的是，钽酸银的禁带宽度较宽，只有紫外光才可以激发材料产生光生电子和空穴，而紫外光仅占太阳光的5%左右，限制了其在可见光下的应用。
为了拓宽钽酸银的光响应到可见光区域，在Ag2Ta4O11的基础上合成了新型催化剂Ag8(Ta0.5Nb0.5)26O69由于其较窄的禁带宽度，可以在可见光的激发下产生光生电子空穴对，对室内甲醛和苯起到催化降解的功能。但是由于其光生电子与空穴的复合率较高，使得该材料的催化性能较低，成为其降解室内甲醛与苯的最大瓶颈。
为了实现在可见光下被激发产生光生载流子，降低光生电子与空穴的复合率。将Ag2Ta4O11与Ag8(Ta0.5Nb0.5)26O69通过热固法复合在一起形成异质结，使得光生电子与空穴在空间上分离，大大的降低载流子的复合效率，与此同时银基材料在光的照射下银纳米颗粒被原位还原出来均匀分布于催化剂表面，作为电子阱将催化剂上的大量电子转移到银纳米颗粒上，提高电子与空穴的分离效率，与此同时银纳米粒子的等离子体共振效应也产生电子，进一步提高催化效果。
本发明制备了一种三相光催化材料用于室内甲醛和苯的净化，制备方便，操作简单，用量少，稳定性好，可回收重复利用。可以在可见光下激发产生光生载流子，并原位还原出银纳米粒子大大提高催化剂的催化活性与稳定性。将甲醛与苯完全降解为水和二氧化碳，无二次污染，达到净化室内污染物的目的。可推广至室内空气净化领域，如空气净化器、内墙涂料等。
发明内容
对于室内甲醛与苯的去除，目前使用较广的材料为，活性炭、硅藻泥等吸附材料以及二氧化钛等只对紫外光响应的光催化材料。吸附材料虽然便宜来源广，可是存在一个弊端，容易达到饱和状态而不能继续吸附，当污染物浓度降低到一定程度，还会脱附释放出污染物从而形成二次污染。而二氧化钛等对可见光没有响应的催化剂，在使用过程中通常要额外配备紫外光源来达到净化空气的目的，无形中增加了使用成本限制了其推广使用。本发明基于开发高效稳定且对可见光响应用于室内甲醛与苯的降解的材料。打破了目前催化剂的使用瓶颈，开发了可以高效利用可见光，将甲醛与苯彻底氧化为二氧化碳和水，而且具有较高稳定性可以循环使用的催化剂，达到一次投入终身使用大大的节约成本的目的。本发明具有较高的催化效果，原料成本低、制作简单，使用条件简单，可以推广至室内空气净化如空气净化器、内墙涂料等领域。
本发明的具体技术方案如下：
钽酸银（Ag2Ta4O11）的制备：将一定量的聚乙烯吡咯烷酮加入100毫升的乙醇溶液中，搅拌15分钟后加入等比五氧化二钽和硝酸银，继续搅拌30分钟后，加热至120oC，然后将材料干燥后继续加热4小时得到白色材料钽酸银；
Ag2Ta4O11/Ag8(Ta0.5Nb0.5)26O69的制备：将一定量的聚乙烯吡咯烷酮加入100毫升的乙醇溶液中，搅拌15分钟后加入物质的量比为1：1：0.5的五氧化二钽、硝酸银和五氧化二铌，继续搅拌30分钟后，加热至120oC并保持2小时，然后将材料干燥后继续加热4小时得到白色二元固体材料；
三相催化剂Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69的制备：将制备的二元固体材料平铺于表面上，用300W紫外光照射30分钟，得到三元催化剂Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69备用；
附图说明
图1为三元光催化材料（Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69）的XRD 图。
图2为三元光催化材料（Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69）的SEM图。
图3为三元光催化材料（Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69）的EDS图。
图4为三元光催化材料（Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69）的TEM图。
图5为三元光催化材料（Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69）的降解气体中的甲醛和苯的曲线图。
具体实施方式
以下结合实施例对本发明进一步说明。
实施例：将合成的三相催化剂15毫克通过乙醇均匀分散于玻璃表面，干燥后放于体积为2升的反应器中，配有空气循环装置，光源为300W氙灯带有可见光滤光片（波长大于420纳米）。反应器中甲醛与苯通过空气鼓泡法带入反应装置，通过调节气流来控制浓度，用气体红外检测器和气相色谱来检测反应气体中物质的变化。降解情况见图5。
以上所述，仅为本发明较好的具体实施方案，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。
Claims (5)
1.用于室内甲醛和苯完全快速降解的可见光催化材料Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69的制备方法，其特征在于，包括以下几种步骤：
步骤1：Ag2Ta4O11/Ag8(Ta0.5Nb0.5)26O69的制备：将一定量的聚乙烯吡咯烷酮加入100毫升的乙醇溶液中，搅拌15分钟后，加入物质量比为1：1：0.5的五氧化二钽、硝酸银和五氧化二铌，继续搅拌30分钟后，加热至120 oC并保持2小时，然后将材料干燥后800 oC下加热4小时得到白色二元固体材料；
步骤2：三元催化剂Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69的制备：将制备的二元固体材料平铺于表面上，用300W紫外光照射30分钟，通过原位还原法得到三元催化剂Ag2Ta4O11/Ag/Ag8(Ta0.5Nb0.5)26O69；
步骤3：光催化反应条件：将合成的三元催化剂15毫克通过乙醇均匀分散于玻璃表面，干燥后放于体积为2升的反应器中，配有空气循环装置，光源为300 W氙灯带有可见光滤光片，波长大于420纳米；反应器中甲醛与苯通过空气鼓泡法带入反应装置，通过调节气流来控制浓度，用气体红外检测器和气相色谱来检测反应气体中物质的变化。
2.根据权利要求1所述的制备方法，其特征在于，反应原料为分析纯的聚乙烯吡咯烷酮、五氧化二钽、五氧化二铌、硝酸银、乙醇。
3.根据权利要求1所述的制备方法，其特征在于，步骤3的光催化反应为处理室内环境的甲醛和苯。
4.根据权利要求1所述的制备方法，其特征在于，步骤3的光催化反应条件为，利用可见光将甲醛与苯氧化为二氧化碳和水，产物二氧化碳的选择性99%以上。
5.根据权利要求1所述的制备方法制备得到的三元催化剂处理室内甲醛与苯，其特征在于，甲醛与苯的初始浓度分别为1.22 ppm和0.40 ppm，催化剂投入量15毫克，反应容器体积2升，可见光源为300W氙灯，测试温度为20 oC，辅以空气循环装置，光照10小时后，甲醛降解率为100%，苯降解率为83%。
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