CN108654589A - 用于降解苯酚的高比表面积多孔碳基二氧化钛光催化剂的制备方法 - Google Patents
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Abstract
本发明涉及环保技术领域，具体涉及一种用于降解水体中苯酚的高比表面积多孔碳基二氧化钛光催化剂的制备方法，包括如下步骤：以钛基金属有机框架化合物为前驱体，先通过高温碳化制备含钛碳基复合材料，经过氯化锌溶液浸渍后，再进行高温活化、水洗、烘干，得到用于降解水体中苯酚的高比表面积多孔碳基二氧化钛光催化剂。本发明制备方法简单、实用，还可以通过改变钛基金属有机框架化合物的种类、活化温度对光催化剂的性能进行调节，所获得的多孔碳基二氧化钛光催化剂具有多孔性好、孔的形状可调控、比表面积高、催化活性高等优点。
Description
技术领域
本发明涉及环保技术领域，具体涉及一种用于降解水体中苯酚的高比表面积多孔碳基二氧化钛光催化剂的制备方法。
背景技术
目前水体中苯酚的光催化降解研究中，最常见的光催化剂是二氧化钛，其优点是廉价无毒，催化活性高，选择性好，反应条件温和，不腐蚀设备，而且二次污染小，制备工艺简单。但二氧化钛用作光催化剂时降解苯酚的光催化效率较低，因为其本身对有机物的吸附能力较差。此外，二氧化钛光催化剂一般比表面积大、表面能高，极易发生团聚，在降解水体中有机物过程中分散不均匀、失活快、分离和回收困难，还有可能成为污染物，使其应用受到了限制。
从实际应用和商业化考虑，二氧化钛光催化剂的活性需要进一步提高和改进，因此制备结晶度高、颗粒尺寸小、比表面积大的二氧化钛光催化剂是必要的。同时，为了解决二氧化钛光催化剂分离和回收困难的问题，并克服二氧化钛颗粒易团聚、稳定性差、对有机物吸附能力差的缺点，制备负载型二氧化钛光催化剂也是必要的。基于以上原因，人们对二氧化钛的制备方法以及二氧化钛同其它多孔材料的联用技术进行了大量研究，如分子筛、膜、多孔碳等多孔材料都被作载体来负载二氧化钛。但是，目前采用氯化锌活化法制备高比表面积多孔碳基二氧化钛光催化剂的研究报道还极为缺乏。
本发明采用具有不同孔道结构和化学特性的金属有机框架化合物前驱体，通过氯化锌活化法来制备高比表面积多孔碳基二氧化钛光催化剂，所获得的光催化剂用于降解苯酚时，具有多孔性好、孔的形状可调控、比表面积高、催化活性高等优点，是一条可行的途径。
发明内容
本发明所要解决的技术问题是针对上述现有技术提供一种用于降解水体中苯酚的多孔性好、孔的形状可调控、比表面积高、催化活性高的多孔碳基二氧化钛光催化剂的制备方法。
本发明解决上述技术问题所采用的技术方案为：一种用于降解苯酚的高比表面积多孔碳基二氧化钛光催化剂的制备方法，其特征在于包括以下步骤：a，称取一定量的钛基金属有机框架化合物放入管式炉，在氩气气流下，升温至400℃高温碳化5h，制得含钛碳基复合材料；b，将得到的含钛碳基复合材料加入氯化锌溶液，于20℃浸渍24h；c，将沉淀取出，真空烘干后，放入管式炉中，在氩气气流下，升温至一定的温度活化2h；d，将活化后的产物用去离子水洗涤至滤液的pH为6～7，真空烘干后，得到高比表面积多孔碳基二氧化钛光催化剂。
作为优选，步骤a所述钛基金属有机框架化合物为ZTOF-1、MIL-125、NH2-MIL-125之一种或几种。
作为优选，步骤c所述沉淀的活化温度为600～1000℃。
与现有技术相比，本发明的优点在于：制备方法简单、实用，还可以通过改变钛基金属有机框架化合物前驱体的种类、活化温度对光催化剂的性能进行调节，所获得的多孔碳基二氧化钛光催化剂具有多孔性好、孔的形状可调控、比表面积高、催化活性高等优点，本发明可用于环保技术领域，特别是用于降解水体中苯酚的光催化剂的制备中。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1：
称取0.4g的ZTOF-1放入管式炉，在氩气气流下以10℃/min的速率升温至400℃，并保温5h，制得0.19g含钛碳基复合材料。将得到的含钛碳基复合材料加入5mL质量浓度为20％的氯化锌溶液中，于20℃浸渍24h后，将沉淀取出，在80℃下真空烘24h，放入管式炉，在氩气气流下以10℃/min的速率升温至1000℃，并保温2h，将活化后的产物用去离子水洗涤至滤液的pH为6～7，真空烘干后，得到0.16g多孔碳基二氧化钛光催化剂，其比表面积为3023m2/g，记为1#光催化剂。
多孔碳基二氧化钛光催化剂在水溶液中对于苯酚的光催化降解实验使用西安比朗仪器公司BILON-GHX-1D多功能光化学反应仪，并采用1000W的高压氙灯作为光源。称取0.06g的1#光催化剂，然后将其加入到60mL浓度为0.06g/L的苯酚水溶液中，并不断搅拌，加入1#光催化剂的苯酚水溶液在氙灯照射下经1.5h光催化降解后，苯酚降解率达到87.1％，是一种高效的光催化材料。
实施例2：
其他同1#光催化剂，多孔碳基二氧化钛光催化剂制备时活化温度为800℃，得到0.17g多孔碳基二氧化钛光催化剂，其比表面积为3270m2/g，记为2#光催化剂，其它与实施例1是类似的。加入2#光催化剂的苯酚水溶液在氙灯照射下经1.5h光催化降解后，苯酚降解率达到96.3％。
对比例1：
称取0.4g的ZTOF-1放入管式炉，在氩气气流下以10℃/min的速率升温至400℃，并保温5h，制得0.19g含钛碳基复合材料。将得到的含钛碳基复合材料在氩气气流下以10℃/min的速率继续升温至800℃，并保温2h，得到0.16g多孔碳基二氧化钛光催化剂，其比表面积为112m2/g，记为3#光催化剂。3#光催化剂在水溶液中对于苯酚的光催化降解实验与实施例1是类似的。加入3#光催化剂的苯酚水溶液在氙灯照射下经1.5h光催化降解后，苯酚降解率为51.3％，明显低于2#光催化剂。
实施例3：
其他同1#光催化剂，多孔碳基二氧化钛光催化剂制备时活化温度为600℃，得到0.18g多孔碳基二氧化钛光催化剂，其比表面积为2885m2/g，记为4#光催化剂，其它与实施例1是类似的。加入4#光催化剂的苯酚水溶液在氙灯照射下经1.5h光催化降解后，苯酚降解率达到81.4％。
实施例4：
其他同2#光催化剂，钛基金属有机框架化合物为MIL-125，得到0.22g多孔碳基二氧化钛光催化剂，其比表面积为2765m2/g，记为5#光催化剂，其它与实施例2是类似的。加入5#光催化剂的苯酚水溶液在氙灯照射下经1.5h光催化降解后，苯酚降解率达到82.1％。
实施例5：
其他同2#光催化剂，钛基金属有机框架化合物为NH2-MIL-125，得到0.24g多孔碳基二氧化钛光催化剂，其比表面积为2690m2/g，记为6#光催化剂，其它与实施例2是类似的。加入6#光催化剂的苯酚水溶液在氙灯照射下经1.5h光催化降解后，苯酚降解率达到78.2％。
Claims (3)
1.一种用于降解苯酚的高比表面积多孔碳基二氧化钛光催化剂的制备方法，其特征在于包括以下步骤：a，称取一定量的钛基金属有机框架化合物放入管式炉，在氩气气流下，升温至400℃高温碳化5h，制得含钛碳基复合材料；b，将得到的含钛碳基复合材料加入氯化锌溶液，于20℃浸渍24h；c，将沉淀取出，真空烘干后，放入管式炉中，在氩气气流下，升温至一定的温度活化2h；d，将活化后的产物用去离子水洗涤至滤液的pH为6～7，真空烘干后，得到高比表面积多孔碳基二氧化钛光催化剂。
2.根据权利要求1所述的制备方法，其特征在于：步骤a的钛基金属有机框架化合物为ZTOF-1、MIL-125、NH2-MIL-125之一种或几种。
3.根据权利要求1所述的制备方法，其特征在于：在步骤c中，沉淀的活化温度为600～1000℃。
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|---|---|---|---|---|
| CN110508271A (zh) * | 2019-08-21 | 2019-11-29 | 西南林业大学 | 一种锌改性水泥光催化剂的制备方法 |
| CN111215042A (zh) * | 2020-01-21 | 2020-06-02 | 广东工业大学 | 一种碳掺杂二氧化钛光催化剂及其制备方法与应用 |
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2017
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110508271A (zh) * | 2019-08-21 | 2019-11-29 | 西南林业大学 | 一种锌改性水泥光催化剂的制备方法 |
| CN111215042A (zh) * | 2020-01-21 | 2020-06-02 | 广东工业大学 | 一种碳掺杂二氧化钛光催化剂及其制备方法与应用 |
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