CN107983376A - 一种钛酸钇铅/氯氧化铋及制备方法 - Google Patents
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Abstract
本发明涉及一种钛酸钇铅/氯氧化铋及制备方法。本发明制备方法步骤如下：先将醋酸铅加入去醋酸中，将Ti(OC4H9)4加入到乙醇和醋酸和混合溶液中，将两溶液混合后再加入醋酸钇溶液，干燥、研磨、高温煅烧后得到钛酸钇铅，将获得的钛酸钇铅粉末与氧化铋粉末混合、分散后加入氢氯酸溶液，搅拌、洗涤、烘干后得到一种钛酸钇铅/氯氧化铋粉末。本发明具有操作简单，制备成本低，条件温和，易于实现工业化等优点。
Description
技术领域
本发明属于功能材料领域，涉及一种钛酸钇铅/氯氧化铋及制备方法。
背景技术
近年来，随着全球工业化进程的迅速发展，环境污染问题日益突出。光催化技术以其直接利用太阳光来解决水体污染的优势，得到了越来越多的关注，光催化剂是这项技术的核心。氯氧化铋在光照条件下可以催化分解水制氢和降解有机污染物，但由于其禁带宽度（禁带宽度为3.4eV）较大，故只能吸收紫外光光子。但是，紫外光仅占太阳光的3%～5%，而可见光约占太阳能的43%，因此，如将氯氧化铋的光降解吸收波段调节至可见光波段将具有重要的现实意义。在专利CN104785280A中公开了一种片状二氧化钛/溴氧化铋复合光催化剂及其制备方法，该复合光催化剂由溴氧化铋沉积在二氧化钛纳米片上形成的异质复合材料，其制备步骤包括：将二氧化钛纳米片、巯基乙酸、溴化钾超声分散于去离子水中，混合得均匀的溶液，将硝酸铋溶于乙二醇中；然后将上述两种溶液混合得到乳白色乳浊液，搅拌后静置，离心分离洗涤后得到二氧化钛/溴氧化铋复合光催化剂。现有技术的复杂性导致成本过高，不易实现工业化生产。迄今为止，钛酸钇铅/氯氧化铋的相关工作尚未见报道，本发明中通过引入第二相钛酸铅基材料吸收可见光光子从而产生电子空穴对，电子空穴对再迁移到氯氧化铋表面参加反应，最终实现氯氧化铋的可见光光催化作用，提高氯氧化铋的光生载流子分子，从而开发具有实用价值的材料。
发明内容
本发明的目的在于提供一种钛酸钇铅/氯氧化铋高效光催化剂的制备方法，具有成本低，生产周期短，易于大规模生产等优点。
本发明采用如下技术方案：
一种钛酸钇铅/氯氧化铋及制备方法，包括以下步骤：
步骤1，将醋酸铅加入去醋酸中，搅拌至均匀，形成A液；
步骤2，将Ti(OC4H9)4加入到乙醇和醋酸和混合溶液中，得到B液；
步骤3，将醋酸钇加入到醋酸中得到醋酸钇溶液，然后加入到A液与B液混合溶液中，形成C液；
步骤4，将C液前驱体干燥、研磨、煅烧后得到钛酸钇铅；
步骤5，将氧化铋粉末与步骤4中得到的钛酸钇铅混合，加入去离子水后超声分散，然后将氢氯酸溶液加入到上述体系中，其中钛酸钇铅与氧化铋摩尔比为1：(0~0.5)，氧化铋与氢氯酸摩尔比为1：(7~10)，将沉淀使用乙醇和去离子水反复洗涤3次，干燥后得到钛酸钇铅/氯氧化铋。
所述的钛酸钇铅/氯氧化铋及制备方法，其特征在于，所述钛酸钇铅/氯氧化铋中的钛酸钇铅结构为四方相，氯氧化铋为四方相结构。所述的钛酸钇铅/氯氧化铋在光催化方面的应用。与现有技术相比，本发明具有以下有益效果：
(1)本发明采用水热法与溶胶法相结合制备了钛酸钇铅/氯氧化铋复合光催化剂，其中氯氧化铋为四方相，钇的引入并没有改变钛酸铅的物相，仍保持为钙钛矿相。本发明具有制备周期短、生产成本低、工艺方法简便等优点。
(2) 本发明比传统的物理混合或表面生成的方法更加有效提高钛酸钇铅与氯氧化铋的有效接触面积，利于得到更加高效的钛酸钇铅/氯氧化铋复合光催化剂。钛酸钇铅/氯氧化铋在可见光照210min后脱色率可达93％，钛酸钇铅粉体在可见光照210min后的脱色率为25％，氯氧化铋在可见光照射210min后脱色率为36%，钛酸钇铅/氯氧化铋的脱色率较氯氧化铋和钛酸钇铅有很大的提高。
附图说明
图1是本发明实施例2中制备的钛酸钇铅/氯氧化铋的XRD衍射图谱；
图2是本发明实施例2中制备的钛酸钇铅/氯氧化铋的扫描电镜图；
图3是本发明实施例1～3中制备的氯氧化铋、钛酸钇铅和钛酸钇铅/氯氧化铋的光催化脱色率曲线。
具体实施方式
下面结合附图和本发明优选的具体实施例对本发明做进一步描述，原料均为分析纯。
实施例1：
步骤1，将9.99mmol的醋酸铅加入去醋酸中，形成A液；
步骤2，将10mmol的将Ti(OC4H9)4加入到乙醇和醋酸和混合溶液中后形成B液；
步骤3，将含0.01mmol的醋酸钇溶液加入到A液与B液混合溶液中，得到C液，其中Ti(OC4H9)4与(醋酸铅+醋酸钇)的摩尔比为1:1，Ti(OC4H9)4与醋酸钇摩尔比为1：0.01；
步骤4，所得到的C液将干燥、研磨、在600℃煅烧3小时后得到钛酸钇铅。
实施例2：
步骤1，将9.99mmol的醋酸铅加入去醋酸中，形成A液；
步骤2，将10mmol的将Ti(OC4H9)4加入到乙醇和醋酸和混合溶液中后形成B液；
步骤3，将含0.01mmol的醋酸钇溶液加入到A液与B液混合溶液中，得到C液，其中Ti(OC4H9)4与(醋酸铅+醋酸钇)的摩尔比为1:1，Ti(OC4H9)4与醋酸钇摩尔比为1：0.01；
步骤4，所得到的C液将干燥、研磨、在600℃煅烧3小时后得到钛酸钇铅；
步骤5，将氧化铋粉末与步骤4中得到的钛酸钇铅混合，加入去离子水后超声分散，然后将氢氯酸溶液加入到上述体系中，其中钛酸钇铅与氧化铋摩尔比为1：0.25，氧化铋与氢氯酸摩尔比为1：7，将得到的沉淀使用乙醇和去离子水反复洗涤3次，干燥后得到钛酸钇铅/氯氧化铋。
实施例3：
将一定量的氧化铋粉末加入到去离子水中后超声分散，然后将氢氯酸溶液加入到上述体系中，其中氧化铋与氢氯酸摩尔比为1：7，将沉淀使用乙醇和去离子水反复洗涤3次，干燥后得到氯氧化铋。
应用例：
对实施列1～3中所制得的氯氧化铋、钛酸钇铅和钛酸钇铅/氯氧化铋进行光催化活性评价，具体操作步骤为：
称量实施例1～3中所制得的氯氧化铋、钛酸钇铅和钛酸钇铅/氯氧化铋分别取光催化剂100 mg，将其加入到罗丹明B染料溶液中(100mL，3.13×10-5mol·L-1)，避光搅拌1h，待脱吸附达到平衡后打开500W氙灯光源，每隔30min检测一次染料的浓度，在给定时间内表征出所制备材料对罗丹明B的催化脱色情况。
以上所述内容仅为本发明构思下的基本说明，通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换，均应属本发明的保护范围。
Claims (7)
1.一种钛酸钇铅/氯氧化铋及制备方法，其特征在于钛酸钇铅/氯氧化铋中钛酸钇铅为钙钛矿结构，氯氧化铋为四方相结构，包括以下制备步骤：
步骤1，将醋酸铅加入去醋酸中，搅拌至均匀，形成A液；
步骤2，将Ti(OC4H9)4加入到乙醇和醋酸和混合溶液中，得到B液；
步骤3，将醋酸钇加入到醋酸中得到醋酸钇溶液，然后加入到A液与B液混合溶液中，形成C液；
步骤4，将C液前驱体干燥、研磨、煅烧后得到钛酸钇铅；
步骤5，将氧化铋粉末与步骤4中得到的钛酸钇铅混合，加入去离子水后超声分散，然后将氢氯酸溶液加入到上述体系中，其中钛酸钇铅与氧化铋摩尔比为1：(0~0.5)，氧化铋与氢氯酸摩尔比为1：(7~10)，将得到的沉淀使用乙醇和去离子水反复洗涤3次，干燥后得到钛酸钇铅/氯氧化铋。
2.所述步骤1中醋酸铅的浓度为0.08～0.30mol/L。
3.所述步骤2中Ti(OC4H9)4的浓度为0.08～0.30mol/L。
4.所述步骤3中醋酸钇溶液的浓度为0.06～0.12mol/L，Ti(OC4H9)4与(醋酸铅+醋酸钇)的摩尔比为1:1，醋酸铅与醋酸钇摩尔比为1：(0～0.02)。
5.所述步骤4中煅烧温度为375～725℃。
6.所述步骤5中钛酸钇铅与氧化铋摩尔比为1：(0~0.5)，氢氯酸浓度为0.008～0.010mol/L，氧化铋与氢氯酸摩尔比为1：(6~9)。
7.所述的钛酸钇铅/氯氧化铋在光催化方面的应用。
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