CN106219508A - 一种混合形态结构磷酸锑的简易制备方法 - Google Patents
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Abstract
本发明涉及一种混合形态结构磷酸锑的简易制备方法,将二乙三胺五乙酸和三氯化锑依次溶解于去离子水中,在60℃水浴条件下,充分搅拌;然后加入磷酸二氢铵,充分搅拌,形成前驱体混合溶液;将所得将前驱体混合溶液倒入聚四氟乙烯内衬不锈钢水热反应釜中,在160℃下恒温水热反应10h,离心洗涤干燥,得到产品。本发明的方法简单易操作,环保,成本低廉,产品纯净,所制得的磷酸锑能够高效去除水中的有机污染物,具有良好的应用前景。本发明制备得到的磷酸锑的光催化活性明显高于商用金红石TiO2。
Description
技术领域
本发明涉及光催化材料领域,具体涉及一种混合形态结构磷酸锑的简易制备方法。
背景技术
由于半导体材料具有优良的光催化性能,在环境污染物降解方面具有良好的应用前景,因此备受人们关注,发现和报道的光催化剂也与日俱增。纳米结构由零维或一维聚集成多维的纳米超结构时,能够出现新的性能,例如:光学、电学、磁学和催化性能。纳米单元组装成的纳米超结构,已经称为目前的研究热点之一,例如:空心球、三维花状纳米结构等。由于半导体材料具有优良的光催化应用性能,被发现和报道的光催化剂也与日俱增。
磷酸锑属于单斜晶系,由于锑离子中存在孤对电子,所以磷酸锑具有良好的吸附、润滑、非线性光学、掺杂、磁性和导电性等特性,广泛应用于低损耗光纤波导、玻璃、激光眼睛、层状材料的添加剂等。目前制备纯相磷酸锑的方法较少。
发明内容
本发明的目的是提供一种混合形态结构磷酸锑的简单制备方法,及其光催化活性。
为达到上述目的,本发明提供的技术方案是:
一种混合形态结构磷酸锑的简易制备方法,包括以下步骤:
(1)将二乙三胺五乙酸和三氯化锑依次溶解于去离子水中,在60℃水浴条件下,充分搅拌;继续加入磷酸二氢铵,充分搅拌,形成前驱体混合溶液;
(2)将步骤(1)所得将前驱体混合溶液倒入聚四氟乙烯内衬不锈钢水热反应釜中,在160℃下恒温水热反应10h,离心洗涤干燥,得到产品。
所述的混合形态为纳米棒和纳米超结构混合;所述纳米棒磷酸锑具有四棱柱状结构,棒的长度在35~45μm之间,横截面的边长在0.15~0.9μm之间;所述的纳米超结构磷酸锑为纳米片组装的不规则超结构球体,球体直径在10~17μm之间,纳米片的厚度约为0.15μm。
所述二乙三胺五乙酸:三氯化锑:磷酸二氢铵的摩尔比为1:1:1。
反应原料的加入顺序为:三胺五乙酸、三氯化锑、磷酸二氢铵,且在加入二乙三胺五乙酸和三氯化锑后,充分搅拌1h后,再加入磷酸二氢铵,再充分搅拌0.5h。
二乙三胺五乙酸、三氯化锑、磷酸二氢铵加入的量分别为5mmol,去离子水的加入量为65mL。
步骤(2)中所述洗涤为依次用无水乙醇和去离子水各洗涤三次。
步骤(2)中所述干燥为在60℃真空干燥12h。
本发明还提供了上述制备的混合形态结构磷酸锑作为光催化剂的应用。
有益效果:
本发明的方法简单易操作,环保,成本低廉,产品纯净,所制得的磷酸锑能够高效去除水中的有机污染物,具有良好的应用前景。本发明制备得到的磷酸锑的光催化活性明显高于商用金红石TiO2。
附图说明
图1为混合形态结构中磷酸锑纳米棒的扫描电子显微镜(SEM)图;
图2为混合形态结构中磷酸锑纳米超结构的扫描电子显微镜(SEM)图;
图3为混合形态结构磷酸锑的X射线衍射(XRD)图;
图4为混合形态结构磷酸锑和TiO2光催化降解RhB的活性对比曲线图;
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例
在60℃水浴条件下,将1.965g二乙三胺五乙酸和1.141g三氯化锑加入65mL的去离子水中,充分搅拌1h;加入0.575g三氯化锑,充分搅拌0.5h,形成前驱体混合溶液。将前驱体混合溶液倒入50mL聚四氟乙烯内衬不锈钢水热反应釜中,在160℃下恒温水热反应10h,离心洗涤干燥。
对制备得到的磷酸锑进行了电子显微镜观察和X射线衍射测定。
从图1中可见,本发明制备的磷酸锑纳米棒具有四棱柱状结构,棒的长度35~45μm,截面的边长0.15~0.9μm。
从图2中可见,本发明制备的混合形态结构中磷酸锑纳米片组装的微球,微球直径10~17μm,纳米片的厚度约为0.15μm。
从图3中可见,与XRD标准卡No.35-0829比较,该产品是纯的SbPO4。
测试例
将制得的混合形态结构磷酸锑和商用金红石TiO2(Commercial Rulite)分别作为光催化剂降解罗丹明B,进行两次活性测试。
配制200mL浓度为0.01g/L的RhB溶液。用电子天平称取0.1g的磷酸锑样品,加入上述溶液,在避光的条件下搅拌30min,使溶液达到吸附-解附平衡。30min后,将达到吸附平衡的溶液取样离心,上层清液用UV-vis对RhB溶液的吸光度进行测量,其吸收度记为C0。对上述达到吸附平衡的溶液在搅拌下进行紫外光照射,进行光催化反应,灯电流15A,灯距为15cm,每次间隔10min进行取样分析。取样后均先离心,取得上层清液用UV-vis对RhB溶液的吸光度进行测量,根据Lambert–Beer定律,有机物特征吸收峰强度的变化,可以定量计算其浓度变化。当吸光物质相同、厚度相同时,可以用吸光度的变化直接表示溶液浓度的变化。因此,将吸光度直接记为浓度符号:C1,C2,C3。将每隔10min测得的RhB溶液的吸光度,绘制催化活性曲线,分析样品的光催化降解RhB的能力。从图4中可见,本发明制备得到的磷酸锑的光催化活性明显高于商用金红石TiO2。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何形式上的限制,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,依据本发明的技术实质,对以上实施例所作的任何简单的修改、等同替换与改进等,均仍属于本发明技术方案的保护范围之内。
Claims (8)
1.一种混合形态结构磷酸锑的简易制备方法,其特征在于:包括以下步骤:
(1)将二乙三胺五乙酸和三氯化锑依次溶解于去离子水中,在60℃水浴条件下,充分搅拌;继续加入磷酸二氢铵,充分搅拌,形成前驱体混合溶液;
(2)将步骤(1)所得将前驱体混合溶液倒入聚四氟乙烯内衬不锈钢水热反应釜中,在160℃下恒温水热反应10h,离心洗涤干燥,得到产品。
2.如权利要求1所述的混合形态结构磷酸锑的简易制备方法,其特征在于:所述的混合形态为纳米棒和纳米超结构混合;所述纳米棒磷酸锑具有四棱柱状结构,棒的长度在35~45μm之间,横截面的边长在0.15~0.9μm之间;所述的纳米超结构磷酸锑为纳米片组装的不规则超结构球体,球体直径在10~17μm之间,纳米片的厚度约为0.15μm。
3.如权利要求1所述的混合形态结构磷酸锑的简易制备方法,其特征在于:所述二乙三胺五乙酸:三氯化锑:磷酸二氢铵的摩尔比为1:1:1。
4.如权利要求1所述的混合形态结构磷酸锑的简易制备方法,其特征在于:反应原料的加入顺序为:三胺五乙酸、三氯化锑、磷酸二氢铵,且在加入二乙三胺五乙酸和三氯化锑后,充分搅拌1h后,再加入磷酸二氢铵,再充分搅拌0.5h。
5.如权利要求1所述的混合形态结构磷酸锑的简易制备方法,其特征在于:二乙三胺五乙酸、三氯化锑、磷酸二氢铵加入的量分别为5mmol,去离子水的加入量为65mL。
6.如权利要求1所述的混合形态结构磷酸锑的简易制备方法,其特征在于:步骤(2)中所述洗涤为依次用无水乙醇和去离子水各洗涤三次。
7.如权利要求1所述的混合形态结构磷酸锑的简易制备方法,其特征在于:步骤(2)中所述干燥为在60℃真空干燥12h。
8.权利要求1所制备的混合形态结构磷酸锑作为光催化剂的应用。
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CN110589789A (zh) * | 2019-09-07 | 2019-12-20 | 中南大学 | 一种负极材料纳米针状磷酸锑的制备方法 |
CN117317199A (zh) * | 2023-11-20 | 2023-12-29 | 湖南娄底华星锑业有限公司 | 一种锑基负极材料及其制备方法 |
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CN104843661A (zh) * | 2015-04-29 | 2015-08-19 | 岭南师范学院 | 一种无模板合成磷酸锑微球的制备方法 |
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CN110589789A (zh) * | 2019-09-07 | 2019-12-20 | 中南大学 | 一种负极材料纳米针状磷酸锑的制备方法 |
CN110589789B (zh) * | 2019-09-07 | 2023-02-17 | 中南大学 | 一种负极材料纳米针状磷酸锑的制备方法 |
CN117317199A (zh) * | 2023-11-20 | 2023-12-29 | 湖南娄底华星锑业有限公司 | 一种锑基负极材料及其制备方法 |
CN117317199B (zh) * | 2023-11-20 | 2024-03-22 | 湖南娄底华星锑业有限公司 | 一种锑基负极材料及其制备方法 |
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