CN107029763A - 一种磷酸铋/碳复合光催化剂的制备方法 - Google Patents
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
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Abstract
本发明公开了一种提供一种磷酸铋/碳复合光催化剂的制备方法。首先采用沉淀法制备植酸铋：取一定量的硝酸铋溶于500mL蒸馏水中，再加入硝酸使其完成溶解，再加入一定量的植酸，生产白色植酸铋沉淀。再在惰性气氛中原位碳化：将干燥后的样品在惰性气体气氛炉中350‑700℃烧结1‑10h小时，降温后得到磷酸铋/碳复合光催化剂。该方法操作简便、条件温和、产率高，所制备的磷酸铋/碳复合光催化剂提高了可见光的吸收、光致电荷的分离效率，从而提高其光催化性能。
Description
技术领域
本发明所属技术领域为光催化、光电化学材料技术领域，特别涉及磷酸铋/碳复合光催化剂的开发及制备方法。
背景技术
新型铋基光催化剂不仅具有在紫外和可见光照射下光催化降解有机物的能力，而且具有良好的光电转换能力和很高的光化学稳定性，如BiVO4、BiPMo12O40、BiFeO3、BiPO4等。由于BiVO4具有比较窄的禁带宽度(2.4eV)，可以直接吸收紫外/可见光光谱中的可见光，因而受到人们的重点关注，在分解水制取氢气以及降解有机污染物等方面都有研究及应用。BiFeO3是一种多铁性的光催化材料，它的禁带宽度小于2.0eV，比BiVO4的禁带宽度(2.4eV)还要窄，非常适于吸收可见光，BiFeO3也因此成为了人们的研究重点。采用水热法合成BiPO4纳米棒光催化剂具有可以控制其形貌生成的优点。BiPO4纳米棒的长径比越大，尺寸越小，其光催化活性越强。BiPO4的晶型不同，其光催化活性也不同，其单斜相的光催化活性比六方相的强。BiPO4光催化剂的禁带宽度为3.85eV，在降解亚甲基蓝方面，BiPO4光催化剂的光催化效率是TiO2光催化剂的两倍。
植酸作为抗氧化剂、保鲜剂、螯合剂、金属防腐蚀剂、蛋白质凝固剂等，广泛应用于食品工业、日用化工、医药、纺织工业、金属加工与防护业、塑料工业及高分子工业等领域当中。植酸对大部分的金属离子都有极强的络合能力，络合力与EDTA较为相似，但比EDTA具有更广泛的应用范围。植酸可以与二价以上的金属盐产生定性沉淀。通过植酸与铋盐沉淀反应生成植酸铋，再进行原位烧结碳还原，构建磷酸铋/碳复合光催化剂，提高磷酸铋光催化剂对可见光的吸收、光致电荷的分离效率，从而提高其光催化性能。希望其突出的性能可以在光催化领域有实际的应用，有效解决现在社会环境污染问题。
发明内容
本发明的目的是提供一种磷酸铋/碳复合光催化剂的制备方法，该方法操作简便、条件温和、产率高，所制备的磷酸铋/碳复合光催化剂具有很高的光催化活性。
具体步骤为：
(1)称0.01mol g硝酸铋溶于500mL蒸馏水中，再加入5mL 6mol/L的强酸溶液，在10-50℃下磁力搅拌加热，至晶体完全溶解，再加入0.5-10g植酸，继续搅拌15min。静置3h，然后离心分离。将白色植酸铋沉淀放干燥箱中60℃下干燥4h备用。
(2)将干燥后的样品在在气氛炉中烧结1-10h小时，温度范围350-700℃，降温后得到磷酸铋/碳复合光催化剂。
步骤(1)中所述强酸为硫酸、硝酸中的一种；
步骤(2)中的气氛炉的保护气为氩气、氮气惰性气体。
所述化学试剂纯度均为化学纯以上纯度。
本发明植酸铋在一定温度下烧结后形成磷酸铋/碳复合光催化材料。使用紫外/可见近红外分光光度计测出磷酸铋/碳复合光催化剂的对可见光的吸收明显增强，氩气中，650℃下烧结的BiPO4/C复合光催化剂材料的结晶性较好，碳在晶体中均匀分布，碳的加入与磷酸铋形成异质结有利于提高光催化剂的电导率，有利于电子空穴对的分离。因此，BiPO4/C复合光催化剂作为一种可见光响应材料，在环境污染如降解染料、光催化处理污水，太阳能电池等方面具有很大的应用潜能。
附图说明
图1为本发明实施例1制备的氩气中不同温度烧结的BiPO4的XRD图。
图2为本发明实施例1制备氩气中650℃下烧结的样品的不同放大倍率SEM图。
图3为本发明实施例1四种样品的紫外/可见吸收光谱图。
图4为本发明实施例1制备的样品光催化降解罗丹明B曲线图。
具体实施方式
实施例1：
(1)采用沉淀法制备植酸铋：称0.01mol g硝酸铋溶于500mL蒸馏水中，再加入20mL6mol/L的硝酸溶液，在40℃下磁力搅拌至晶体完全溶解，再加入2g植酸，继续搅拌15min。静置3h，然后离心分离。将白色植酸铋沉淀放干燥箱中60℃下干燥4h备用。(2)惰性气体中原位碳化：将干燥后的样品在氩气气氛炉中500℃烧结4h小时，降温后得到磷酸铋/碳复合光催化剂。
光催化性能的评价：将50mg复合光催化剂加入到装有50mL的20mg/L的罗丹明B的石英管中，在超声分散15min，超声过程中样品要避光。之后放入磁性转子，放到光化学反应仪中。开启低温度冷却液循环泵，将温度降到5℃以下，开启反应器，用1000W的高压汞灯进行照射，每隔一定时间取样一次，然后用罗丹明B标准溶液进行参比对照，测出该时刻罗丹明B的剩余浓度，继续测量，待各种样品完全降解罗丹明B，记录罗丹明B降解的时间。磷酸铋/碳复合光催化剂降解罗丹明B的时间为40min，较磷酸铋(100min)大幅降低，且650℃下烧结的BiPO4/C复合光催化剂材料的光催化性能(35min)最好。
实施例2：
(1)称0.01mol g硝酸铋溶于500mL蒸馏水中，再加入10mL 6mol/L的硫酸溶液，在40℃下磁力搅拌至晶体完全溶解，再加入3g植酸，继续搅拌15min。静置3h，然后离心分离。将白色植酸铋沉淀放干燥箱中60℃下干燥4h备用。(2)将干燥后的样品在氩气气氛炉中650℃烧结2h小时，降温后得到磷酸铋/碳复合光催化剂。合成的磷酸铋/碳复合光催化剂降解罗丹明B的时间为40min。
实施例3：
(1)称0.01mol g硝酸铋溶于500mL蒸馏水中，再加入10mL 6mol/L的硝酸溶液，在40℃下磁力搅拌至晶体完全溶解，再加入3g植酸，继续搅拌15min。静置3h，然后离心分离。将白色植酸铋沉淀放干燥箱中60℃下干燥4h备用。(2)将干燥后的样品在氮气气氛炉中700℃烧结2h小时，降温后得到磷酸铋/碳复合光催化剂。合成的磷酸铋/碳复合光催化剂降解罗丹明B的时间为45min。
Claims (1)
1.一种磷酸铋/碳复合光催化剂的制备，其特征在于具体步骤为：
(1)称0.01mol g硝酸铋溶于500mL蒸馏水中，再加入5-40mL 6mol/L的强酸溶液，在10-50℃下磁力搅拌加热，至晶体完全溶解，再加入0.5-10g植酸，继续搅拌15min。静置3h，离心分离。得到的白色植酸铋沉淀放在干燥箱中60℃下干燥4h备用。
(2)将干燥后的样品在在气氛炉中烧结1-10h小时，温度范围350-700℃，降温后得到磷酸铋/碳复合光催化剂。
步骤(1)中所述强酸为硫酸、硝酸中的一种；
步骤(2)中的气氛炉的保护气为氩气、氮气惰性气体。
所述化学试剂纯度均为化学纯以上纯度。
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