CN106215930A - 一种新型钒酸铋光催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种新型钒酸铋光催化剂的制备方法,按照重量份数称取各原料:硝酸铋40‑60份、偏钒酸铵10‑15份、聚乙二醇5‑10份、赤泥5‑10份、氮化硅5‑10份、金属卟啉2‑4份和壳聚糖5‑10份;将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;将溶液A与溶液B混合,得混合液;将混合液、聚乙二醇、赤泥、氮化硅、金属卟啉和壳聚糖加入球磨机,再加入适量水搅拌,得糊状物;先用蒸馏水洗涤糊状物,干燥,研磨,焙烧,即得光催化剂。本发明具有原料来源广泛、成本低廉、制备工艺简单、生产效率高、能耗低、催化活性高、催化效率高等优点,能高效催化降解废水有机污染物,具有很好的经济效益、社会效益和生态效益,市场前景广阔。
Description
技术领域
本发明涉及光催化材料技术领域,具体是一种新型钒酸铋光催化剂的制备方法。
背景技术
21世纪以来,随着工业化步伐的提升和自然资源的过度使用,伴随着各种环境污染、能源稀缺问题不断加剧。因此,治理各种污染,寻找新能源以缓解地球的压力迫在眉睫。光催化技术已经在废水处理、气体净化、杀菌、防污、自洁材料、染料敏化太阳能电池、化妆品、气体传感器等许多领域有着广泛的应用。光催化是基于半导体材料在光激发下能够产生具有强还原性的光生电子和具有强氧化性的空穴的基本特性,固体光催化剂能吸收太阳光将水和生物质分解成氢气,也能将空气和水体环境中的有机污染物和无机污染物氧化或还原降解为无害物质。因此,具有低能耗、绿色环保的特点。
目前,国内外研究最多的半导体光催化材料主要是金属氧化物和硫化物,如Ti02,W03,ZnO,Fe203,CdS等。钒酸铋,作为单斜晶系白钨矿结构,在可见光照射时具有光催化活性,可以催化水分子分解产生氧和降解有机污染物,是一种很有发展前景的催化剂。然而,钒酸铋产生的光生电子- 空穴对容易在催化剂体相和表面复合,导致光催化活性降低。同时钒酸铋因其颗粒过于细微,在使用环境中易于失活和凝聚、不易沉降,导致其很难分离、回收和重复利用。为解决上述问题,增加其使用稳定性,将钒酸铋负载于一定载体上,如玻璃 、硅胶 、活性炭等,但这些载体存在机械强度较弱、化学稳定性和热稳定性差等局限。因此,如何有效阻止其光生电子- 空穴对的复合,改善光生载流子的分离效率,提高钒酸铋的催化活性和稳定性,是近年来光催化的研究热点。
发明内容
本发明针对现有光催化剂存在的问题,提供一种新型钒酸铋光催化剂的制备方法。本方法制备的光催化剂具有比表面积大、催化活性高、对光源的利用率高、稳定性好、环保无毒、成本低、可多次重复使用等优点。
为了实现以上目的,本发明采用的技术方案如下:
一种新型钒酸铋光催化剂的制备方法,包括以下步骤:
(1)按照重量份数称取各原料:硝酸铋40-60份、偏钒酸铵10-15份、聚乙二醇5-10份、赤泥5-10份、氮化硅5-10份、金属卟啉2-4份和壳聚糖5-10份;
(2)将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;
(3)将溶液A放入超声波发生器中,再将溶液B倒入溶液A中,用氨水调节pH至3-4,在频率为40-60KHz下继续超声30-60min,得混合液;
(4)将混合液、聚乙二醇、赤泥、氮化硅、金属卟啉和壳聚糖加入球磨机,再加入适量水搅拌,得糊状物;
(5)先用蒸馏水洗涤糊状物,然后将糊状物在60-80℃下微波干燥2-3h,干燥后研磨成粉末,再放入马沸炉在温度为400-500℃下焙烧2-4h,即得光催化剂。
优选的,以上所述金属卟啉为铁卟啉或钴卟啉中的一种。
优选的,以上步骤(4)所述搅拌是在转速为300-500r/min下搅拌30-60min。
优选的,以上所述焙烧的升温速率为5-10℃/min。
优选的,以上步骤(5)所述研磨是将物料研磨至粒径为1.0-2.0mm。
与现有技术相比,本发明的优点及有益效果为:
1、本发明方法制得的光催化剂具有较大的比表面积、良好的孔隙结构及较多的催化活性中心,提高了催化剂的吸附性能,使得光生电子和空穴能够有效的分离,进而提高催化剂的活性和效率,扩大了催化剂在可见光范围的吸收,大大提高催化剂对太阳光的利用率。
2、本发明以聚乙二醇作为分散剂,可以解决光催化剂在使用环境中易于失活和凝聚、不易沉降的问题。
3、本发明以赤泥和氮化硅作为载体,不仅能使得催化剂性能更加稳定,更容易分离、回收及多次重复利用,还能提高催化剂的吸附性能和光催化性能。
4、本发明制备的光催化剂比表面积为150-200m2/g,60分钟内对亚甲基蓝的降解率达到92%以上。
5、本发明具有原料来源广泛、成本低廉、制备工艺简单、生产效率高、能耗低、反应条件温和、环境友好、吸附性能好、催化活性高、催化效率高等优点,在可见光辐照下能高效催化降解废水有机污染物,具有很好的经济效益、社会效益和生态效益,更适用于工业生产。
具体实施方式
下面将结合具体实施例对本方案进一步说明,但不限于本发明的保护范围。
实施例1
一种新型钒酸铋光催化剂的制备方法,包括以下步骤:
(1)按照比例称取各原料:硝酸铋40g、偏钒酸铵10g、聚乙二醇6g、赤泥5g、氮化硅8g、铁卟啉2g和壳聚糖5g;
(2)将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;
(3)将溶液A放入超声波发生器中,再将溶液B倒入溶液A中,用氨水调节pH至3,在频率为40KHz下继续超声60min,得混合液;
(4)将混合液、聚乙二醇、赤泥、氮化硅、铁卟啉和壳聚糖加入球磨机,再加100mL水搅拌,在转速为300r/min下搅拌60min,得糊状物;
(5)先用蒸馏水洗涤糊状物,然后将糊状物在60℃下微波干燥3h,干燥后研磨成粒径为1.0mm的粉末,再放入马沸炉在温度为400℃下焙烧4h,即得光催化剂。
实施例2
一种新型钒酸铋光催化剂的制备方法,包括以下步骤:
(1)按照比例称取各原料:硝酸铋50g、偏钒酸铵12g、聚乙二醇5g、赤泥10g、氮化硅5g、铁卟啉3g和壳聚糖8g;
(2)将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;
(3)将溶液A放入超声波发生器中,再将溶液B倒入溶液A中,用氨水调节pH至4,在频率为50KHz下继续超声45min,得混合液;
(4)将混合液、聚乙二醇、赤泥、氮化硅、铁卟啉和壳聚糖加入球磨机,再加100mL水搅拌,在转速为400r/min下搅拌45min,得糊状物;
(5)先用蒸馏水洗涤糊状物,然后将糊状物在70℃下微波干燥2.5h,干燥后研磨成粒径为1.0mm的粉末,再放入马沸炉在温度为450℃下焙烧3h,即得光催化剂。
实施例3
一种新型钒酸铋光催化剂的制备方法,包括以下步骤:
(1)按照比例称取各原料:硝酸铋60g、偏钒酸铵15g、聚乙二醇8g、赤泥8g、氮化硅10g、钴卟啉3g和壳聚糖10g;
(2)将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;
(3)将溶液A放入超声波发生器中,再将溶液B倒入溶液A中,用氨水调节pH至4,在频率为60KHz下继续超声30min,得混合液;
(4)将混合液、聚乙二醇、赤泥、氮化硅、钴卟啉和壳聚糖加入球磨机,再加100mL水搅拌,在转速为500r/min下搅拌30min,得糊状物;
(5)先用蒸馏水洗涤糊状物,然后将糊状物在80℃下微波干燥2h,干燥后研磨成粒径为2.0mm的粉末,再放入马沸炉在温度为500℃下焙烧2h,即得光催化剂。
实施例4
一种新型钒酸铋光催化剂的制备方法,包括以下步骤:
(1)按照比例称取各原料:硝酸铋50g、偏钒酸铵12g、聚乙二醇10g、赤泥10g、氮化硅8g、钴卟啉2g和壳聚糖8g;
(2)将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;
(3)将溶液A放入超声波发生器中,再将溶液B倒入溶液A中,用氨水调节pH至3,在频率为50KHz下继续超声60min,得混合液;
(4)将混合液、聚乙二醇、赤泥、氮化硅、钴卟啉和壳聚糖加入球磨机,再加100mL水搅拌,在转速为300r/min下搅拌60min,得糊状物;
(5)先用蒸馏水洗涤糊状物,然后将糊状物在70℃下微波干燥3h,干燥后研磨成粒径为2.0mm的粉末,再放入马沸炉在温度为400℃下焙烧5h,即得光催化剂。
催化剂的光催化试验:下面将通过市售钒酸铋与本发明各实施例制备的光催化剂对亚甲基蓝的降解率进行对比,测定结果如下表所示:
将各实施例制备的光催化剂和市售钒酸铋光催化剂分别称取1g,放入1L浓度为10mg/L的亚甲基蓝模拟水样,加入石英夹层的反应器中,以500 W 氙灯作为太阳光源,在转速为500r/min下搅拌辐射1h,采用高效液相色谱法测定水样中亚甲基蓝的浓度,计算出光催化剂降解率。
由表可知,本发明各实施例所制备的光催化剂有较高的光催化活性,对亚甲基蓝的降解率均达到92%以上,远远高于目前市售的产品,具有很好的市场前景。
以上内容不能认定本发明具体实施只局限于这些说明,对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思前提下,还可以做出若干简单推演或替换,都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。
Claims (5)
1.一种新型钒酸铋光催化剂的制备方法,其特征在于:包括以下步骤:
(1)按照重量份数称取各原料:硝酸铋40-60份、偏钒酸铵10-15份、聚乙二醇5-10份、赤泥5-10份、氮化硅5-10份、金属卟啉2-4份和壳聚糖5-10份;
(2)将硝酸铋溶解于乙二醇中,得溶液A,将偏钒酸铵溶解于水中,得溶液B;
(3)将溶液A放入超声波发生器中,再将溶液B倒入溶液A中,用氨水调节pH至3-4,在频率为40-60KHz下继续超声30-60min,得混合液;
(4)将混合液、聚乙二醇、赤泥、氮化硅、金属卟啉和壳聚糖加入球磨机,再加入适量水搅拌,得糊状物;
(5)先用蒸馏水洗涤糊状物,然后将糊状物在60-80℃下微波干燥2-3h,干燥后研磨成粉末,再放入马沸炉在温度为400-500℃下焙烧2-4h,即得光催化剂。
2.根据权利要求1所述新型钒酸铋光催化剂的制备方法,其特征在于:所述金属卟啉为铁卟啉或钴卟啉中的一种。
3.根据权利要求1所述新型钒酸铋光催化剂的制备方法,其特征在于:步骤(4)所述搅拌是在转速为300-500r/min下搅拌30-60min。
4.根据权利要求1所述新型钒酸铋光催化剂的制备方法,其特征在于:所述焙烧的升温速率为5-10℃/min。
5.根据权利要求1所述新型钒酸铋光催化剂的制备方法,其特征在于:步骤(5)所述研磨是将物料研磨至粒径为1.0-2.0mm。
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