CN106179315A - 一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法 - Google Patents
一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法 Download PDFInfo
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Abstract
本发明属于一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,包括以下步骤:①85~100℃下将石墨烯加入到浓硫酸与浓硝酸的混酸中,洗涤,干燥,得改性石墨烯;②将硝酸铋溶于无水乙醇中,得到硝酸铋的乙醇溶液,将步骤①制备的改性石墨烯加入到浓度为0.3~1mol/L的硝酸铋的乙醇溶液中,超声分散0.5~1h,得A液;③将NaOH溶于70~75%乙醇中,得到B液;④搅拌条件下将B液滴入A液中,得到C液;⑤向C液中加入CTAB和丝氨酸,搅拌均匀后转移至反应釜中,180~200℃下水热反应2~4h,过滤、洗涤、干燥后即得石墨烯负载的具有四十八面体形貌的Bi光催化剂。
Description
技术领域
本发明属于有机物污染物降解技术领域,具体涉及一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法。
背景技术
以光催化降解的方法处理工业废水、废气中的有机物,近年来引起人们重视,通过对结构和形貌控制以及掺杂等可改进催化剂的光催化性能,在光催化降解有机污染物的研究中,金属分散度和催化剂在染料溶液中的分散状况都是影响其光降解染料分子催化活性的关键因素。纳米光催化材料比一般光催化材料在促进光催化反应的活性作用上主要体现在两个方面:其一从上述光催化机理来看,氧化、还原作用的强弱取决于光生电子和空穴的浓度。显然光催化剂颗粒尺寸越小,总表面积越大,光吸收效率越高,并且电子和空穴移动到表面的几率也越大。粉末石墨烯因其比表面积大,逐渐成为研究的焦点,使得光催化技术在水处理领域的应用成为可能。20世纪70年代以来,利用金属光催化剂氧化水中污染物的工作日益为人们所重视,其优点主要在于:首先,利用金属光催化剂氧化降解水中污染物不同于单纯的物理方法、化学方法和生物方法的水处理,处理流程简单,无二次污染,处理速度比微生物法快;其次,金属光催化剂氧化可以处理各种无机和有机污染物使其矿化,是一种氧化处理方法,最关键的是光催化氧化过程有可能利用太阳光资源,节能且无污染。
发明内容
本发明的目的是提供一种对罗丹明B的降解率高、降解时间短的石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法。
为实现上述目的,本发明采用的技术方案是,一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,包括以下步骤:①85~100℃下将石墨烯加入到浓硫酸与浓硝酸的混酸中,石墨烯与混酸的重量比0.5~2︰1,2~8小时后过滤,洗涤,干燥,得改性石墨烯;②将硝酸铋溶于无水乙醇中,得到浓度为0.3~1mol/L的硝酸铋的乙醇溶液,将步骤①制备的改性石墨烯按固液比1g︰20ml~1g︰30ml加入到浓度为0.3~1mol/L的硝酸铋的乙醇溶液中,超声分散0.5~1h,得A液;③将NaOH溶于70~75%乙醇中,得到B液,B液中NaOH的浓度为1.5~2mol/L;④搅拌条件下将B液滴入A液中,得到C液,其中,B液中NaOH与A液中硝酸铋的摩尔比为1~1.05︰1;⑤向C液中加入CTAB(十六烷基三甲基溴化铵)和丝氨酸,搅拌均匀后转移至反应釜中,180~200℃下水热反应2~4h,过滤、洗涤、干燥后即得石墨烯负载的具有四十八面体形貌的Bi 光催化剂。
优选的,所述步骤⑤中CTAB与丝氨酸的质量比为1~1.5︰1,CTAB与C液的固液比为8~10g︰1L。
所述步骤①中浓硫酸与浓硝酸的体积比为2~4︰1,浓硫酸的浓度为98wt%,浓硝酸的浓度为69wt%。
本发明产生的有益效果是:本发明通过Bi 催化剂负载在石墨烯上,避免了普通的Bi光催化剂尺寸较大、分散性较差、容易团聚缺点;通过加入CTAB和丝氨酸,结合水热反应条件,制备出了选择性较高的石墨烯负载的四十八面体形貌的Bi光催化剂,该光催化剂在紫外光源下对罗丹明B的降解率显示出很好的催化活性,具有广泛的应用前景。
附图说明
图1为实施例1制备的石墨烯负载的具有四十八面体形貌的Bi光催化剂的透射电镜照片;
图2为实施例1制备的石墨烯负载的具有四十八面体形貌的Bi光催化剂的XRD图;
图3为实施例1制备的石墨烯负载的具有四十八面体形貌的Bi 光催化剂对罗丹明B的降解效果图;
图4为对照实验1制备的石墨烯负载的Bi 光催化剂的透射电镜照片。
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,但本发明的保护范围不限于此。
实施例1
一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,包括以下步骤:①90℃下将石墨烯加入到浓硫酸与浓硝酸的混酸(浓硫酸与浓硝酸的体积比为3︰1,浓硫酸的浓度为98wt%,浓硝酸的浓度为69wt%)中,石墨烯与混酸的重量比1︰1,6小时后过滤,洗涤,干燥,得改性石墨烯;②将硝酸铋溶于无水乙醇中,得到浓度为0.6mol/L的硝酸铋的乙醇溶液,将步骤①制备的改性石墨烯按固液比1g︰25ml加入到浓度为0.6mol/L的硝酸铋的乙醇溶液中,超声分散0.5h,得A液;③将NaOH溶于75%乙醇中,得到B液,B液中NaOH的浓度为1.5mol/L;④搅拌条件下将B液滴入A液中,得到C液,其中,B液中NaOH与A液中硝酸铋的摩尔比为3︰1;⑤向C液中加入CTAB(十六烷基三甲基溴化铵)和丝氨酸,搅拌均匀后转移至反应釜中,180℃下水热反应2h,过滤、洗涤、干燥后即得石墨烯负载的具有四十八面体形貌的Bi光催化剂。所述步骤⑤中CTAB与丝氨酸的质量比为1︰1,CTAB与C液的固液比为10g︰1L。
实施例1制备的石墨烯负载的具有四十八面体形貌的Bi光催化剂的透射电镜(TEM)照片如图1所示,由图1可以看出,制备出的石墨烯负载的Bi光催化剂为规则的四十八面体,形貌选择性较好。
对照例1
对照例1与实施例1的不同之处在于,步骤⑤中不加入CTAB和丝氨酸,将C液直接转入反应釜中,180℃下水热反应2h,过滤、洗涤、干燥。
对照例1制备的石墨烯负载的Bi光催化剂如图4所示,从图4可以看出,制备出的光催化剂形貌为不规则形状。
实施例2
一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,包括以下步骤:①100℃下将石墨烯加入到浓硫酸与浓硝酸的混酸(浓硫酸与浓硝酸的体积比为4︰1,浓硫酸的浓度为98wt%,浓硝酸的浓度为69wt%)中,石墨烯与混酸的重量比0.5︰1,2小时后过滤,洗涤,干燥,得改性石墨烯;②将硝酸铋溶于无水乙醇中,得到浓度为0.3mol/L的硝酸铋的乙醇溶液,将步骤①制备的改性石墨烯按固液比1g︰20ml加入到浓度为0.3mol/L的硝酸铋的乙醇溶液中,超声分散1h,得A液;③将NaOH溶于70%乙醇中,得到B液,B液中NaOH的浓度为2mol/L;④搅拌条件下将B液滴入A液中,得到C液,其中,B液中NaOH与A液中硝酸铋的摩尔比为3.05︰1;⑤向C液中加入CTAB(十六烷基三甲基溴化铵)和丝氨酸,搅拌均匀后转移至反应釜中, 200℃下水热反应2h,过滤、洗涤、干燥后即得石墨烯负载的具有四十八面体形貌的Bi 光催化剂。所述步骤⑤中CTAB与丝氨酸的质量比为1.5︰1,CTAB与C液的固液比为8g︰1L。
实施例3
一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,包括以下步骤:①85℃下将石墨烯加入到浓硫酸与浓硝酸的混酸(浓硫酸与浓硝酸的体积比为2︰1,浓硫酸的浓度为98wt%,浓硝酸的浓度为69wt%)中,石墨烯与混酸的重量比2︰1,8小时后过滤,洗涤,干燥,得改性石墨烯;②将硝酸铋溶于无水乙醇中,得到浓度为1mol/L的硝酸铋的乙醇溶液,将步骤①制备的改性石墨烯按固液比1g︰30ml加入到浓度为1mol/L的硝酸铋的乙醇溶液中,超声分散0.5h,得A液;③将NaOH溶于75%乙醇中,得到B液,B液中NaOH的浓度为1.5mol/L;④搅拌条件下将B液滴入A液中,得到C液,其中,B液中NaOH与A液中硝酸铋的摩尔比为3.03︰1;⑤向C液中加入CTAB(十六烷基三甲基溴化铵)和丝氨酸,搅拌均匀后转移至反应釜中,180℃下水热反应4h,过滤、洗涤、干燥后即得石墨烯负载的具有四十八面体形貌的Bi 光催化剂。所述步骤⑤中CTAB与丝氨酸的质量比为1~1.2︰1,CTAB与C液的固液比为9g︰1L。
降解试验
实施例1制备的石墨烯负载的具有四十八面体形貌的Bi光催化剂在紫外光源照射下对罗丹明B的降解实验步骤如下:将浓度为10mg/L的罗丹明B溶液100mL加入光催化仪器反应管内,然后加入经水热反应制备的Bi光催化剂0.02g,超声分散4min,在暗室中静态吸附30min后达到反应吸附平衡,开启紫外光源及磁力搅拌装置,光照过程中每间隔20min取样,离心分离后取上层清液在罗丹明B最大吸收波长l=554nm处,使用722N可见分光光度计测定样品吸光度,并通过公式:DC=[(A0-Ai)/A0]´100%完成降解率的计算,其中为A0为10mg/L的罗丹明B溶液的吸光度,Ai为定时取样时测定的罗丹明B溶液的吸光度。在254nm波长紫外光下照射2小时,罗丹明B的降解率为97.1%。
Claims (3)
1.一种石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,其特征在于包括以下步骤:①85~100℃下将石墨烯加入到浓硫酸与浓硝酸的混酸中,石墨烯与混酸的重量比0.5~2︰1,2~8小时后过滤,洗涤,干燥,得改性石墨烯;②将硝酸铋溶于无水乙醇中,得到浓度为0.3~1mol/L的硝酸铋的乙醇溶液,将步骤①制备的改性石墨烯按固液比1g︰20ml~1g︰30ml加入到浓度为0.3~1mol/L的硝酸铋的乙醇溶液中,超声分散0.5~1h,得A液;③将NaOH溶于70~75%乙醇中,得到B液,B液中NaOH的浓度为1.5~2mol/L;④搅拌条件下将B液滴入A液中,得到C液,其中,B液中NaOH与A液中硝酸铋的摩尔比为3~3.2︰1;⑤向C液中加入CTAB和丝氨酸,搅拌均匀后转移至反应釜中,180~200℃下水热反应2~4h,过滤、洗涤、干燥后即得石墨烯负载的具有四十八面体形貌的Bi 光催化剂。
2.如权利要求2所述石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,其特征在于,所述步骤⑤中CTAB与丝氨酸的质量比为1~1.5︰1,CTAB与C液的固液比为8~10g︰1L。
3.如权利要求1所述石墨烯负载的具有四十八面体形貌的Bi光催化剂的制备方法,其特征在于,所述步骤①中浓硫酸与浓硝酸的体积比为2~4︰1。
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