CN111957328A - 一种催化剂模块、制备方法及应用 - Google Patents
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Abstract
本发明公开了一种催化剂模块、制备方法及应用,催化剂模块包括多孔载体和复合催化剂,复合催化剂吸附在所述多孔载体上,且所述多孔载体可再生的重复负载所述复合催化剂。多孔载体为碳布,复合催化剂为Co3O4/Ag3PO4复合光催化剂。催化剂模块应用于降解有机污染物。碳布负载Co3O4/Ag3PO4复合光催化剂的制备方法包括清洗碳布、碳布生长氧化钴和复合磷酸银等步骤。该催化剂模块催化效率高,且可在可见光条件下降解有机污染物,且便于回收。制备的氧化钴为树枝状可以很好地与磷酸银缠结在一起防止磷酸银脱落,使得稳定性更好;并且氧化钴与磷酸银复合形成异质结可以有效促进电荷转移,提高光催化活性;载体可以重复回收利用,降低成本。
Description
技术领域
本发明属于催化剂制造领域,具体涉及一种碳布负载Co3O4/Ag3PO4复合光催化剂、其制备方法和应用。
背景技术
随着科技与工业的极速发展,环境污染越来越严重并且已经成为迫切解决的严重问题之一,特别是工业中的有机染料废水会严重污染地球环境;近几十年来,半导体光催化材料对有机污染物的净化有很好的效果并且引起广泛关注,其中TiO2、ZnO等具有很好的氧化能力、光稳定性强并且成本低。但是TiO2、ZnO等只能被紫外光激发。众所周知,紫外光只占太阳光的3-5%左右,远远低于可见光的比例(大约在45%左右)。因此,迫切需要开发具有较高活性和良好稳定性的可见光响应的光催化剂。
近年来,一系列Ag基光催化剂如Ag2CO3和Ag3PO4等被陆续研发,其在可见光照射下降解有机污染物时表现出来了优异的光催化活性。虽然单一的Ag基光催化剂虽然光催化效果好,但是这些Ag基光催化剂粉末存在难以分离回收并且容易发生光腐蚀、且稳定性不好的缺点,利用光催化剂的固定负载和耦合方法是解决上述问题的有效途径之一。并且负载型Ag基光催化剂更方便回收,复合后的Ag基光催化剂活性更高。
例如,申请号为CN201310462452.7的中国发明专利《一种二硫化钼/磷酸银复合可见光光催化材料及其制备方法》,该制备方法是由质量比为0.1:100~3:100的类石墨烯二硫化钼和磷酸银复合而成,具体是利用类石墨烯二硫化钼对磷酸银光催化剂进行改性处理,而得到一种类石墨烯二硫化钼/磷酸银复合材料。然而。粉末状的催化剂仍然存在回收困难的问题。
又如申请号为CN201810960073.3的中国发明专利《一种纳米片状磷酸银及其制备方法和作为可见光催化剂的应用》,该发明制备方法是将钼酸铵溶液滴加至硝酸银溶液中搅拌均匀,得到混合液;在所述混合液中滴加磷酸氢二钠溶液,搅拌反应,即得纳米片状磷酸银晶体,虽然该方法制备的磷酸银具有较好的可见光光催化活性,但是单一的磷酸银光催化材料容易发生光腐蚀,稳定性不高。
发明内容
为了克服现有技术的不足,本发明的目的在于提供一种催化剂模块、应用及其制备方法,其能解决上述问题。
本发明的目的采用以下技术方案实现:
一种催化剂模块,所述催化剂模块包括多孔载体和复合催化剂,所述复合催化剂吸附在所述多孔载体上,且所述多孔载体可再生的重复负载所述复合催化剂。
优选的,所述多孔载体包括但不限于碳基载体或陶瓷基载体的一种或组合,所述碳基载体包括但不限于碳布、多孔石墨中的一种或组合,所述陶瓷基载体包括但不限于多孔蜂窝状陶瓷载体;所述复合催化剂为Co3O4/Ag3PO4复合光催化剂。
优选的,所述多孔载体具有经化学方法改善的亲水性表面。
优选的,所述Co3O4通过水热法附着在多孔载体上,所述Ag3PO4通过沉淀法附着在所述多孔载体上。
优选的,所述催化剂模块应用于降解有机污染物。
一种碳布负载Co3O4/Ag3PO4复合光催化剂的制备方法,所述制备方法包括以下步骤。
S1碳布表面亲水处理,将碳布先后分别用丙酮、无水乙醇和去离子水中清洗15-25min,然后将碳布浸泡在60-65%的硝酸中15-24h以改善表面亲水性并进行干燥。
S2制取浸泡用混合溶液,将0.1-0.2g的氟化铵、0.5-2g的尿素、1g-1.5g的六水硝酸钴溶解在20mL去离子水和20mL的乙二醇的混合溶液中。
S3碳布水热化处理,将S1中表面亲水处理过的碳布浸泡在S2中的混合溶液中并转移到100mL反应釜中,在100-150℃下水热反应6-12h,自冷后取出清洗干燥。
S4碳布初负载,将水热后的碳布在300-350℃下加热1-3h,得到负载Co3O4的碳布。
S5完成复合负载,将步骤S4中得到的负载了Co3O4的碳布在0.3-0.5mol/L硝酸银溶液中浸泡6-12h,将浸泡过的碳布夹出放到0.15-0.2mol/L磷酸氢二氨溶液当中,浸泡0.5-1min,再将碳布反复浸泡在两种溶液中15-20次,水洗干燥,获得碳布负载Co3O4/Ag3PO4复合光催化材料的催化剂模块。
相比现有技术,本发明的有益效果在于:(1)催化效率高,碳布上生长树枝状自组装氧化钴并且复合磷酸银,有利于促进光生电子-空穴对的分离,提高光催化活性;(2)回收方便,很好的解决了粉末难以分离回收的问题,具有很好的产业化应用前景;(3)稳定性好,制备的氧化钴为树枝状,可以很好的与磷酸银复合,防止磷酸银脱落,使得稳定性更好。
附图说明
图1为本发明的催化剂模块中碳布负载Co3O4/Ag3PO4复合光催化剂的扫描电镜图;
图2为采用本发明催化剂模块在可见光下降解有机污染物的效果对比图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
一种催化剂模块,包括多孔载体和复合催化剂,所述复合催化剂吸附在所述多孔载体上,且所述多孔载体可再生的重复负载所述复合催化剂。
其中,所述多孔载体为碳基载体或陶瓷基载体,所述碳基载体包括但不限于碳布、多孔石墨,所述陶瓷基载体包括但不限于多孔陶瓷。优选的,所述多孔载体的BET比表面积大于等于80m2/g。
进一步的,所述多孔载体具有经化学方法改善的亲水性表面,即经过化学处理后提高其表面的亲水性,以便于后续的催化剂吸附。
其中,所述复合催化剂为Co3O4/Ag3PO4复合光催化剂。进一步的,所述复合催化剂分步的先后附着在多孔载体的表面上。优选的,所述Co3O4通过水热法优先附着在多孔载体上,再将所述Ag3PO4通过沉淀法附着在所述多孔载体上。
其中,氧化钴Co3O4为树枝状的生长在多孔载体上,且与后续附着的磷酸银Ag3PO4缠结在一起防止磷酸银脱落,使得稳定性更好。
一种碳布负载Co3O4/Ag3PO4复合光催化剂的制备方法,所述制备方法包括以下步骤。
S1碳布表面亲水处理,将碳布分别用20mL丙酮、20mL无水乙醇和20mL去离子水清洗20min并放在60℃的干燥箱中干燥2h,并称取重量,然后将清洗后的碳布浸泡在20mL的硝酸(浓度为65%)中24h以改善表面亲水性并在60℃的干燥箱中干燥2h。以此完成碳布清洗的预处理。
S2制取浸泡用混合溶液,将0.1445g的氟化铵和0.9009g的尿素和1.0592g六水硝酸钴溶解在20mL去离子水和20mL乙二醇中并搅拌30min,配成混合液。
S3碳布水热化处理,将S1中处理过的碳布浸泡在S2中的混合溶液中并转移到100mL反应釜中在120℃下水热反应8h,取出碳布后用乙醇和去离子水清洗并干燥,制得负载Co2(CO3)(OH)2的碳布。
S4碳布初负载,将步骤S3中水热后的碳布放进通入氩气的马弗炉中在350℃下加热2h,碳布上生长氧化钴,制得负载CO3O4的碳布,并称取重量。
通过该步骤S4,将碳布上负载的Co2(CO3)(OH)2在煅烧后转变成了Co3O4。
综上,通过步骤S2-S4完成碳布上的氧化钴生长。
S5完成复合负载,将步骤S4中得到的碳布在30mL的0.5mol/L硝酸银溶液中浸泡6h,再将浸泡过的碳布夹出放到30mL的0.17mol/L磷酸氢二氨溶液当中,浸泡1min,再将碳布反复浸泡在以上两种溶液中20次,并用水清洗并干燥2h,制得碳布负载Co3O4/Ag3PO4复合光催化材料的催化剂模块。以此完成复合磷酸银。参见图1,为采用上述方法获得的碳布负载Co3O4/Ag3PO4的复合光催化剂的扫描电镜图,可见在碳布上生长了枝状Co3O4并复合了Ag3PO4颗粒。
采用上述催化剂模块,尤其是碳布负载Co3O4/Ag3PO4的复合光催化剂模块,其被应用于降解有机污染物,且在可见光下即可完成降解处理。参见图2,分别采用纯碳布、碳布负载Ag3PO4和碳布负载Co3O4/Ag3PO4催化剂模块在可见光下降解罗丹明B,从图中可以看出,在50min后碳布负载Co3O4/Ag3PO4对罗丹明B的降解率达到了94.7%,而在同样的时间内单纯用碳布负载/Ag3PO4对罗丹明B降解率仅为43%。
该催化剂性能稳定,这主要归因于碳布可以提高材料的导电性和稳定性。Co3O4/Ag3PO4优化了材料的电子结构,该催化剂可见光下催化活性高,在有机污物降解处理领域具有广泛的应用前景。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (7)
1.一种催化剂模块,其特征在于:所述催化剂模块包括多孔载体和复合催化剂,所述复合催化剂吸附在所述多孔载体上,且所述多孔载体可再生的重复负载所述复合催化剂。
2.根据权利要求1所述的催化剂模块,其特征在于:所述多孔载体包括但不限于碳基载体或陶瓷基载体的一种或组合,所述碳基载体包括但不限于碳布、多孔石墨中的一种或组合,所述陶瓷基载体包括但不限于多孔蜂窝状陶瓷载体;所述复合催化剂为Co3O4/Ag3PO4复合光催化剂。
3.根据权利要求1或2所述的催化剂模块,其特征在于:所述多孔载体具有经化学方法改善的亲水性表面。
4.根据权利要求1或2所述的催化剂模块,其特征在于:所述复合催化剂分步的先后附着在多孔载体的表面上。
5.根据权利要求2所述的催化剂模块,其特征在于:所述Co3O4通过水热法附着在多孔载体上,所述Ag3PO4通过沉淀法附着在所述多孔载体上。
6.根据权利要求2所述的催化剂模块,其特征在于:所述催化剂模块应用于降解有机污染物。
7.一种碳布负载Co3O4/Ag3PO4复合光催化剂的制备方法,其特征在于,所述制备方法包括以下步骤:
S1碳布表面亲水处理,将碳布分别用丙酮、无水乙醇和去离子水清洗15-25min,然后将碳布浸泡在60-65%的硝酸中15-24h以改善表面亲水性并进行干燥;
S2制取浸泡用混合溶液,将0.1-0.2g的氟化铵、0.5-2g的尿素、1g-1.5g的六水硝酸钴溶解在20mL去离子水和20mL的乙二醇的混合溶液中;
S3碳布水热化处理,将S1中表面亲水处理过的碳布浸泡在S2中的混合溶液中并转移到100mL反应釜中,在100-150℃下水热反应6-12h,自冷后取出清洗干燥;
S4碳布初负载,将水热后的碳布在300-350℃下加热1-3h,得到负载Co3O4的碳布;
S5完成复合负载,将步骤S4中得到的负载了Co3O4的碳布在0.3-0.5mol/L硝酸银溶液中浸泡6-12h,将浸泡过的碳布夹出放到0.15-0.2mol/L磷酸氢二氨溶液当中,浸泡0.5-1min,再将碳布反复浸泡在两种溶液中15-20次,水洗干燥,获得碳布负载Co3O4/Ag3PO4复合光催化材料的催化剂模块。
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