CN112691683A - 一种具有可见光催化净化室内空气和灭菌的材料制备方法 - Google Patents
一种具有可见光催化净化室内空气和灭菌的材料制备方法 Download PDFInfo
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Abstract
本发明涉及可见光催化氧化催化剂制备领域,具体为一种具有可见光催化净化室内空气和灭菌的材料制备方法,所述材料为Ag+/Cu‑BiVO4负载在海泡石构成的复合材料,该复合硅酸盐对室内空气污染物具有良好的净化效果,其中甲醛的净化效率在90%以上,甲苯的净化效率在95%以上,复合硅酸盐室内净化材料具有优秀除菌性能,在与大肠杆菌作用24h后,细菌大部分已被溶解,失去活性,该材料的特点是可见光利用率较高,无需消耗能源,节省了生产和使用成本;光催化净化效率高、无二次污染、作用持久等优点。
Description
技术领域
本发明涉及可见光催化氧化催化剂制备领域,具体为一种具有可见光催化净化室内空气和灭菌的材料制备方法。
背景技术
室内空气环境作为建筑环境中重要组成部分,越来越引起人们对它的重视,由于合成建筑装饰材料和室内空调、电脑等产品的大量使用以及室内人员生产生活等影响,导致大量有毒有害物质和细菌的散发,严重降低了室内空气品质,建筑物内空气中有毒有害物质与细菌、病毒的存在,严重的威胁着人体的生命健康安全,21世纪的我们正进入以“室内空气污染”为标志的第三污染时期,室内空气污染物对人体健康的影响与其成分有关,室内污染物主要由挥发性有机物(VOCs),可吸入颗粒物,细菌、病毒等成分组成,近年来的研究表明室内空气负离子浓度的高低也是影响人体健康的重要因素之一,室内空气净化材料按照净化机理的不同可分为生物型、化学型、物理型、和复合型净化材料,各种净化材料都是利用自身的性质发生物理或化学反应从而达到净化空气的作用,室内空气净化材料具有诸多优点,例如节能环保、净化效果好、装饰美观、二次污染少等,由于空气净化材料的多重优势,使其广泛应用于环保、建材等领域,空气净化材料虽然种类比较多,但是每种材料都有其特定的优势与特点的同时也存在一些不足,这些不足导致无法满足实际的应用需要,在开发利用中存在各种问题,例如功能单一,重复利用性差,净化效率不高等缺点,为克服这些缺点,人们将研究重点从单一空气净化材料转变为复合空气净化材料的研究,其中以硅酸盐材料为基础,多种材料复合制备出新型复合硅酸盐室内空气净化材料已成为研究的热点,目前国内外对室内空气净化材料的研究主要还是集中在活性炭、TiO2等传统净化材料,但活性炭存在着净化效率低,易产生二次污染等问题,TiO2由于其禁带宽度比较宽(3.2eV),可见光响应范围比较窄,导致其量子效率低,影响其光催化反应效率,均不能全面满足人们对净化空气的要求,由于室内空气污染物成分复杂,单纯的依靠一种净化材料,一种净化技术对室内污染物进行处理,处理效果难以让人满意,所以以多种材料进行复合,不同净化技术进行联合的复合净化材料有着非常好的发展前景,其中以非金属矿物为基体复合新型光催化剂的复合室内空气净化材料,被认为是最理想的治理室内空气污染的技术与材料。
发明内容
本发明的目的在于提供一种具有可见光催化净化室内空气和灭菌的材料制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,一种具有可见光催化净化室内空气和灭菌的材料制备方法,所述复合硅酸盐为Ag+/Cu-BiVO4复合海泡石材料,以海泡石、硝酸铋(Bi(NO3)3·5H2O)、偏钒酸铵(NH4VO3)、硝酸铜(Cu(NO3)2)、硝酸银(AgNO3)为原材料,具体流程分为(1)、(2)和(3)。
优选的:所述海泡石改性(1)具体为,将海泡石加入含有20%过氧化氢的蒸馏水中,用磁力搅拌器中速搅拌1h,静置2h,除去上层清液和下层悬浊物,取中层均匀分散物进行抽滤,重复实验操作3次,对海泡石的提纯过程;将初提纯的海泡石放入1mol/L盐酸溶液中,固液比1∶10混合,将混合液放入80℃恒温水浴锅中,用恒温磁力搅拌器低速搅拌4h,然后静置2h,用去离子水抽滤洗涤多次,直至混合液pH值呈中性,在鼓风干燥箱中80℃烘干,对海泡石的酸活化过程;将海泡石在250℃环境下焙烧2h,即为海泡石热活化过程。
优选的:所述海泡石改性(2)具体为,按摩尔比1∶1称取一定量Bi(NO3)3·5H2O和NH4VO3,将Bi(NO3)3·5H2O溶于一定体积浓度为2mol/L的浓硝酸溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到A溶液;将NH4VO3溶于一定体积浓度为2mol/L的NaOH溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到B溶液,将B溶液逐滴加入A溶液中,缓慢加入的同时并用磁力搅拌器搅拌,加入一定量的DMF,再搅拌30min,用NaOH溶液调节混合液的pH至中性,将制得的混合液倒入高压反应釜中,在恒温箱内180℃加热20h,自然冷却后,经过离心分离,蒸馏水多次洗涤、过滤,在80℃干燥2h,制得m型BiVO4晶体粉末,按Cu2+占BiVO4质量的5%为标准,分别称取一定量单斜型BiVO4晶体粉末与Cu(NO3)2·3H2O晶体,采用浸渍法制备Cu-BiVO4复合体,用蒸馏水将BiVO4和Cu(NO3)2·3H2O混合,放至水浴锅中加热搅拌,搅拌至液体蒸干,将蒸干的混合物放在马弗炉中,在300℃的环境温度下焙烧4h,即制得Cu-BiVO4复合体。
优选的:所述材料浸渍复合(3)具体为,在室温条件下,取一定量酸热活化后的海泡石材料,溶于AgNO3浓度为3400mg/L的溶液中(海泡石吸附Ag+质量为16.03mg/g),然后再掺杂占海泡石质量分数25%Cu-BiVO4晶体,用磁力搅拌器搅拌1h,得到混合液,将混合液转入高压反应釜中,放入恒温箱中加热180℃反应2h,自然冷却后,使用超声波振荡器在蒸馏水中振荡30min,再用蒸馏水反复洗涤,然后进行真空抽滤,抽滤后放入电热鼓风干燥箱中,在80℃下烘干2h,即得Ag+/Cu-BiVO4/复合海泡石材料与现有技术相比,
本发明的有益效果是:
该方法制作简单,针对室内空气净化效率高,作用持久,可见光利用率高,节能环保,不产生二次污染。可同时处理多种有害气体,包括氨气、氮化物、硫化物以及VOCs,如甲醛和甲苯等。对海泡石进行酸热活化改性,可使海泡石孔容、孔洞增加,比表面积增大,吸附性能明显提高。采用水热合成法来制备m型BiVO4晶体,该工艺方便可行,制得的BiVO4晶体具有结晶度高、分散性好等优点,以Cu(NO3)2·3H2O晶体为材料,采用浸渍法对BiVO4进行改性,操作方法简单,可进一步提高BiVO4晶体的催化性能。将改性海泡石、改性钒酸铋以及硝酸银复合而成的材料不仅可以光催化净化有害气体,还可以对室内空气进行灭菌并释放对人体有益的负氧离子;该复合硅酸盐净化材料在可见光照射下就可以产生氧化性极强的羟基自由基,无需通电,节省能源。
附图说明
图1为本发明的流程图。
图中:1、海泡石改性;2、钒酸铋改性;3、材料浸渍复合。
具体实施方式
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,所描述的实施例仅仅是本发明一部分实施例,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。
请参阅图1结合实施例对本发明的技术特征作进一步的说明:
实施例1:
一种新型可见光催化净化室内空气复合硅酸盐材料制备方法,所述复合硅酸盐为Ag+/Cu-BiVO4复合海泡石材料,以海泡石、Bi(NO3)3·5H2O、NH4VO3、Cu(NO3)2、AgNO3为原材料,将海泡石以酸活化和热活化的方法进行改性,采用水热合成法制出BiVO4并进行改性,将改性海泡石、改性BiVO4与AgNO3三种材料按照一定的质量比进行浸渍复合,具体方法如下:
1)海泡石改性方法
将海泡石加入含有20%过氧化氢的蒸馏水中,用磁力搅拌器中速搅拌1h,静置2h,除去上层清液和下层悬浊物,取中层均匀分散物进行抽滤,重复实验操作3次,对海泡石的提纯过程;
将初提纯的海泡石放入1mol/L盐酸溶液中,固液比1∶10混合,将混合液放入80℃恒温水浴锅中,用恒温磁力搅拌器低速搅拌4h,然后静置2h,用去离子水抽滤洗涤多次,直至混合液pH值呈中性,在鼓风干燥箱中80℃烘干,对海泡石的酸活化过程;
将海泡石在250℃环境下焙烧2h,即为海泡石热活化过程。
2)钒酸铋改性方法
按摩尔比1∶1称取一定量Bi(NO3)3·5H2O和NH4VO3,将Bi(NO3)3·5H2O溶于一定体积浓度为2mol/L的浓硝酸溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到A溶液;将NH4VO3溶于一定体积浓度为2mol/L的NaOH溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到B溶液。将B溶液逐滴加入A溶液中,缓慢加入的同时并用磁力搅拌器搅拌,加入一定量的DMF,再搅拌30min,用NaOH溶液调节混合液的pH至中性,将制得的混合液倒入高压反应釜中,在恒温箱内180℃加热20h,自然冷却后,经过离心分离,蒸馏水多次洗涤、过滤,在80℃干燥2h,制得m型BiVO4晶体粉末。
按Cu2+占BiVO4质量的2%为标准,分别称取一定量单斜型BiVO4晶体粉末与Cu(NO3)2·3H2O晶体,采用浸渍法制备Cu-BiVO4复合体,用蒸馏水将BiVO4和Cu(NO3)2·3H2O混合,放至水浴锅中加热搅拌,搅拌至液体蒸干,将蒸干的混合物放在马弗炉中,在300℃的环境温度下焙烧4h,即制得Cu-BiVO4复合体。
3)改性海泡石、改性BiVO4与AgNO3三种材料浸渍复合方法
在室温条件下,取一定量酸热活化后的海泡石材料,溶于AgNO3浓度为3400mg/L的溶液中(海泡石吸附Ag+质量为16.03mg/g),然后再掺杂占海泡石质量分数15%Cu-BiVO4晶体,用磁力搅拌器搅拌1h,得到混合液。将混合液转入高压反应釜中,放入恒温箱中加热180℃反应2h,自然冷却后,使用超声波振荡器在蒸馏水中振荡30min,再用蒸馏水反复洗涤,然后进行真空抽滤,抽滤后放入电热鼓风干燥箱中,在80℃下烘干2h,即得Ag+/Cu-BiVO4/复合海泡石材料。
该催化剂在甲苯初始浓度为2mg/m3,停留时间为4h,空气流速为0.2m/s的条件下,对室内空气污染物甲苯的净化效率为87.7%。
实施例2:
一种新型可见光催化净化室内空气复合硅酸盐材料制备方法,所述复合硅酸盐为Ag+/Cu-BiVO4复合海泡石材料,以海泡石、Bi(NO3)3·5H2O、NH4VO3、Cu(NO3)2、AgNO3为原材料,将海泡石以酸活化和热活化的方法进行改性,采用水热合成法制出钒酸铋(BiVO4)并进行改性,将改性海泡石、改性BiVO4与AgNO3三种材料按照一定的质量比进行浸渍复合。具体方法如下:
1)海泡石改性方法
将海泡石加入含有20%过氧化氢的蒸馏水中,用磁力搅拌器中速搅拌1h,静置2h,除去上层清液和下层悬浊物,取中层均匀分散物进行抽滤,重复实验操作3次,对海泡石的提纯过程;
将初提纯的海泡石放入1mol/L盐酸溶液中,固液比1∶10混合,将混合液放入80℃恒温水浴锅中,用恒温磁力搅拌器低速搅拌4h,然后静置2h,用去离子水抽滤洗涤多次,直至混合液pH值呈中性,在鼓风干燥箱中80℃烘干,对海泡石的酸活化过程;
将海泡石在250℃环境下焙烧2h,即为海泡石热活化过程。
2)钒酸铋改性方法
按摩尔比1∶1称取一定量Bi(NO3)3·5H2O和NH4VO3,将Bi(NO3)3·5H2O溶于一定体积浓度为2mol/L的浓硝酸溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到A溶液;将NH4VO3溶于一定体积浓度为2mol/L的NaOH溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到B溶液。将B溶液逐滴加入A溶液中,缓慢加入的同时并用磁力搅拌器搅拌,加入一定量的DMF,再搅拌30min,用NaOH溶液调节混合液的pH至中性,将制得的混合液倒入高压反应釜中,在恒温箱内180℃加热20h,自然冷却后,经过离心分离,蒸馏水多次洗涤、过滤,在80℃干燥2h,制得m型BiVO4晶体粉末。
按Cu2+占BiVO4质量的5%为标准,分别称取一定量单斜型BiVO4晶体粉末与Cu(NO3)2·3H2O晶体,采用浸渍法制备Cu-BiVO4复合体,用蒸馏水将BiVO4和Cu(NO3)2·3H2O混合,放至水浴锅中加热搅拌,搅拌至液体蒸干,将蒸干的混合物放在马弗炉中,在300℃的环境温度下焙烧4h,即制得Cu-BiVO4复合体。
3)改性海泡石、改性BiVO4与AgNO3三种材料浸渍复合方法
在室温条件下,取一定量酸热活化后的海泡石材料,溶于AgNO3浓度为3400mg/L的溶液中(海泡石吸附Ag+质量为16.03mg/g),然后再掺杂占海泡石质量分数25%Cu-BiVO4晶体,用磁力搅拌器搅拌1h,得到混合液。将混合液转入高压反应釜中,放入恒温箱中加热180℃反应2h,自然冷却后,使用超声波振荡器在蒸馏水中振荡30min,再用蒸馏水反复洗涤,然后进行真空抽滤,抽滤后放入电热鼓风干燥箱中,在80℃下烘干2h,即得Ag+/Cu-BiVO4/复合海泡石材料。
该催化剂在甲苯初始浓度为2mg/m3,停留时间为4h,空气流速为0.2m/s的条件下,对室内空气污染物甲醛的净化效率为96.8%。
实施例3:
一种新型可见光催化净化室内空气复合硅酸盐材料制备方法,所述复合硅酸盐为Ag+/Cu-BiVO4复合海泡石材料,以海泡石、Bi(NO3)3·5H2O、NH4VO3、Cu(NO3)2、AgNO3为原材料,将海泡石以酸活化和热活化的方法进行改性,采用水热合成法制出钒酸铋(BiVO4)并进行改性,将改性海泡石、改性BiVO4与AgNO3三种材料按照一定的质量比进行浸渍复合。具体方法如下:
1)海泡石改性方法
将海泡石加入含有20%过氧化氢的蒸馏水中,用磁力搅拌器中速搅拌1h,静置2h,除去上层清液和下层悬浊物,取中层均匀分散物进行抽滤,重复实验操作3次,对海泡石的提纯过程;
将初提纯的海泡石放入1mol/L盐酸溶液中,固液比1∶10混合,将混合液放入80℃恒温水浴锅中,用恒温磁力搅拌器低速搅拌4h,然后静置2h,用去离子水抽滤洗涤多次,直至混合液pH值呈中性,在鼓风干燥箱中80℃烘干,对海泡石的酸活化过程;
将海泡石在250℃环境下焙烧2h,即为海泡石热活化过程。
2)钒酸铋改性方法
按摩尔比1∶1称取一定量Bi(NO3)3·5H2O和NH4VO3,将Bi(NO3)3·5H2O溶于一定体积浓度为2mol/L的浓硝酸溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到A溶液;将NH4VO3溶于一定体积浓度为2mol/L的NaOH溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到B溶液。将B溶液逐滴加入A溶液中,缓慢加入的同时并用磁力搅拌器搅拌,加入一定量的DMF,再搅拌30min,用NaOH溶液调节混合液的pH至中性,将制得的混合液倒入高压反应釜中,在恒温箱内180℃加热20h,自然冷却后,经过离心分离,蒸馏水多次洗涤、过滤,在80℃干燥2h,制得m型BiVO4晶体粉末。
按Cu2+占BiVO4质量的7%为标准,分别称取一定量单斜型BiVO4晶体粉末与Cu(NO3)2·3H2O晶体,采用浸渍法制备Cu-BiVO4复合体,用蒸馏水将BiVO4和Cu(NO3)2·3H2O混合,放至水浴锅中加热搅拌,搅拌至液体蒸干,将蒸干的混合物放在马弗炉中,在300℃的环境温度下焙烧4h,即制得Cu-BiVO4复合体。
3)改性海泡石、改性BiVO4与AgNO3三种材料浸渍复合方法
在室温条件下,取一定量酸热活化后的海泡石材料,溶于AgNO3浓度为3400mg/L的溶液中(海泡石吸附Ag+质量为16.03mg/g),然后再掺杂占海泡石质量分数35%Cu-BiVO4晶体,用磁力搅拌器搅拌1h,得到混合液。将混合液转入高压反应釜中,放入恒温箱中加热180℃反应2h,自然冷却后,使用超声波振荡器在蒸馏水中振荡30min,再用蒸馏水反复洗涤,然后进行真空抽滤,抽滤后放入电热鼓风干燥箱中,在80℃下烘干2h,即得Ag+/Cu-BiVO4/复合海泡石材料。
其中,该催化剂在甲苯初始浓度为2mg/m3,停留时间为4h,空气流速为0.2m/s的条件下,对室内空气污染物甲醛的净化效率为91.2%。
本方案中的技术分析:Ag+/Cu-BiVO4复合海泡石材料作为催化剂在可见光条件下与室内空气充分接触,可见光照射BiVO4,价带电子受到激发发生跃迁,产生空穴-电子对,未复合的空穴-电子对在BiVO4表面遇到捕获剂或适合的表面缺陷,光生电子(e-)会同氧气发生反应产生超氧负离子(O2-),超氧负离子(O2-)继续与体系中的氧气和水反应最后生成活性氧自由基和羟基自由基(·OH),光生空穴(h+)会直接与水发生反应生成羟基自由基(·OH),羟基自由基(·OH)和超氧负离子(O2-)都具有超强的氧化能力,几乎可以把所有的有机物氧化分解,最终得到二氧化碳和水等小分子物质,其主要反应如下:
BiVO4+hv→h++e
e-+h+→heat energy
e-+O2→O2-
H2O+O2+e-→·OH+OH-
h++H2O→·OH+H+
organic pollutant+·OH→CO2+H2O
将BiVO4进行Ag+和Cu掺杂改性后负载于热活化后的海泡石上,不仅提高了催化剂的杀菌能力,还使催化剂吸附能力增强,可见光利用率增大,进而大大提高了光催化活性和净化效率,Ag+和BiVO4都具有很强的杀菌功能,两者掺杂在一起杀菌能力更强,效果更好,海泡石经活化后,品味得到提高,孔道变大,表面酸性增强,热稳定性提高,作为催化剂载体其吸附性能和催化性能得到很大提高,有利于催化剂充分发挥其催化性能,钒酸铋(BiVO4)作为一种新型可见光型光催化材料,禁带宽度比较窄(2.4eV),但其在可见光下并不能达到对有机污染物预期的催化效率,Cu掺杂改性能进一步提高m型BiVO4晶体的可见光催化性能。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (4)
1.一种具有可见光催化净化室内空气和灭菌的材料制备方法,其特征在于:所述复合硅酸盐为Ag+/Cu-BiVO4复合海泡石材料,以海泡石、硝酸铋(Bi(NO3)3·5H2O)、偏钒酸铵(NH4VO3)、硝酸铜(Cu(NO3)2)、硝酸银(AgNO3)为原材料,具体流程分为(1)、(2)和(3)。
2.根据权利要求1所述的一种运用智能图像打印风景人物的系统,其特征在于:所述海泡石改性(1)具体为,将海泡石加入含有20%过氧化氢的蒸馏水中,用磁力搅拌器中速搅拌1h,静置2h,除去上层清液和下层悬浊物,取中层均匀分散物进行抽滤,重复实验操作3次,对海泡石的提纯过程;将初提纯的海泡石放入1mol/L盐酸溶液中,固液比1∶10混合,将混合液放入80℃恒温水浴锅中,用恒温磁力搅拌器低速搅拌4h,然后静置2h,用去离子水抽滤洗涤多次,直至混合液pH值呈中性,在鼓风干燥箱中80℃烘干,对海泡石的酸活化过程;将海泡石在250℃环境下焙烧2h,即为海泡石热活化过程。
3.根据权利要求1所述的一种运用智能图像打印风景人物的系统,其特征在于:所述(2)具体为,按摩尔比1∶1称取一定量Bi(NO3)3·5H2O和NH4VO3,将Bi(NO3)3·5H2O溶于一定体积浓度为2mol/L的浓硝酸溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到A溶液;将NH4VO3溶于一定体积浓度为2mol/L的NaOH溶液中,在60℃的水浴锅内,用恒温磁力搅拌器搅拌30min,得到B溶液,将B溶液逐滴加入A溶液中,缓慢加入的同时并用磁力搅拌器搅拌,加入一定量的DMF,再搅拌30min,用NaOH溶液调节混合液的pH至中性,将制得的混合液倒入高压反应釜中,在恒温箱内180℃加热20h,自然冷却后,经过离心分离,蒸馏水多次洗涤、过滤,在80℃干燥2h,制得m型BiVO4晶体粉末,按Cu2+占BiVO4质量的5%为标准,分别称取一定量单斜型BiVO4晶体粉末与Cu(NO3)2·3H2O晶体,采用浸渍法制备Cu-BiVO4复合体,用蒸馏水将BiVO4和Cu(NO3)2·3H2O混合,放至水浴锅中加热搅拌,搅拌至液体蒸干,将蒸干的混合物放在马弗炉中,在300℃的环境温度下焙烧4h,即制得Cu-BiVO4复合体。
4.根据权利要求1所述的一种运用智能图像打印风景人物的系统,其特征在于:所述(3)具体为,在室温条件下,取一定量酸热活化后的海泡石材料,溶于AgNO3浓度为3400mg/L的溶液中(海泡石吸附Ag+质量为16.03mg/g),然后再掺杂占海泡石质量分数25%Cu-BiVO4晶体,用磁力搅拌器搅拌1h,得到混合液,将混合液转入高压反应釜中,放入恒温箱中加热180℃反应2h,自然冷却后,使用超声波振荡器在蒸馏水中振荡30min,再用蒸馏水反复洗涤,然后进行真空抽滤,抽滤后放入电热鼓风干燥箱中,在80℃下烘干2h,即得Ag+/Cu-BiVO4/复合海泡石材料。
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