CN110252278A - 一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法 - Google Patents
一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法 Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 6
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 5
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- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 5
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 5
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 5
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- 239000001393 triammonium citrate Substances 0.000 claims description 5
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- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
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- HQAITFAUVZBHNB-UHFFFAOYSA-N sodium;pentahydrate Chemical compound O.O.O.O.O.[Na] HQAITFAUVZBHNB-UHFFFAOYSA-N 0.000 claims description 2
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims 1
- 239000006193 liquid solution Substances 0.000 claims 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims 1
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- 229910052797 bismuth Inorganic materials 0.000 abstract description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
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- DQUIAMCJEJUUJC-UHFFFAOYSA-N dibismuth;dioxido(oxo)silane Chemical compound [Bi+3].[Bi+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O DQUIAMCJEJUUJC-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂及其制备方法。以硝酸铋为铋源,九水偏硅酸钠、正硅酸乙酯等为硅源,无水乙醇和去离子水为溶剂,以复配有机物为分散剂,制备了均匀的前驱体溶液,以聚苯乙烯球为模板,通过水浴、干燥获得干凝胶,干凝胶经煅烧获得Bi2OSiO3/Bi12SiO20多孔光催化剂。该方法工艺简单、周期短、设备简单、成本低,所得多孔的Bi2OSiO3/Bi12SiO20光催化剂具有良好的光催化性能。
Description
技术领域
本发明属于光催化剂技术领域,特别涉及一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法。
背景技术
硅酸铋体系光催化剂由于其合适的禁带宽度,能够响应可见光,具有一定光催化性能。但单相光催化剂往往不能实现光电荷的快速迁移和分离,限制了光催化活性。同时,采用溶胶-凝胶技术所得硅酸铋粉体材料团聚严重,有效作用面积大大减小,而采用传统的模板技术所得多孔材料易造成材料本身晶相的变化以及晶粒的增大,不利于其光催化性能。
发明内容
为了克服上述现有技术的缺点,本发明的目的在于提供一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,通过调节硅源与铋源的比例调节和控制其组成制备最佳异质结的Bi2O2SiO3/Bi12SiO20粉体,优化其光催化活性,同时利用复配的分散剂,在保证材料晶相及晶粒大小的同时,获得高表面积、高孔隙率和低密度的多孔材料,进一步提高光催化性能并使光催化过程更充分,本发明生产工艺、设备简单、周期短,所得催化剂晶相稳定,结晶度高,具有更高的光催化效率。
为了实现上述目的,本发明采用的技术方案是:
一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,包括如下步骤:
(1)取硝酸铋加入水中,并加入分散剂一搅拌至溶解;
(2)向步骤(1)所得溶液中加入硅源,其中硅离子与硝酸铋的摩尔比为1:(1~10),搅拌均匀;
(3)向步骤(2)搅拌均匀的体系中加入分散剂二搅拌溶解获得Bi2O2SiO3/Bi12SiO20前驱体溶液;
(4)制备聚苯乙烯球并超声在乙醇溶液中备用浓度为0.01~1mol/L;
(5)将所述Bi2O2SiO3/Bi12SiO20前驱体溶液与超声在乙醇溶液中的聚苯乙烯球溶液混合搅拌后转移到水浴锅中水浴得到凝胶,然后再转移到烘箱中烘干得到干凝胶;
(6)将所得干凝胶热处理得到多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂。
所述步骤(1)中,硝酸铋浓度为0.1~0.9mol/L。
所述分散剂一为复配有机物,浓度控制在0.1~0.5mol/L。
所述步骤(2)中,硅源为九水偏硅酸钠、五水偏硅酸钠、正硅酸乙酯或硅酸钠。
所述分散剂二为柠檬酸、六偏磷酸钠、焦磷酸钠、柠檬酸三铵、乙二醇、聚丙烯酸钠等中的一种或者多种,每种分散剂的浓度控制在0.5~3mol/L。
所述聚苯乙烯球采用无皂乳液聚合法制备,步骤如下:在三口烧瓶中加入蒸馏水50~150mL,放在恒温加热磁力搅拌器上搅拌,然后依次加入1~10mL的苯乙烯以及0.1~0.5mL的α-甲基丙烯酸,加热到50~100℃,待温度稳定5~10min后加入0.1~0.5g的过硫酸钾,在此温度下反应5~10h,冷却到室温即可得到聚苯乙烯乳液,将聚苯乙烯乳液在9000~12000的转速下离心,再用1:1~5的水醇混合液洗数次得到洗后的聚苯乙烯球。
所述聚苯乙烯球在乙醇溶液中的浓度为0.01~1mol/L。
所述Bi2O2SiO3/Bi12SiO20前驱体溶液与聚苯乙烯球溶液混合搅拌20~60min后转移到水浴锅中,水浴条件为60~100℃,4~8h;烘干温度为120~180℃。
Bi2O2SiO3/Bi12SiO20溶胶与超声在乙醇溶液中的聚苯乙烯球溶液体积之比为1~10。
所述热处理是:先200~400℃温度下保温2~5h,接着升温至550~700℃温度下保温3~8h。
与现有技术相比,本发明的有益效果是:
本发明提供的多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法中,以柠檬酸、六偏磷酸钠、焦磷酸钠、柠檬酸三铵、乙二醇、聚丙烯酸钠等为分散剂,使铋离子与硅离子与分散剂等形成网络结构,更好地分布于溶液体系中,大大提高其热稳定性,减少偏析现象的产生,从而获得所需晶相。另外,本发明利用复合分散剂及聚苯乙烯球,更好地控制其热解过程,避免其他中间杂相的生成,从而更有效地获得Bi2O2SiO3/Bi12SiO20异质晶相,另外一方面,可有效控制分解燃烧过程使保证晶相的同时,减小晶粒的过分生长,在形成多孔Bi2O2SiO3/Bi12SiO20光催化剂,使其具有高效率的光催化性能。本发明制备周期短、成本低,反应条件温和,无二次污染。
附图说明
图1是实施例3制备的多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的SEM图。
图2是实施例3制备的多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的XRD图。
具体实施方式
下面结合附图和实施例详细说明本发明的实施方式。
实施例1
(1)取浓度为0.6mg/mL硝酸铋加入水中,并加入柠檬酸(浓度为0.1mg/mL)搅拌至溶解;
(2)向步骤(1)所得溶液中加入正硅酸乙酯,其中硅离子与硝酸铋的摩尔比为1:1,磁力搅拌30min使其溶解并混合均匀觉得溶液A;
(3)向溶液A中加入柠檬酸、六偏磷酸钠复配有机物分散剂(浓度均为0.1mg/mL),搅拌溶解获得前驱体溶液;
(4)制备聚苯乙烯球并超声分散于乙醇溶液中备用,其浓度为0.01mol/L;
(5)将(3)中所制备的前驱体溶液与超声在乙醇溶液中的聚苯乙烯球悬浮液混合搅拌20min,后转移到水浴锅中水浴得到凝胶(温度为60℃,4h),然后再转移到烘箱中(120℃)烘干得到干凝胶;
(6)将所得干凝胶在200℃温度下先保温2h,接着升温至550℃温度下热处理3h得到多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂。
Bi2O2SiO3/Bi12SiO20复合粉体在可见光照射下,150min对Rh B的降解率为80%,而本实施例所得多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂在可见光照射下,60min对Rh B的降解率可达94%,大大缩短了降解时间。
实施例2
(1)取浓度为0.6mg/mL硝酸铋加入水中,并加入柠檬酸和乙二醇(浓度为0.1mg/mL)搅拌至溶解;
(2)向步骤(1)所得溶液中加入九水偏硅酸钠,其中硅离子与硝酸铋的摩尔比为1:3,磁力搅拌50min使其溶解并混合均匀觉得溶液A;
(3)向溶液A中加入柠檬酸、焦磷酸钠复配有机物分散剂(浓度为0.2mg/mL),搅拌溶解获得前驱体溶液;
(4)制备聚苯乙烯球并超声分散于乙醇溶液中备用,其浓度为0.02mol/L;
(5)将(3)中所制备的前驱体溶液与超声在乙醇溶液中的聚苯乙烯球悬浮液混合搅拌30min,后转移到水浴锅中水浴得到凝胶(温度为70℃,5h),然后再转移到烘箱中(130℃)烘干得到干凝胶;
(6)将所得干凝胶在300℃温度下先保温3h,接着升温至600℃温度下热处理5h得到多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂。
Bi2O2SiO3/Bi12SiO20复合粉体在可见光照射下,150min对Rh B的降解率为80%,而本实施例所得多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂在可见光照射下,60min对Rh B的降解率可达95%,大大缩短了降解时间。
实施例3
(1)取浓度为0.6mg/mL硝酸铋加入水中,并加入柠檬酸(浓度为0.1mg/mL)搅拌至溶解;
(2)向步骤(1)所得溶液中加入正硅酸乙酯,其中硅离子与硝酸铋的摩尔比为1:5,磁力搅拌60min使其溶解并混合均匀觉得溶液A;
(3)向溶液A中加入柠檬酸、柠檬酸三铵复配有机物分散剂(浓度为0.3mg/mL),搅拌溶解获得前驱体溶液;
(4)制备聚苯乙烯球并超声分散于乙醇溶液中备用,其浓度为0.03mol/L;
(5)将(3)中所制备的前驱体溶液与超声在乙醇溶液中的聚苯乙烯球悬浮液混合搅拌50min,后转移到水浴锅中水浴得到凝胶(温度为85℃,6h),然后再转移到烘箱中(150℃)烘干得到干凝胶;
(6)将所得干凝胶在350℃温度下先保温3h,接着升温至600℃温度下热处理5h得到多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂。
Bi2O2SiO3/Bi12SiO20复合粉体在可见光照射下,150min对Rh B的降解率为80%,而本实施例所得多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂在可见光照射下,60min对Rh B的降解率可达97%,大大缩短了降解时间。
从图1可以看出通过本实施例得到了不同形状的多孔结构,增大了光催化剂的比表面积,提升了光催化性能。
从图2可以看出通过本实施例得到了含有Bi2O2SiO3、Bi12SiO20两种晶相的物质。
综上,本发明方法工艺简单、周期短、设备简单、成本低,所得多孔的Bi2OSiO3/Bi12SiO20光催化剂,表现出较高的光催化性能。
Claims (9)
1.一种多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,包括如下步骤:
(1)取硝酸铋加入水中,并加入分散剂一搅拌至溶解;
(2)向步骤(1)所得溶液中加入硅源,其中硅离子与硝酸铋的摩尔比为1:(1~10),搅拌均匀;
(3)向步骤(2)搅拌均匀的体系中加入分散剂二搅拌溶解获得Bi2O2SiO3/Bi12SiO20前驱体溶液;
(4)制备聚苯乙烯球并超声在乙醇溶液中备用;
(5)将所述Bi2O2SiO3/Bi12SiO20前驱体溶液与超声在乙醇溶液中的聚苯乙烯球溶液混合搅拌后转移到水浴锅中水浴得到凝胶,然后再转移到烘箱中烘干得到干凝胶;
(6)将所得干凝胶热处理得到多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂。
2.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述步骤(1)中,硝酸铋浓度为0.1~0.9mol/L。
3.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述分散剂一为柠檬酸、六偏磷酸钠、焦磷酸钠、柠檬酸三铵、乙二醇、聚丙烯酸钠等中的一种或者多种,每种分散剂的浓度控制在0.1~0.5mol/L;所述分散剂二为柠檬酸、六偏磷酸钠、焦磷酸钠、柠檬酸三铵、乙二醇、聚丙烯酸钠等中的一种或者多种,每种分散剂的浓度控制在0.5~3mol/L。
4.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述步骤(2)中,硅源为九水偏硅酸钠、五水偏硅酸钠、正硅酸乙酯或硅酸钠。
5.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述聚苯乙烯球采用无皂乳液聚合法制备,步骤如下:在三口烧瓶中加入蒸馏水50~150mL,放在恒温加热磁力搅拌器上搅拌,然后依次加入1~10mL的苯乙烯以及0.1~0.5mL的α-甲基丙烯酸,加热到50~100℃,待温度稳定5~10min后加入0.1~0.5g的过硫酸钾,在此温度下反应5~10h,冷却到室温即可得到聚苯乙烯乳液,将聚苯乙烯乳液在9000~12000的转速下离心,再用1:1~5的水醇混合液洗数次得到洗后的聚苯乙烯球。
6.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述聚苯乙烯球在乙醇溶液中的浓度为0.01~1mol/L。
7.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述Bi2O2SiO3/Bi12SiO20前驱体溶液与聚苯乙烯球溶液混合搅拌20~60min后转移到水浴锅中,水浴条件为60~100℃,4~8h;烘干温度为120~180℃。
8.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,Bi2O2SiO3/Bi12SiO20溶胶与超声在乙醇溶液中的聚苯乙烯球溶液体积之比为1~10。
9.根据权利要求1所述多孔异质Bi2O2SiO3/Bi12SiO20高效光催化剂的制备方法,其特征在于,所述热处理是:先200~400℃温度下保温2~5h,接着升温至550~700℃温度下保温3~8h。
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