CN106076354B - 一种溶胶凝胶制备钼酸铋共掺杂样品的方法 - Google Patents
一种溶胶凝胶制备钼酸铋共掺杂样品的方法 Download PDFInfo
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- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
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- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
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- 238000003760 magnetic stirring Methods 0.000 claims description 3
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 3
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- 244000248349 Citrus limon Species 0.000 claims 1
- 235000005979 Citrus limon Nutrition 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 21
- 229910002900 Bi2MoO6 Inorganic materials 0.000 abstract description 14
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Abstract
本发明提供了一种溶胶凝胶制备钼酸铋共掺杂样品的方法,属包括以下步骤:取10mmolBi(NO3)3·5H2O溶于50ml稀硝酸中,加入10mmol柠檬酸混合均匀,记为A;取1.45mmol的(NH4)6MO7O24·4H2O溶于50ml蒸馏水中,加入10mmol柠檬酸,搅拌均匀,记为B;将B注入A中,混合均匀至澄清液体时,调节pH值至6.5,然后向溶液中掺杂Eu3+和Fe3+,调节pH至6.5,待变成粘稠的凝胶状后转入坩埚中,然后放入80℃的烘箱中烘干,待变成黑色蜂窝状固体,研磨至粉末状,在450℃下煅烧5h,得到淡黄色粉末。本发明的有益效果为:采用柠檬酸络合溶胶‑凝胶法,首次利用Eu3+和Fe3+共掺杂提高Bi2MoO6活性,通过光催化实验验证表明所得共掺杂钼酸铋催化剂相比单掺杂催化剂的活性有了显著提高,具有更加优越的物化性能。
Description
技术领域
本发明涉及光催化剂制备技术领域,尤其涉及一种溶胶凝胶制备钼酸铋共掺杂样品的方法。
背景技术
近年来,采用新型半导体光催化材料处理工业、农业以及生活污水中的有机污染物已经成为最具发展前景的新兴技术之一。Bi2MoO6的化学通式是Bi2O3·nMoO3,其中n=3,2,1,分别对应α-Bi2Mo3O12、β-Bi2Mo2O9和γ-Bi2MoO6这三种形式。根据相关文献的研究记载表明,当Bi2MoO6以γ-Bi2MoO6的形式存在时,其光催化性能明显优于α-Bi2Mo3O12和β-Bi2Mo2O9这两种存在形式。γ-Bi2MoO6作为一种极其简单的奥里维里斯(Aurivillius)型氧化物,它是由共角的MoO6钙钛矿片层和交替的(Bi2O2)2+层组成的层状结构复合氧化物。Bi2MoO6作为一种新型优良的环保半导体光催化剂具有以下优点:高效、无毒、稳定性高、价格低廉、氧化还原能力强、光能利用率高且响应波长在可见光范围内。同时,Bi2MoO6可以作为离子导体、光导体、声光材料、气体传感器以及光催化剂使用,其优越的物理化学性能备受科研人员的青睐。
Bi2MoO6的禁带宽度在2.5~2.8eV之间,由于其禁带宽度较小故而能被可见光(420~500nm)激发,并表现出较高的光催化活性。现在对Bi2MoO6的研究主要集中于利用各种制备方法对其微观形貌进行调控以及掺杂金属、非金属或者稀土元素对光催化剂进行改性试验以提高其光催化性能,但是在目前所见的报道中,尚未发现通过共掺杂稀土与碱土金属共掺杂提高Bi2MoO6活性等的研究。
发明内容
本发明提供了一种溶胶凝胶制备钼酸铋共掺杂样品的方法,采用柠檬酸络合溶胶-凝胶法,首次利用Eu3+和Fe3+共掺杂提高Bi2MoO6活性,通过光催化实验验证表明所得共掺杂钼酸铋催化剂相比单掺杂催化剂的活性有了显著提高,具有更加优越的物化性能。
为解决上述技术问题,本申请实施例提供了一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,包括以下步骤:
a)制备A溶液:常温常压下取10mmolBi(NO3)3·5H2O溶于50ml稀硝酸中,然后加入10mmol柠檬酸,通过磁力搅拌器加热至80℃混合均匀,记为溶液A;
b)制备B溶液:取1.45mmol的(NH4)6MO7O24·4H2O溶于50ml蒸馏水中,并加入10mmol柠檬酸,用玻璃棒搅拌均匀,记为溶液B;
c)制备C溶液:将B溶液缓慢注入A溶液,混合均匀至澄清液体时,调节pH值至6.5,记为溶液C;
d)制备D溶液:向C溶液掺杂Eu3+,搅拌均匀,记为溶液D;
e)制备E溶液:向D溶液中掺杂Fe3+,5min后调节pH至6.5,记为溶液E;
f)制备钼酸铋催化剂:待E溶液变成粘稠的凝胶状,将其转入坩埚中,然后放入80℃的烘箱中烘干,待坩埚中的凝胶状前驱体变成黑色蜂窝状固体,将其取出,并在研钵中研磨至粉末状,取3g黑色粉末于坩埚中,在450℃下煅烧5h,得到淡黄色粉末,即为制备的钼酸铋光催化剂。
作为本方案的优选实施例,所述的步骤a)中所使用的稀硝酸为45ml蒸馏水和5ml浓硝酸稀释而成。
作为本方案的优选实施例,所述的步骤c)中调节pH值时,先利用浓氨水调节pH至6.3-6.7之间,再继续加热搅拌40min,最后再调pH至6.5。
作为本方案的优选实施例,所述的步骤d)中掺杂Eu3+的摩尔比为n(Eu)/n(Bi)=0.75%。
作为本方案的优选实施例,所述的步骤e)中掺杂Fe3+的摩尔比为n(Fe)/n(Bi)=0.5%。
本申请实施例中提供的一个或多个技术方案,至少具有如下技术效果或优点:
采用柠檬酸络合溶胶-凝胶法,首次利用Eu3+和Fe3+共掺杂提高Bi2MoO6活性,通过光催化实验验证表明所得共掺杂钼酸铋催化剂相比单掺杂催化剂的活性有了显著提高,具有更加优越的物化性能。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。
图1是本申请实施例的流程结构示意图;
图2是本申请实施例的光催化实验中不同催化剂降解罗丹明效率变化曲线;
图3是本申请实施例的不同催化剂的XRD图谱。
具体实施方式
本发明提供了一种溶胶凝胶制备钼酸铋共掺杂样品的方法,采用柠檬酸络合溶胶-凝胶法,首次利用Eu3+和Fe3+共掺杂提高Bi2MoO6活性,通过光催化实验验证表明所得共掺杂钼酸铋催化剂相比单掺杂催化剂的活性有了显著提高,具有更加优越的物化性能。
为了更好的理解上述技术方案,下面将结合说明书附图以及具体的实施方式对上述技术方案进行详细的说明。
如图1-图3所示,一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,包括以下步骤:
a)制备A溶液:常温常压下取10mmolBi(NO3)3·5H2O溶于50ml稀硝酸中,然后加入10mmol柠檬酸,通过磁力搅拌器加热至80℃混合均匀,记为溶液A;
b)制备B溶液:取1.45mmol的(NH4)6MO7O24·4H2O溶于50ml蒸馏水中,并加入10mmol柠檬酸,用玻璃棒搅拌均匀,记为溶液B;
c)制备C溶液:将B溶液缓慢注入A溶液,混合均匀至澄清液体时,调节pH值至6.5,记为溶液C;
d)制备D溶液:向C溶液掺杂Eu3+,搅拌均匀,记为溶液D;
e)制备E溶液:向D溶液中掺杂Fe3+,5min后调节pH至6.5,记为溶液E;
f)制备钼酸铋催化剂:待E溶液变成粘稠的凝胶状,将其转入坩埚中,然后放入80℃的烘箱中烘干,待坩埚中的凝胶状前驱体变成黑色蜂窝状固体,将其取出,并在研钵中研磨至粉末状,取3g黑色粉末于坩埚中,在450℃下煅烧5h,得到淡黄色粉末,即为制备的钼酸铋光催化剂
其中,在实际应用中,所述的步骤a)中所使用的稀硝酸为45ml蒸馏水和5ml浓硝酸稀释而成。
其中,在实际应用中,所述的步骤c)中调节pH值时,先利用浓氨水调节pH至6.3-6.7之间,再继续加热搅拌40min,最后再调pH至6.5。
其中,在实际应用中,所述的步骤d)中掺杂Eu3+的摩尔比为n(Eu)/n(Bi)=0.75%。
其中,在实际应用中,所述的步骤e)中掺杂Fe3+的摩尔比为n(Fe)/n(Bi)=0.5%。
对所得共掺杂钼酸铋光催化剂进行光催化实验,过程如下:将初始浓度为5mg·L-1罗丹明B(RhB)溶液100ml作为目标降解物置于500ml烧杯中,称取0.05g光催化剂并使其均匀分布于罗丹明B(RhB)溶液中,光催化剂在溶液中呈悬浮状态,加入0.1ml浓度为10%的H2O2。为了达到溶解-吸附平衡,将此悬浮液在磁力搅拌条件下暗反应30min,将其置于距液面14cm的可见光光源(250W金卤灯)下进行光催化实验,每隔10min取上清液在罗丹明B(RhB)的最大吸收波长处(554nm)测其吸光度,共光照反应50min,所得结果如图2和图3所示。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (5)
1.一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,包括以下步骤:
a)制备A溶液:常温常压下取10mmolBi(NO3)3·5H2O溶于50ml稀硝酸中,然后加入10mmol柠檬酸,通过磁力搅拌器加热至80℃混合均匀,记为溶液A;
b)制备B溶液:取1.45mmol的(NH4)6MO7O24·4H2O溶于50ml蒸馏水中,并加入10mmol柠檬酸,用玻璃棒搅拌均匀,记为溶液B;
c)制备C溶液:将B溶液缓慢注入A溶液,混合均匀至澄清液体时,调节pH值至6.5,记为溶液C;
d)制备D溶液:向C溶液掺杂Eu3+,搅拌均匀,记为溶液D;
e)制备E溶液:向D溶液中掺杂Fe3+,5min后调节pH至6.5,记为溶液E;
f)制备钼酸铋共掺杂样品:待E溶液变成粘稠的凝胶状,将其转入坩埚中,然后放入80℃的烘箱中烘干,待坩埚中的凝胶状前驱体变成黑色蜂窝状固体,将其取出,并在研钵中研磨至粉末状,取3g黑色粉末于坩埚中,在450℃下煅烧5h,得到淡黄色粉末,即为制备的钼酸铋共掺杂样品。
2.根据权利要求1所述的一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,所述的步骤a)中所使用的稀硝酸为45ml蒸馏水和5ml浓硝酸稀释而成。
3.根据权利要求1所述的一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,所述的步骤c)中调节pH值时,先利用浓氨水调节pH至6.3-6.7之间,再继续加热搅拌40min,最后再调pH至6.5。
4.根据权利要求1所述的一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,所述的步骤d)中掺杂Eu3+的摩尔比为n(Eu)/n(Bi)=0.75%。
5.根据权利要求1所述的一种溶胶凝胶制备钼酸铋共掺杂样品的方法,其特征在于,所述的步骤e)中掺杂Fe3+的摩尔比为n(Fe)/n(Bi)=0.5%。
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