CN105561976B - 一种具有可见光活性的Bi2WO6微米球的制备方法 - Google Patents
一种具有可见光活性的Bi2WO6微米球的制备方法 Download PDFInfo
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- 238000005507 spraying Methods 0.000 claims abstract description 14
- 229910003893 H2WO4 Inorganic materials 0.000 claims abstract description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 41
- 239000011780 sodium chloride Substances 0.000 claims description 25
- 239000007832 Na2SO4 Substances 0.000 claims description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 16
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 7
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- 230000015572 biosynthetic process Effects 0.000 description 7
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- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
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- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 241000165940 Houjia Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 230000005540 biological transmission Effects 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种具有可见光活性的Bi2WO6微米球的制备方法,以BiC6H5O7和H2WO4为原料,经超声喷雾法制得均匀的具有中空结构的Bi2WO6微米球。本发明将Bi2WO6可见光催化剂用于气相空气污染物NO的去除,具有高催化效率。该催化剂制备方法简单,以可见光为驱动能,用于大气污染控制,有利于环境和能源的可持续发展。本发明通过简单的调整溶液配方,制备出不同形貌的Bi2WO6微米球,这些形貌的存在均对NO的降解效率有提升的作用;得到了一例具有中空结构的Bi2WO6微米球,该中空微球有利于光生电子和空穴的分离,对NO的降解效率提升最为显著;本方法制备产品操作简单、设备要求低、无需复杂的合成装置。
Description
技术领域
本发明涉及一种具有可见光活性的催化剂,具体涉及一种具有可见光活性的Bi2WO6微米球的制备方法。
背景技术
目前,环境污染与防治是全球的重要课题,去除大气中的有害污染物更成为环境保护行业的一项重要任务。当前,以二氧化钛为代表的光催化材料尽管表现出优良的光催化性能,但光响应范围主要以紫外光为主,使其实际应用受到很大程度的限制。因此,开发能有效利用可见光的新型光催化材料在大气污染控制方面具有重要意义。
Bi2WO6是典型的n型直接半导体,带隙宽度约为2.70eV。它的价带顶主要由Bi 6s和O2p轨道杂化组成,而导带底则主要由W 5d轨道与少量Bi 6s轨道构成。由于Bi 6s轨道和O2p轨道杂化,是催化剂的价带电位升高,带隙宽度减少,因此Bi2WO6对可见光有吸收。另外,Bi2WO6三明治结构的层间空间能够为光催化反应提供活化点,夹层能接受光生电子,从而有效的抑制光生电子与空穴的复合,使光催化效率得到大幅度的提高。因此,Bi2WO6是一种很有发展前景的可见光催化材料。
目前,Bi2WO6通常采用高温固相反应和水热法等方法制备,制备的实验条件要求较苛刻,且得到的样品粉末通常粒径较大、比表面积较小,严重影响该光催化剂的光催化活性。
发明内容
为克服现有技术中的问题,本发明的目的是提供了一种具有可见光活性的Bi2WO6微米球的制备方法,该方法制得的Bi2WO6微米球在太阳光照射下具有良好的降解大气污染物NO 的能力,且制备过程成本低廉。
为了实现上述目的,本发明采用如下的技术方案:
一种具有可见光活性的Bi2WO6微米球的制备方法,将BiC6H5O7溶于氨水中,得到前驱体A,将H2WO4溶于氨水中,得到前驱体B;将前驱体A和前驱体B混合,并加入无机盐,然后加水定容至a,持续搅拌至形成均匀液体,再将得到的均匀的液体超声喷雾,喷雾形成的液滴经过煅烧,得到具有可见光活性的Bi2WO6微米球;其中,BiC6H5O7、H2WO4的物质的量比为10:5,无机盐为NaCl、Na2SO4或KCl;BiC6H5O7与NaCl的物质的量的比为10:1,BiC6H5O7与Na2SO4的物质的量的比为10:1;BiC6H5O7与KCl的物质的量的比为10:1;BiC6H5O7的物质的量与a的比为20mmol:80~100mL。
所述氨水的质量浓度为28%。
所述BiC6H5O7与氨水的比为2mmol:1mL。
所述H2WO4与氨水的比为1mmol:1mL。
所述喷雾功率采用1.7MHZ±10%。
所述煅烧是在马弗炉中进行的,并且煅烧的温度为600℃。
与现有技术相比,本发明具有的有益效果:
(1)本发明以BiC6H5O7和H2WO4为原料,通过先将BiC6H5O7的氨水溶液和H2WO4的氨水溶液混合,然后加入NaCl和水,由于加入了NaCl,使得在超声喷雾过程中形成以NaCl为核,Bi2WO6为壳的核壳包覆结构,最后经过水洗将NaCl洗出,留下具有可见光活性的中空Bi2WO6微米球;该中空Bi2WO6微米球由纳米片组装而成,粒径约为0.4微米,具有表面多孔,比表面积较大等优点。本发明通过添加一种廉价的NaCl原料,极大的改善了Bi2WO6的形貌及理化性能:将由纳米颗粒堆积而成的现有技术中的Bi2WO6实心微米球改善成具有可见光活性的中空结构的Bi2WO6微米球,该中空微球有利于光生电子和空穴的分离,显著 提升NO的降解效率,通过对比,其较现有技术中的Bi2WO6使NO去除效率显著提升了70.1%;
(2)本发明通过简单的调整溶液配方,实现了表面多孔的Bi2WO6中空微米球的可控制备。以KCl或Na2SO4替换NaCl显著影响Bi2WO6的形貌,确定NaCl对形成表面多孔中空结构的独特贡献。加入KCl后,微米球仍由和现有技术中的Bi2WO6一样的纳米颗粒堆积而成,但部分球的表面出现孔结构,说明Cl离子对表面孔结构的出现起主要作用;加入Na2SO4后,微米球变为由纳米片堆积而成,但并未观察到孔结构,说明Na离子对纳米片的形成起主要作用。加入KCl和Na2SO4均未形成中空结构,说明NaCl独特的结晶特性(结晶温度、晶型等)对中空结构的形成起主要作用;
(3)本发明加入KCl或Na2SO4均一定程度上改善Bi2WO6的光催化性能,其降解NO的效率较现有技术中的Bi2WO6分别提升了67.3%和16.7%,为提升Bi2WO6的光催化性能提供更多易操作的选择;
(4)另外,采用超声喷雾法制备产品,操作简单、设备要求低、无需复杂的合成装置。该Bi2WO6微米球可作为催化剂,以可见光为驱动能,用于大气污染控制,有利于环境和能源的可持续发展。
附图说明
图1为Bi2WO6、Bi2WO6-NaCl、Bi2WO6-KCl、Bi2WO6-Na2SO4在太阳光下降解NO的效果图;
图2为对比例1的Bi2WO6的SEM图片;
图3为实施例2的Bi2WO6-KCl的SEM图片;
图4为实施例3的Bi2WO6-Na2SO4的SEM图片;
图5为实施例1的Bi2WO6-NaCl的SEM图片;
图6为实施例1的Bi2WO6-NaCl的TEM图片。
具体实施方式
以下结合附图和具体实施例对本发明作具体的介绍。
实施例1
步骤一:20mmol BiC6H5O7溶于10mL的质量浓度为28%的氨水得到澄清透明的前驱体A,10mmol的H2WO4溶于10mL的质量浓度为28%的氨水得到澄清透明的前驱体B。
步骤二:将步骤一的前驱体A、前驱体B两者混合搅拌后,加入2mmol的NaCl,随后加水定容至100mL,持续搅拌至形成均匀液体。
步骤三:将步骤二得到的均匀液体进行超声喷雾,喷雾功率采用1.7MHZ±10%,喷雾形成的液滴随即进入管式马弗炉中,煅烧温度设置为600℃,在管式炉出口处收集固体产物,并将得到固体产物用去离子水清洗三次,得到具有可见光活性的Bi2WO6微米球(即Bi2WO6-NaCl),该微米球具有中空结构。
实施例2
步骤一:20mmol BiC6H5O7溶于10mL的质量浓度为28%的氨水得到澄清透明的前驱体A,10mmol的H2WO4溶于10mL的质量浓度为28%的氨水得到澄清透明的前驱体B;
步骤二:将前驱体A、前驱体B两溶液混和,并向其中加入2mmol的KCl,随后加水定容至100mL,持续搅拌至形成均匀液体。
步骤三:将步骤二得到的均匀液体进行超声喷雾,喷雾功率采用1.7MHZ±10%,喷雾形成的液滴随即进入管式马弗炉中,煅烧温度设置为600℃,在管式炉出口处收集固体产物,并将得到固体产物用去离子水清洗三次,得到Bi2WO6-KCl。
实施例3
步骤一:20mmol BiC6H5O7溶于10mL的质量浓度为28%的氨水得到澄清透明的前驱体A,10mmol的H2WO4溶于10mL的质量浓度为28%的氨水得到澄清透明的前驱体B。
步骤二:将步骤一的前驱体A、前驱体B两溶液混和,并向其中加入2mmol的Na2SO4,随后加水定容至100mL,持续搅拌至形成均匀液体。
步骤三:将步骤二得到的均匀液体进行超声喷雾,喷雾功率采用1.7MHZ±10%,喷雾形成的液滴随即进入管式马弗炉中,煅烧温度设置为600℃,在管式炉出口处收集固体产物,并将得到固体产物用去离子水清洗三次,得到Bi2WO6-Na2SO4。
对比例1
对比例1制得Bi2WO6,Bi2WO6的制备方法是将实施例1中的NaCl溶液换成去离子水,制备方法已发表于J.Phys.Chem.C 2010,114,6342-6349。据文献报道,Bi2WO6光催化性能优越于高温固相反应所制备的Bi2WO6,且超声喷雾的最佳煅烧温度为600℃(催化效果比400和500℃好)。
对对比例1的Bi2WO6、实施例1的Bi2WO6-NaCl、实施例2的Bi2WO6-KCl、实施例3的Bi2WO6-Na2SO4分别进行活性测试,以NO为目标污染物。将包含0.3g催化剂样品的培养皿放置在具有石英玻璃视窗的连续流动反应器中,通入起始浓度为400ppb的NO。待气流稳定后,打开模拟太阳光(300W卤钨灯)进行测试。采用NO光学分析仪动态监测反应器中的NO浓度,以NO出口浓度与初始浓度的比率(C/Co)来评价两种Bi2WO6的催化性能。图1为四种催化剂对NO降解效率图,由图可见,通过本发明制备的Bi2WO6-NaCl、Bi2WO6-KCl、Bi2WO6-Na2SO4均具备良好的光催化性能,分别显示出43.5%、43%、30.0%的最佳NO去除效率。相比于对比例1的Bi2WO625.7%的去除效率(图1的“Bi2WO6”表示对比例1制得的Bi2WO6),加盐的三种Bi2WO6的光催化性能都好于对比例1制备的Bi2WO6。这其中,Bi2WO6-NaCl性能最优,其NO去除效率比对比例中的Bi2WO6提升了0.7倍。
图2、图3、图4、图5分别为对比例1的Bi2WO6、实施例1的Bi2WO6-NaCl、实施例2的Bi2WO6-KCl和实施例3的Bi2WO6-Na2SO4的扫描电子显微镜(SEM)图片。从图2、图3、图4、图5可以看出,在制备过程中在加入盐后,Bi2WO6的微观形貌发生很大变化:对比例1的Bi2WO6是由粒径为20-30nm的纳米颗粒堆积而成的实心微米球(J.Phys.Chem.C 2010,114,6342-6349已发表其TEM图片);加入NaCl后,Bi2WO6微米球的表面分布着大量的孔,且微球变为空心结构(透射电子显微镜图,见图6),进一步证实了Bi2WO6-NaCl的表面多孔的中空结构,且该中空球表面由纳米片组装而成;加入KCl后,微米球仍由颗粒堆积而成,但部分球的表面出现孔结构,说明Cl离子对孔结构的形成起主要作用;加入Na2SO4后,微米球变为由纳米片堆积而成,但并未看到孔结构,说明Na离子对纳米片的形成起主要作用。
本发明步骤二中加水定容为80~100mL都可以,均能够得到如上述实施例中的结构,因为经步骤三中煅烧后均不含水。
需要说明的是,上述实施不以任何形式限制本发明,凡采用等同或替换或等效变化的方式所获得的技术方案,均落在本发明的保护范围内。
Claims (6)
1.一种具有可见光活性的Bi2WO6微米球的制备方法,其特征在于,将BiC6H5O7溶于氨水中,得到前驱体A,将H2WO4溶于氨水中,得到前驱体B;将前驱体A和前驱体B混合,并加入无机盐,然后加水定容至a,持续搅拌至形成均匀液体,再将得到的均匀的液体超声喷雾,喷雾形成的液滴经过煅烧,得到具有可见光活性的Bi2WO6微米球;其中,BiC6H5O7、H2WO4的物质的量比为10:5,无机盐为NaCl、Na2SO4或KCl;BiC6H5O7与NaCl的物质的量的比为10:1,BiC6H5O7与Na2SO4的物质的量的比为10:1;BiC6H5O7与KCl的物质的量的比为10:1;BiC6H5O7的物质的量与a的比为20mmol:80~100mL;
无机盐为NaCl时,0.3g Bi2WO6微米球对起始浓度为400ppb的NO的去除效率为43.5%;
无机盐为Na2SO4时,0.3g Bi2WO6微米球对起始浓度为400ppb的NO的去除效率为43%;
无机盐为KCl时,0.3g Bi2WO6微米球对起始浓度为400ppb的NO的去除效率为30.0%。
2.根据权利要求1所述的一种具有可见光活性的Bi2WO6微米球的制备方法,其特征在于,所述氨水的质量浓度为28%。
3.根据权利要求2所述的一种具有可见光活性的Bi2WO6微米球的制备方法,其特征在于,所述BiC6H5O7与氨水的比为2mmol:1mL。
4.根据权利要求2所述的一种具有可见光活性的Bi2WO6微米球的制备方法,其特征在于,所述H2WO4与氨水的比为1mmol:1mL。
5.根据权利要求1所述的一种具有可见光活性的Bi2WO6微米球的制备方法,其特征在于,所述喷雾功率采用1.7MHZ±10%。
6.根据权利要求1所述的一种具有可见光活性的Bi2WO6微米球的制备方法,其特征在于,所述煅烧是在马弗炉中进行的,并且煅烧的温度为600℃。
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