CN110614103A - 一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法 - Google Patents
一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法 Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- -1 bismuth phosphate compound Chemical class 0.000 title claims abstract description 10
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000004090 dissolution Methods 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
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- 239000007788 liquid Substances 0.000 claims abstract description 9
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- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 6
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
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- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 150000002989 phenols Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,包括以下步骤:(1)将表面活性剂加入到稀硝酸中,超声分散溶解,再加入硝酸铋,超声分散溶解,得到溶液A;(2)将偏钒酸铵、磷酸氢二钠加入到水中,超声分散溶解,得到溶液B;(3)将B溶液缓慢加入到溶液A中混合均匀得到溶液C;(4)将溶液C转入圆底烧瓶中,微波辐照,加热回流得到回流液;(5)将回流液的上层清液除去,离心分离,用纯水洗涤沉淀,再经脱水、干燥后即得。本发明提供的方法简单、高效、节能、环保,制备时间大幅缩短,所制备的产品光催化性能好,催化性能高。
Description
技术领域
本发明属于无机合成领域,具体涉及一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法。
背景技术
BiVO4的禁带宽度为2.4eV,此外,其具有价格更便宜,较高的光利用率,可重复利用和更简单的生产特性。BiVO4在可见光照射下具有良好的催化活性,其无毒、无害、无腐蚀性,可重复使用,可将污染物完全矿化为H2O、CO2。
磷酸铋光催化剂具有较高的电子-空穴分离率。磷酸铋中的磷酸盐带一个大的负电荷,这些负电荷使磷酸铋的偶极矩有了很大的提高,而这些偶极矩对电子-空穴对的分离有很积极的促进作用,然后使其获得较高的光催化活性。PO4 3-具有较强的亲水性,并且可以产生静电引力吸引光生空穴,可有效促进光生载流子从原始载体上分离开来。很多研究实践表明,BiPO4对有机物质均有良好的降解效果,如:酚类,苯类,染料、聚苯乙烯薄膜,药物等。且BiPO4因其低成本、高活性的特点,但在实际应用中仍存在一些缺点,如带隙较宽(Eg=3.85eV),只对紫外光敏感,光能利用率低等。
制备钒酸铋、磷酸铋的方法包括:溶胶-凝胶法,水热法、溶剂热法,高温固相法,液体沉淀法,超声波合成法,微乳液法等。上述制备方法存在一个共同问题,费时且耗能。
发明内容
为了解决上述技术问题,本发明提供一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法。该合成方法利用微波辐照作为反应条件,结合表面活性剂SDS的分散作用,能够快速、高效地合成具有良好光催化效果的钒酸铋、磷酸铋复合物。
本发明提供的技术方案如下:
一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,包括以下步骤:
(1)将表面活性剂加入到稀硝酸中,超声分散溶解,再加入硝酸铋,超声分散溶解,得到溶液A;
(2)将偏钒酸铵、磷酸氢二钠加入到水中,超声分散溶解,得到溶液B;
(3)将B溶液缓慢加入到溶液A中混合均匀得到溶液C;
(4)将溶液C转入圆底烧瓶中,微波辐照,加热回流得到回流液;
(5)将回流液的上层清液除去,离心分离,用纯水洗涤沉淀,再经脱水、干燥后即得。
具体的,所述表面活性剂为十二烷基硫酸钠。
具体的,所述步骤(1)中,稀硝酸的浓度为1mol/L,表面活性剂剂:稀硝酸:硝酸铋=1g:50ml:4.85g。
具体的,所述步骤(2)中偏钒酸铵、磷酸氢二钠与水的比例为0.58g:1.79g:50mL。
具体的,所述溶液A中铋离子与溶液B中钒酸根离子的摩尔比为2:1。
具体的,所述步骤(4)中微波辐照以间歇式工作,以30s为一个工作周期,工作12s,停止18s,微波功率为650W。
具体的,所述步骤(4)中微波辐照时间为20分钟。
具体的,所述步骤(5)中纯水洗涤次数为4~5次。
具体的,所述步骤(5)中脱水溶剂为丙酮。
具体的,所述步骤(5)中干燥温度为80℃,干燥时间为8小时。
本发明的有益效果:
(1)采用间歇式微波辐照的反应条件,一方面利用微波降低反应能垒,大幅加快反应速度以大幅缩短反应时间,提高反应效率;另一方面间歇式辐照能有效控制反应剧烈程度,兼顾反应平稳进行和反应体系稳定,并能节能降耗;
(2)选择SDS作为表面活性剂以达到良好分散体系的目的,利用SDS所制备的产物的光催化性能明显好于其他表面活性剂;
(3)合成方法简单,高效、节能、环保。
附图说明
图1为实施例1所制备产品的XRD图谱;
图2为实施例1所制备产品的SEM图;
图3为实施例1所制备的BiVO4/BiPO4光催化降解曲线。
具体实施方式
下面结合具体实施例对本发明进一步说明,本发明的内容完全不限于此。
实施例1
制备BiVO4/BiPO4复合光催化剂
制备步骤如下:
(1)将1g十二烷基硫酸钠(SDS)加入到50mL 1mol/L稀硝酸中,超声分散溶解,再加入4.85g硝酸铋(Bi(NO3)3·5H2O),超声分散溶解得到溶液A;
(2)将0.58g偏钒酸铵(NH4VO3)、1.79g磷酸氢二钠(Na2HPO4)溶于50mL纯水中,超声分散溶解得到溶液B;
(3)将B缓慢加入A中,边加边搅拌,混合均匀得到溶液C;
(4)将溶液C转入圆底烧瓶中,接上回流装置,在微波辐照下(微波的功率为650W,间歇式工作以30s为一个工作循环,工作12s,停止18s)的条件下微波加热20分钟得到回流液;
(5)将回流液冷却至室温,除去上层清液,然后转入离心管高速离心分离,用纯水洗涤4~5次,再用丙酮脱水一次后,于80℃真空干燥8小时,即得产品。
对比实施例1
合成方法同实施例1,区别在于表面活性剂为PVP。
对比实施例2
合成方法同实施例1,区别在于表面活性剂为CTAB。
实施例2
1、产品表征
(1)XRD图
如图1所示,通过与标准图谱的比对发现实施例1所合成的产品证实为BiVO4/BiPO4复合物。
(2)扫描电镜图像
从图2可以看出,实施例1所合成的钨酸钇为由许多小粒子堆积形成的多孔团状结构。
2、催化性能测试
(1)测试方法
取10mg/L甲基橙溶液50mL于250ml烧杯中,加入1.0g/L光催化剂,超声分散30s,转移至暗室中,静置30min后,待达到吸附平衡后,加入0.20ml H2O2作为引发剂,350W的氙灯作为光催化降解甲基橙溶液的可见光光源(用滤光片滤掉400nm以下的光),样品液面到氙灯光源出口高度约为14cm进行光催化降解,每隔一段时间将溶液离心,取上层清液用紫外可见分光光度计测量(~480nm)甲基橙溶液的吸光度,直到样品溶液吸光度不再下降。降解率通过下式计算:
Dt=(A0-At)/A0×100%
式中:A0为未经光照催化降解时甲基橙起始吸光度;
At为甲基橙降解t min之后的吸光度。
(2)测试结果
实施例1制备的样品,在光催化时间到达60min时,甲基橙降解率达到97.43%。
对比实施例1制备的样品,在光催化时间达到390min时,甲基橙降解率达到94.31%。
对比实施例2制备的样品,在光催化时间达到30min时,甲基橙降解率达到92.8%,虽然时间短但不再继续降解,综合比较实施例1明显优于后两者,其光催化活性和催化效率更高。
以上所述,仅为本发明较佳的具体实施方式,但本发明保护的范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内所做的任何修改,等同替换和改进等,均应包含在发明的保护范围之内。
Claims (10)
1.一种钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于,包括以下步骤:
(1)将表面活性剂加入到稀硝酸中,超声分散溶解,再加入硝酸铋,超声分散溶解,得到溶液A;
(2)将偏钒酸铵、磷酸氢二钠加入到水中,超声分散溶解,得到溶液B;
(3)将B溶液缓慢加入到溶液A中混合均匀得到溶液C;
(4)将溶液C转入圆底烧瓶中,微波辐照,加热回流得到回流液;
(5)将回流液的上层清液除去,离心分离,用纯水洗涤沉淀,再经脱水、干燥后即得。
2.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述表面活性剂为十二烷基硫酸钠。
3.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(1)中,稀硝酸的浓度为1mol/L,表面活性剂剂:稀硝酸:硝酸铋=1g:50ml:4.85g。
4.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(2)中偏钒酸铵、磷酸氢二钠与水的比例为0.58g:1.79g:50mL。
5.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述溶液A中铋离子与溶液B中钒酸根离子的摩尔比为2:1。
6.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(4)中微波辐照以间歇式工作,以30s为一个工作周期,工作12s,停止18s,微波功率为650W。
7.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(4)中微波辐照时间为20分钟。
8.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(5)中纯水洗涤次数为4~5次。
9.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(5)中脱水溶剂为丙酮。
10.根据权利要求1所述的钒酸铋、磷酸铋复合物可见光催化剂的微波合成方法,其特征在于:所述步骤(5)中干燥温度为80℃,干燥时间为8小时。
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