CN111659429B - 一种硫化镉-磷钨酸铯复合材料的制备方法及其作为可见光催化剂制取氢的用途 - Google Patents
一种硫化镉-磷钨酸铯复合材料的制备方法及其作为可见光催化剂制取氢的用途 Download PDFInfo
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Abstract
本发明公开了一种硫化镉‑磷钨酸铯复合材料的制备方法及其作为可见光催化剂制取氢的用途,采用原位合成法制备了一种硫化镉‑磷钨酸铯复合材料,将所制得的材料作为可见光催化剂,在300W的氙灯照射下进行光催化产氢实验,结果所制备的材料显示出良好的光催化性能。本发明通过将具有可见光催化性能的硫化镉纳米颗粒和具有多孔径特性的多金属氧酸盐复合,提高了该类材料的稳定性以及抗光腐蚀性能。本发明催化剂制备方法简单,易于操作,反应条件温和,反应后产物易于分离出,无腐蚀性,对环境无污染,设备投资少,成本低,适合批量生产。
Description
技术领域
本发明属于光催化技术领域,具体涉及一种硫化镉-磷钨酸铯复合材料的制备方法及其作为可见光催化剂制取氢的用途。
背景技术
氢能作为一种环境友好、清洁无污染的新型能源可以通过光催化分解水来制备。光催化被认为是一种理想的环境处理和能源再生技术,反应可在常温常压下进行。为了实现高效水分解生成氢气,人们开发出了大量用于制氢气的半导体光催化剂。硫化镉是一种典型的Ⅱ-Ⅳ型半导体,波尔半径为2.4nm,禁带宽度为2.42eV。硫化镉纳米材料随着纳米尺寸的变化以及形貌变化,其禁带宽度会跟着发生明显的变化,表现出比块状材料更为优异的光催化性能;但是由于硫化镉不稳定,易发生光腐蚀反应,影响其催化反应活性和稳定性,限制其在光催化方面的应用。磷钨酸铯盐在应用上可作为固体酸催化剂和载体,由于其具有酸性活性中心,更有利于水中分离出氢离子进而转化为氢气,可以提高光催化产氢反应的效率,且当其和硫化镉复合后形成的长条状结构更有利于电荷转移,降低光生电子和空穴的复合几率,从而提高光催化反应中光催化机的活性。
发明内容
本发明所要解决的技术问题是针对现有技术,旨在将具有良好的可见光响应能力的CdS与磷钨酸铯结合在一起,克服各自的弱点,增强其光催化性能,提供一种硫化镉-磷钨酸铯复合材料的制备方法及其作为可见光催化剂制取氢的用途。
本发明为解决上述技术问题所采取的技术方案为:一种硫化镉-磷钨酸铯复合材料的制备方法,首先合成磷钨酸铯,再利用原位合成法以磷钨酸铯、乙酸镉和硫化钠为主要原料,合成粗产物,然后通过高温煅烧,得到一种硫化镉-磷钨酸铯复合材料,具体包括以下步骤:
(1)称取适量的碳酸铯和磷钨酸分别溶于一定体积的蒸馏水中,得到碳酸铯溶液和磷钨酸溶液,然后在室温搅拌下将碳酸铯溶液缓慢滴加到磷钨酸溶液中,滴加完后继续搅拌8h,室温静置陈化12h;然后在60℃下蒸发干水分,得到白色固体,将白色固体研磨成粉末,于450℃下煅烧4h,得到磷钨酸铯;
(2)称取适量的上述制备的磷钨酸铯,超声分散于体积比为1:1的蒸馏水与乙醇的混合溶液中,得溶液A;
(3)将适量的水合乙酸镉加至溶液A中,在搅拌下用500W的氙灯照射30min,得溶液B;
(4)将九水硫化钠溶于一定体积的蒸馏水中,得溶液C;
(5)搅拌条件下将溶液C缓慢滴加至B液中,然后在暗处搅拌1h,室温条件下静置24h,离心分离沉淀,用蒸馏水和乙醇交替洗涤三次,70℃下蒸发水分,得到粗产物;
(6)将上述得到的粗产物研磨成粉末,然后转移至马弗炉中,在450℃下煅烧4h,得到所述的一种硫化镉-磷钨酸铯复合材料;
所述乙酸镉与硫化钠的物质的量比为1:1;
所述水合乙酸镉的化学式为Cd(Ac)2·2H2O;
所述磷钨酸的化学式为H3PW12O40;
所述磷钨酸铯的化学式为Cs2.5H0.5PW12O40;
所述硫化镉-磷钨酸铯复合材料的化学表示式为CdS/Cs2.5H0.5PW12O40;
所述反应的溶剂、试剂或原料均为化学纯。
进一步的,本发明还提供了所述硫化镉-磷钨酸铯复合材料的用途,该复合材料作为可见光催化剂,使用300W的氙灯模拟太阳光照射,以Na2S/Na2SO3作为牺牲剂的条件下,产氢速率可达到286.1μmol/(g·h)。
与现有技术相比,本发明的特点如下:
1、本发明所使用的化学试剂均为常用试剂、廉价易得;合成制备工艺简单,产生的污染极少,合成的光催化剂稳定性好,活性高;
2、本发明采用的原位合成法,有效防止磷钨酸铯盐的流失,较好的保持了磷钨酸铯盐的Keggin结构,负载后其特性不变,从而保证该催化剂具有较高的催化活性;
3、在制备的硫化镉/磷钨酸铯复合材料光催化剂中,硫化镉稳定而均匀的附着于磷钨酸铯盐表面,磷钨酸铯盐能有效降低光生电子与空穴的复合率,且提高了硫化镉的抗光腐蚀性,使其具有更加优异的光催化性能。
附图说明
图1为本发明制得的硫化镉-磷钨酸铯复合材料的XRD图。
图2为本发明制得的硫化镉-磷钨酸铯复合材料的IR图。
图3a为本发明制得的磷钨酸铯的SEM图,图3b为本发明制备得到的硫化镉-磷钨酸铯复合材料的SEM图。
图4为本发明制得的硫化镉-磷钨酸铯复合材料作为可见光催化剂催化产氢的曲线图。
具体实施方式
以下结合实施例对本发明作进一步详细描述,本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意组合。
实施例1
称取5.0mmol(1.64g)的碳酸铯和2.0mmol(5.76g)磷钨酸分别溶于25mL蒸馏水中,得到碳酸铯溶液和磷钨酸溶液,在室温搅拌下将碳酸铯溶液以1.0mL/min的速率缓慢滴加到磷钨酸溶液中,滴加完后继续搅拌8h,室温静置陈化12h;然后60℃下蒸干水分,得到白色固体,将白色固体研磨成粉末,450℃下煅烧4h,得到磷钨酸铯Cs2.5H0.5PW12O40;称取1.38mmol(4.43g)上述制备的磷钨酸铯Cs2.5H0.5PW12O40,超声分散于10mL蒸馏水与10mL乙醇的混合溶液中,得溶液A;称取1.38mmol(0.367g)的二水乙酸镉加至溶液A中,在搅拌下用500W Xe灯照射30min,得均匀透明的溶液B;称取1.38mmol(0.33g)的九水硫化钠溶于10mL水中,得溶液C;室温在搅拌条件下,将溶液C缓慢的滴入到溶液B中,暗处搅拌1h,再静置24h,离心分离,得到黄色沉淀物,将黄色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到粗产物;将上述得到的粗产物研磨成粉末,然后转移至马弗炉中,在450℃下煅烧4h,得到一种硫化镉-磷钨酸铯复合材料CdS/Cs2.5H0.5PW12O40。
用粉末X射线对所制得的硫化镉-磷钨酸铯复合材料进行组成结构分析,得到相应的衍射谱图(图1);用红外光谱对所制备的硫化镉CdS、磷钨酸铯Cs2.5H0.5PW12O40以及硫化镉-磷钨酸铯复合材料CdS/Cs2.5H0.5PW12O40进行红外谱结构分析,得到相应的红外吸收峰图谱(图2);用扫描电子显微镜SEM对所的制备的材料进行形貌表征,图3a为所制备的磷钨酸铯Cs2.5H0.5PW12O40的SEM图,图3b为所制备的硫化镉-磷钨酸铯复合材料CdS/Cs2.5H0.5PW12O40的SEM图。
称取0.1g所制备的硫化镉-磷钨酸铯复合材料并作为可见光催化剂分散于50mL的蒸馏水中,以0.5g的Na2S/Na2SO3作为牺牲剂溶于上述蒸馏水中的条件下,使用300W氙灯模拟太阳光照射,产氢速率可达到286.1μmol/(g·h)(图4)。
实施例2
称取5.0mmol(1.64g)的碳酸铯和2.0mmol(5.76g)磷钨酸分别溶于25mL蒸馏水中,得到碳酸铯溶液和磷钨酸溶液,在室温搅拌下将碳酸铯溶液以1.0mL/min的速率缓慢滴加到磷钨酸溶液中,滴加完后继续搅拌8h,室温静置陈化12h;然后60℃下蒸干水分,得到白色固体,将白色固体研磨成粉末,450℃下煅烧4h,得到磷钨酸铯Cs2.5H0.5PW12O40;称取1.0mmol(3.21g)上述制备的磷钨酸铯Cs2.5H0.5PW12O40,超声分散于10mL蒸馏水与10mL乙醇的混合溶液中,得溶液A;称取1.0mmol(0.27g)的二水乙酸镉加至溶液A中,在搅拌下用500W Xe灯照射30min,得均匀透明的溶液B;称取1.0mmol(0.24g)的九水硫化钠溶于10mL水中,得溶液C;室温在搅拌条件下,将溶液C缓慢的滴入到溶液B中,暗处搅拌1h,再静置24h,离心分离,得到黄色沉淀物,将黄色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到粗产物;将上述得到的粗产物研磨成粉末,然后转移至马弗炉中,在450℃下煅烧4h,得到一种硫化镉-磷钨酸铯复合材料CdS/Cs2.5H0.5PW12O40。
用粉末X射线对所制得的硫化镉-磷钨酸铯复合材料进行组成结构分析;用红外光谱对所制备的硫化镉-磷钨酸铯复合材料进行红外谱结构分析;用扫描电子显微镜SEM对所的制备的材料进行形貌表征。以所制备的硫化镉-磷钨酸铯复合材料作为可见光催化剂,以Na2S/Na2SO3作为牺牲剂的条件下,使用300W氙灯模拟太阳光照射,进行催化制取氢的实验。
实施例3
称取5.0mmol(1.64g)的碳酸铯和2.0mmol(5.76g)磷钨酸分别溶于25mL蒸馏水中,得到碳酸铯溶液和磷钨酸溶液,在室温搅拌下将碳酸铯溶液以1.0mL/min的速率缓慢滴加到磷钨酸溶液中,滴加完后继续搅拌8h,室温静置陈化12h;然后60℃下蒸干水分,得到白色固体,将白色固体研磨成粉末,450℃下煅烧4h,得到磷钨酸铯Cs2.5H0.5PW12O40;称取2.0mmol(6.42g)上述制备的磷钨酸铯Cs2.5H0.5PW12O40,超声分散于20mL蒸馏水与20mL乙醇的混合溶液中,得溶液A;称取2.0mmol(0.54g)的二水乙酸镉加至溶液A中,在搅拌下用500W Xe灯照射30min,得均匀透明的溶液B;称取2.0mmol(0.48g)的九水硫化钠溶于15mL水中,得溶液C;室温在搅拌条件下,将溶液C缓慢的滴入到溶液B中,暗处搅拌1h,再静置24h,离心分离,得到黄色沉淀物,将黄色沉淀物分别用蒸馏水和无水乙醇交替洗三次,然后在70℃下干燥12h后,得到粗产物;将上述得到的粗产物研磨成粉末,然后转移至马弗炉中,在450℃下煅烧4h,得到一种硫化镉-磷钨酸铯复合材料CdS/Cs2.5H0.5PW12O40。
用粉末X射线对所制得的硫化镉-磷钨酸铯复合材料进行组成结构分析;用红外光谱对所制备的硫化镉-磷钨酸铯复合材料进行红外谱结构分析;用扫描电子显微镜SEM对所的制备的材料进行形貌表征。以所制备的硫化镉-磷钨酸铯复合材料作为可见光催化剂,以Na2S/Na2SO3作为牺牲剂的条件下,使用300W氙灯模拟太阳光照射,进行催化制取氢的实验。
Claims (1)
1.一种硫化镉-磷钨酸铯复合材料的用途,其特征在于,该复合材料作为可见光催化剂,使用300W的氙灯模拟太阳光照射,以Na2S/Na2SO3作为牺牲剂的条件下,产氢速率可达到286.1μmol/(g·h);
所述硫化镉-磷钨酸铯复合材料的制备方法包括以下步骤:
(1)称取适量的碳酸铯和磷钨酸分别溶于一定体积的蒸馏水中,得到碳酸铯溶液和磷钨酸溶液,然后在室温搅拌下将碳酸铯溶液缓慢滴加到磷钨酸溶液中,滴加完后继续搅拌8h,室温静置陈化12h;然后在60℃下蒸发干水分,得到白色固体,将白色固体研磨成粉末,于450℃下煅烧4h,得到磷钨酸铯;
(2)称取适量的上述制备的磷钨酸铯,超声分散于体积比为1:1的蒸馏水与乙醇的混合溶液中,得溶液A;
(3)将适量的水合乙酸镉加至溶液A中,在搅拌下用500W的氙灯照射30min,得溶液B;
(4)将九水硫化钠溶于一定体积的蒸馏水中,得溶液C;
(5)搅拌条件下将溶液C缓慢滴加至B液中,然后在暗处搅拌1h,室温条件下静置24h,离心分离沉淀,用蒸馏水和乙醇交替洗涤三次,70℃下蒸发水分,得到粗产物;
(6)将上述得到的粗产物研磨成粉末,然后转移至马弗炉中,在450℃下煅烧4h,得到所述的一种硫化镉-磷钨酸铯复合材料;
所述乙酸镉与硫化钠的物质的量比为1:1;
所述磷钨酸的化学式为H3PW12O40;
所述磷钨酸铯的化学式为Cs2.5H0.5PW12O40;
所述水合乙酸镉的化学式为Cd(Ac)2·2H2O;
所述硫化镉-磷钨酸铯复合材料的化学表示式为CdS/Cs2.5H0.5PW12O40;
参加原料均为化学纯。
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