CN113952971A - 一种制备具有高效光催化析氢活性的红磷/过渡金属磷化物/SiO2光催化剂的方法 - Google Patents
一种制备具有高效光催化析氢活性的红磷/过渡金属磷化物/SiO2光催化剂的方法 Download PDFInfo
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000001257 hydrogen Substances 0.000 title claims abstract description 35
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 35
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 32
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
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- 239000007864 aqueous solution Substances 0.000 claims 3
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Abstract
本发明公开了一种制备具有高效光催化析氢活性的红磷/过渡金属磷化物/SiO2光催化剂的方法,属于光催化析氢领域。该光催化剂采用二氧化硅,金属盐(乙酸盐,硝酸盐),红磷(RP)为原料,成功地制备了具有超高光催化析氢活性的红磷/过渡金属磷化物光催化剂。该光催化剂相对于传统的纯RP以Pt作为助催化剂的光催化剂具有超高的光催化析氢活性(不添加任何牺牲剂和pH调节,外加助催化剂,可见光下的析氢活性为11.79μmol·h−1)和广谱响应,这是由于过渡金属磷化物与RP之间的密切相互作用提高了可见光吸收,加速了光致电子‑空穴分离。本发明中,过渡金属来源丰富,价格低廉,作为光催化析氢反应的助催化剂具有比贵金属Pt更优异的性能,是一种很有前景的环境友好材料。
Description
技术领域
本发明属于光催化领域,具体涉及制备具有高效光催化析氢活性的红磷/过渡金属磷化物/SiO2光催化剂的方法。
背景技术
光催化被认为是将太阳能转化为H2化学能的最佳策略之一,以应对全球能源短缺和环境污染这两大棘手危机。氢是一种通过光催化裂解水获得的清洁可再生能源,可以部分替代传统化石燃料,从而缓解日益严重的能源危机和环境恶化。同时,H2的燃烧产物是水,不会对环境造成任何破坏。到目前为止,超分子、共价有机框架、氮化碳、红磷(RP)、等无金属光催化剂因其成本低、易得、无毒等独特优势而成为研究热点。特别是富含地球的RP,其可见光吸收范围可达700 nm,且具有负导带位置特性,是一种很有前景的制氢光催化剂。然而,缓慢的电荷迁移和表面反应动力学的固有缺陷限制了其析氢反应(HER)效率的不理想水平。为了克服这些缺点,提高RP光催化剂的效率,人们进行了许多努力,值得注意的是,在光催化剂上负载助催化剂可以提供更多的活性位点,降低HER的活化能。迄今为止,大多数基于RP的光催化剂使用贵金属Pt作为HER的助催化剂。遗憾的是,铂的稀有和昂贵的性质严重限制了它的大规模应用。因此,开发地球丰富、廉价、高效的无贵金属助催化剂是光催化HER的迫切需要。近年来,高电导率、低产氢过电位的过渡(Ni, Fe, Co, Cu, Mo)金属磷酸盐被广泛地用作光催化HER的候选助催化剂。
发明内容
本发明利用来源丰富且环境友好的红磷作为原料之一,制备了可用作光催化析氢的光催化剂。
本发明制备过程简单,成本较低,不需要昂贵设备,所得产品光催化析氢性能高,在将来光催化领域具有很好的发展前景。
一种制备具有高效光催化析氢活性的红磷/过渡金属磷化物/SiO2光催化剂的方法,制作过程包括以下步骤:
1)将5mL浓氨水,50mL无水乙醇,10mL去离子水,5mL正硅酸四乙酯加入到圆底烧瓶中,室温下搅拌6h制备SiO2纳米球;
2)0.0002M金属盐(乙酸盐,硝酸盐),0.00016M尿素,200mgSiO2加入到300mL去离子水中,70℃-80℃下水浴4h, 6h, 8h,制备不同时间的(Co, Fe, Ni)Px/SiO2;
3)将1g 商业RP加入到60mL 去离子水中,并转移到反应釜中200℃反应12h,得到纯净RP;
4)将100mg RP 粉末与100mg不同时间的(Co, Fe, Ni)Px/SiO2研磨混合均匀低真空条件下密封于石英安瓿内,500℃-600℃(5℃/min)煅烧2h,1℃/min降到280℃并保持3h,随后0.1℃/min降到室温,用CS2,无水乙醇,水清洗后得到RP/(Co, Fe, Ni)Px/SiO2;
5)采用场发射扫描电子显微镜(HITACHI Regulus 8100)和透射电子显微镜(JEOLJEM-2100F)观察样品的形貌和组成;
6)将100 mg的RP/(Co, Fe, Ni)Px/SiO2粉末分散在150 mL的超纯水中,不添加任何牺牲剂和pH调节。然后用300 W氙灯顶辐照色散,420 nm截止滤波器作为可见光(λ> 420nm)源。用气相色谱测定产氢量。
本发明具有以下优点:
本发明使用的原料主要是红磷,来源广泛、环保绿色、安全性高。
本发明方法制备的红磷/过渡金属磷化物,可用作光催化析氢的光催化剂,具有良好的光催化析氢活性。
本发明方法制备的具有超高光催化析氢活性的红磷/过渡金属磷化物光催化剂可大量合成,不需要昂贵设备,可广泛用于光催化析氢领域。
附图说明
图1是具体实施例1的具有高效光催化析氢性能的RP/CoP2/SiO2的制备流程图。
图2是具体实施例1的具有高效光催化析氢性能的RP/CoP2/SiO2的光催化产氢性能对比图。
图3是具体实施例1的具有高效光催化析氢性能的RP/CoP2/SiO2的光催化剂的SEM与TEM。
图4左为具体实施例2具有高效光催化析氢性能的RP/(Pt,CoFe,Ni)/SiO2的光催化产氢性能对比图;右为具体实施例4具有高效光催化析氢性能RP/CoP2/SiO2的光催化产氢性能对比图。
以下结合具体实施例,对本发明进行详细说明。
实施例1
1)将5mL浓氨水,50mL无水乙醇,10mL水,5mL正硅酸四乙酯加入到圆底烧瓶中,室温下搅拌6h制备SiO2;
2)0.0002M乙酸钴,0.00016M尿素,200mg SiO2加入到300mL去离子水中,80℃下水浴6h,制备不同时间的CoP2(6)/SiO2;
3)将1g 商业RP加入到60mL 去离子水中,并转移到反应釜中200℃反应12h,得到纯净RP;
4)将100mg RP 粉末与100mg CoP2(6)/SiO2研磨混合均匀低真空条件下密封于石英安瓿内,500℃(5℃/min)煅烧2h,1℃/min降到280℃并保持3h,随后0.1℃/min降到室温,用CS2,无水乙醇,水清洗后得到RP/ CoP2(6)/SiO2;
5)采用场发射扫描电子显微镜(HITACHI Regulus 8100)和透射电子显微镜(JEOLJEM-2100F)观察样品的形貌和组成;
6)将100 mg的RP/CoP2(6)/SiO2粉末分散在150 mL的超纯水中,不添加任何牺牲剂和pH调节。然后用300 W氙灯顶辐照色散,420 nm截止滤波器作为可见光(λ> 420 nm)源。用载氩气和热导检测器在线气相色谱测定产氢量。
实施例2
1)将所用的乙酸钴水溶液的溶度改为乙酸铁和乙酸镍, 其他操作同实例1。
实施例3
1)将所用的乙酸盐水溶液的溶度改为硝酸盐水溶液, 其他操作同实例1。
实施例4
1)将水浴改为4h, 8h其他操作同实例1。
实施例5
1)将水浴温度改为70℃,其他操作同实例1。
实施例6
1)将磷化温度改为550℃,600℃其他操作同实例1。
Claims (7)
1.一种制备具有高效光催化析氢活性的红磷/过渡金属磷化物/SiO2光催化剂的方法,其特征在于所述方法包括以下步骤:
1)将适量浓氨水,无水乙醇,正硅酸四乙酯加入到适量的水溶液中,搅拌混合均匀,连续搅拌得到SiO2纳米球;
2)将适量金属盐(乙酸盐,硝酸盐),尿素,硅球加入适量的水溶液中,恒温水浴,制备(Co, Fe, Ni)Px/SiO2;
3)将适量商业RP加入到水溶液中高温去除表面氧化层,得到纯净RP;
4)将适量RP与(Co, Fe, Ni)Px/SiO2研磨混合均匀,低真空条件下密封于石英安瓿内,退火,用CS2,无水乙醇,水清洗后得到RP/(Co, Fe, Ni)Px/SiO2;
5)采用场发射扫描电子显微镜(HITACHI Regulus 8100)和透射电子显微镜(JEOLJEM-2100F)观察样品的形貌和组成;
6)用气相色谱测定RP/(Co, Fe, Ni)Px/SiO2产氢量。
2.根据权利要求书1所述的制备方法,其特征在于,步骤1)中所述将5mL浓氨水,50mL无水乙醇,10mL水,5mL正硅酸四乙酯加入到圆底烧瓶中,室温下搅拌6h,制备SiO2纳米球。
3.根据权利要求书1所述的制备方法,其特征在于,步骤2)中所述金属盐(乙酸盐,硝酸盐)浓度为0.0002M,尿素浓度为0.00016M,SiO2纳米球200mg , 去离子水300mL,70℃-80℃下水浴4h, 6h, 8h,得到不同时间的(Co, Fe, Ni)Px/SiO2。
4.根据权利要求书1所述的制备方法,其特征在于,步骤3)中所述的将1g 商业RP加入到60mL 去离子水中,并转移到反应釜中200℃反应12h。
5.根据权利要求书1所述的制备方法,其特征在于,步骤4)中所述,将100mg RP 粉末与100mg不同时间的(Co, Fe, Ni)Px/SiO2研磨混合均匀低真空条件下密封于石英安瓿内,500℃-600℃(5℃/min)煅烧2h,1℃/min降到280℃并保持3h,随后0.1℃/min降到室温。
6.根据权利要求书1所述的制备方法,其特征在于,步骤5)中采用场发射扫描电子显微镜(HITACHI Regulus 8100)和透射电子显微镜(JEOL JEM-2100F)观察样品的形貌和组成。
7.根据权利要求书1所述的制备方法,其特征在于,步骤6)中所将100mg的不同时间的RP/(Co, Fe, Ni)Px/SiO2粉末分散在150 mL的超纯水中,不添加任何牺牲剂和pH调节,然后用300 W氙灯顶辐照色散,420 nm截止滤波器作为可见光(λ> 420 nm)源,用气相色谱测定产氢量。
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