CN107308953A - 高活性Au‑Cu双金属纳米可见光催化剂及其制备方法 - Google Patents
高活性Au‑Cu双金属纳米可见光催化剂及其制备方法 Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 239000000243 solution Substances 0.000 description 10
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical class [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 9
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
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- 238000006243 chemical reaction Methods 0.000 description 5
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- 239000011943 nanocatalyst Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开一种高活性Au‑Cu双金属纳米可见光催化剂及其制备方法，是将可见光催化剂负载于金属氧化物载体表面，所述可见光催化剂为经过含氧气氛等离子体活化处理的Au和Cu纳米复合颗粒，金属总负载量为1~10wt%，Au与Cu的摩尔比为1~4：1~4。不仅制造成本显著低于常规纳米Au可见光催化剂，而且可见光催化活性及稳定性也远优于纳米Au可见光催化剂或Cu可见光催化剂；制备工艺简单，仅需采用等离子体快速的活化处理即可直接使用，极大地节省能量，缩短了催化剂的制备周期。
Description
技术领域
本发明属于气体污染治理领域，尤其涉及一种成本低、稳定性好的高活性Au-Cu双金属纳米可见光催化剂及其制备方法。
背景技术
负载于半导体载体表面的纳米催化剂因其独特的可见光吸收性质及优异的催化性能，将成为环境领域极具应用前景的可见光催化剂，纳米Au催化剂就是其中一种。纳米Au催化剂在可见光下能激发强局域表面等离激元共振效应产生热电子/空穴对，从而驱动表面氧化还原反应的进行；同时纳米Au-载体界面处形成的肖特基能垒则可有效阻止热电子跃回与空穴复合以提高量子效率，因而其可应用于可见光催化脱除室内气体污染物。然而，纳米Au催化剂的昂贵成本及其较差的稳定性，限制了其实际应用。
发明内容
本发明为了解决现有技术所存在的上述技术问题，提供一种成本低、稳定性好的高活性Au-Cu双金属纳米可见光催化剂及其制备方法。
本发明的技术方案是：一种高活性Au-Cu双金属纳米可见光催化剂，是将可见光催化剂负载于金属氧化物载体表面，所述可见光催化剂为经过含氧气氛等离子体活化处理的Au和Cu纳米复合颗粒，金属总负载量为1~10wt%，Au与Cu的摩尔比为1~4：1~4。
一种如上所述高活性Au-Cu双金属纳米可见光催化剂的制备方法，依次按照如下步骤进行：
a. 分别配制Au的前驱体标准溶液和Cu的前驱体标准溶液；
b. 按照金属总负载量1~10wt%、Au与Cu的摩尔比为1~4：1~4的比例将两种前驱体溶液混合，然后将混合的前驱体溶液浸渍金属氧化物载体，得浸渍品；
c. 用碱液或热水清洗浸渍品并通过抽滤或离心的方法去除多余溶液；
d．将c步骤所得固体在60~100 oC干燥3~10 h；
e．用含氧气氛等离子体活化处理，活化处理气体流量50~300 ml/min，氧含量5~100%，输入功率5~10 W，处理时间10~40 min，制得金属氧化物上负载Au-Cu纳米复合颗粒的可见光催化剂。
本发明的可见光催化剂是经过含氧气氛等离子体活化处理的Au和Cu纳米复合颗粒，不仅制造成本显著低于常规纳米Au可见光催化剂，而且可见光催化活性及稳定性也远优于纳米Au可见光催化剂或Cu可见光催化剂；制备工艺简单，仅需采用等离子体快速的活化处理即可直接使用，极大地节省能量，缩短了催化剂的制备周期。
具体实施方式
实施例1：
依次按照如下步骤进行：
a. 称取1 g氯金酸溶于100 ml去离子水中配制2.43×10-2 mol/L的氯金酸标准溶液（Au的前驱体标准溶液），称取1.3 g硝酸铜溶于50 ml去离子水中配制0.11 mol/L的硝酸铜标准溶液（Cu的前驱体标准溶液）；
b．称取1 g氧化铈（CeO2）置于25ml烧杯中，用移液管量取1.1 ml氯金酸标准溶液和2.25 ml硝酸铜溶液逐滴加入烧杯中浸渍氧化铈，并超声处理30 min，静置过夜，得以氧化铈为载体的浸渍品；
c．用大量80 oC热水清洗所得浸渍品并进行抽滤处理，直到在滤过液中滴加硝酸银溶液不产生白色沉淀为止，即彻底去除残留氯离子；
d．将所得固体在烘箱中70 oC干燥6 h；
e．将所得干燥固体用O2含量50%的氧氩混合气介质阻挡放电等离子体处理30 min，气体流速120 ml/min，输入功率5 W，制得金属担载量为2 wt%的Au-Cu/CeO2纳米可见光催化剂，两金属的摩尔比为Au:Cu = 0.5:1.5。
本发明实施例1的Au-Cu/CeO2纳米可见光催化剂在可见光辐照下，对模拟空气中甲醛氧化脱除实验如下：含50 ppm 甲醛、流量为100 SCCM的模拟空气，单程流过光催化反应器，当可见光光强为100 mW/cm2，高达90%的甲醛氧化为CO2，显示了高可见光催化活性且活性稳定；Au担载量2 wt%的Au/CeO2可见光催化剂，相同测试条件下甲醛转化率不足80%且活性逐渐下降；而担载量2 wt%的Cu/CeO2可见光催化剂，在相同测试条件下甲醛几乎无转化。
实施例2：
依次按照如下步骤进行：
a. 称取1 g氯金酸溶于100 ml去离子水中配制2.43×10-2 mol/L的氯金酸标准溶液（Au的前驱体标准溶液），称取1.3 g硝酸铜溶于50 ml去离子水中配制0.11 mol/L的硝酸铜标准溶液（Cu的前驱体标准溶液）；
b．称取2 g氧化钛（TiO2）置于100ml烧杯中，用移液管量取a中4.4 ml氯金酸标准溶液和3.0 ml硝酸铜溶液逐滴加入烧杯中浸渍氧化钛，并超声处理30 min，静置过夜，得以氧化钛为载体的浸渍品；
c．采用pH≈9的氨水溶液对所得浸渍品进行10 min的超声清洗，后离心处理10 min除去上层清液，重复上述过程，直到在上层清液中滴加硝酸银溶液不产生白色沉淀为止，即彻底去除残留氯离子；
d．将所得固体在烘箱中80 oC干燥6 h；
e．将所得干燥固体用O2气氛介质阻挡放电等离子体处理30 min，气体流速100 ml/min，输入功率5 W，制得金属担载量为2 wt%的Au-Cu/ TiO2纳米可见光催化剂，两金属的摩尔比为Au:Cu =1:1。
本发明实施例2的Au-Cu/ TiO2纳米可见光催化剂在可见光辐照下，对模拟空气中CO氧化脱除实验如下：含1200 ppm CO、流量为100 SCCM的模拟空气，单程流过光催化反应器，当可见光光强为100 mW/cm2，高达87%的CO氧化为CO2，显示了高可见光催化活性且活性稳定；Au担载量2 wt%的Au/ TiO2可见光催化剂，相同测试条件下CO转化率不足60%且活性逐渐下降；而担载量2 wt%的Cu/ TiO2可见光催化剂，在相同测试条件下CO几乎无转化。
实施例3：
依次按照如下步骤进行：
a. 称取1 g氯金酸溶于100 ml去离子水中配制2.43×10-2 mol/L的氯金酸标准溶液（Au的前驱体标准溶液），称取1.3 g硝酸铜溶于50 ml去离子水中配制0.11 mol/L的硝酸铜标准溶液（Cu的前驱体标准溶液）；
b．称取1 g氧化锌（ZnO）置于100ml烧杯中，用移液管量取a中4.4 ml氯金酸标准溶液和3.0 ml硝酸铜溶液逐滴加入烧杯中浸渍氧化锌，并超声处理30 min，静置过夜，得以氧化锌为载体的浸渍品；
c．称取0.72 g氢氧化钠溶于180 ml去离子水中配制0.1 mol/L的氢氧化钠碱性溶液，向所得浸渍品中加入氢氧化钠溶液并进行10 min的超声清洗，后离心处理10 min除去上层清液，重复上述过程，直到在上层清液中滴加硝酸银溶液不产生白色沉淀为止，即彻底去除残留氯离子；
d．将所得固体在烘箱中60 oC干燥6 h；
e．将所得干燥固体用O2气氛辉光放电等离子体处理30 min，气体流速100 ml/min，输入功率5 W，制得担载量2 wt% Au-Cu/ZnO纳米可见光催化剂，两金属的摩尔比为Au:Cu =1.5:0.5。
本发明实施例3的Au-Cu/ZnO纳米可见光催化剂在可见光辐照下，对模拟空气中CO氧化脱除实验如下：含1000 ppm CO、流量为200 SCCM的模拟空气，单程流过光催化反应器，当可见光光强为100 mW/cm2，高达70%的CO氧化为CO2，显示了高可见光催化活性且活性稳定；Au担载量2 wt%的Au/ ZnO可见光催化剂，相同测试条件下CO转化率不足50%且活性逐渐下降；而担载量2 wt%的Cu/ZnO可见光催化剂，在相同测试条件下CO几乎无转化。
Claims (2)
1.一种高活性Au-Cu双金属纳米可见光催化剂，是将可见光催化剂负载于金属氧化物载体表面，其特征在于：所述可见光催化剂为经过含氧气氛等离子体活化处理的Au和Cu纳米复合颗粒，金属总负载量为1~10wt%，Au与Cu的摩尔比为1~4：1~4。
2.一种如权利要求1所述高活性Au-Cu双金属纳米可见光催化剂的制备方法，其特征在于依次按照如下步骤进行：
a. 分别配制Au的前驱体标准溶液和Cu的前驱体标准溶液；
b. 按照金属总负载量1~10wt%、Au与Cu的摩尔比为1~4：1~4的比例将两种前驱体溶液混合，然后将混合的前驱体溶液浸渍金属氧化物载体，得浸渍品；
c. 用碱液或热水清洗浸渍品并通过抽滤或离心的方法去除多余溶液；
d．将c步骤所得固体在60~100 oC干燥3~10 h；
e．用含氧气氛等离子体活化处理，活化处理气体流量50~300 ml/min，氧含量5~100%，输入功率5~10 W，处理时间10~40 min，制得金属氧化物上负载Au-Cu纳米复合颗粒的可见光催化剂。
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