CN111569867A - 一种球磨法制备负载型贵金属VOCs降解催化剂的方法 - Google Patents
一种球磨法制备负载型贵金属VOCs降解催化剂的方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 12
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 7
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Abstract
本发明涉及一种球磨法制备负载型贵金属VOCs降解催化剂的方法,属于材料科学与工程技术和化学领域。本发明方法制备的催化剂为以高表面积和孔隙率的惰性材料(如Al2O3、堇青石等)和过渡金属氧化物(Co3O4、MnO2、Fe3O4以及TiO2等)为载体,通过球磨法负载贵金属Pt、Rh、Pd、Au等贵金属单原子、团簇或纳米颗粒,制备用于VOCs催化氧化的催化剂。首先配置一定浓度的载体分散溶液A,分散均匀后加入贵金属前驱体溶液B,将溶液B加入到溶液A中均匀搅拌吸附后置于行星球磨机中进行液相球磨,经过抽滤、干燥回收得到催化剂。通过控制载体种类、贵金属前驱体浓度和球磨工艺参数可以得到不同种类的负载型贵金属催化剂。本发明具有高效快捷、成本低廉、大规模制备、结构均一稳定等优点。相对于传统方法具有显著的优势。
Description
(2)技术领域
本发明涉及球磨法制备负载型贵金属VOCs降解催化剂的方法,属于材料科学与工程技术和化学领域。
(3)背景技术
近年来,由挥发性有机化合物(VOCs)引起的环境问题(如光化学烟雾、臭氧和PM2.5)以及人类健康问题引起了国家和社会的高度关注。在VOCs的降解技术中,催化氧化法因降解效果显著,能耗较低而被认为是有发展前途的处理技术,其关键在于催化剂的选择和制备。目前常用的是贵金属催化剂(如Pt、Au、Pd、Rh等),其d电子轨道未被填满,有利于反应物的吸附和活化。虽然贵金属催化剂的活性较高,但普遍存在合成路线繁琐,价格较高,在制备和反应过程中容易发生烧结、流失或中毒现象。
在提高VOCs催化氧化效率,降低其转化温度的同时增加贵金属的分散度、减少贵金属的用量仍然是一个挑战。金属纳米结构(例如单原子、团簇和纳米颗粒)作为负载型催化剂的活性物质,其形貌和尺寸是影响VOCs转化效率的重要因素。因此,合理并精确调控金属纳米结构的尺寸和形貌,选择合适的载体能够增强金属-载体相互作用,提高催化过程中的电子传输性能。由于VOCs的分子结构较大,选用高表面积的介孔和大孔材料有利于反应物分子与催化剂活性中心的接触,促进了反应中的吸附、脱附、扩散等过程。尽管现阶段的研究中已经合成了一系列负载型贵金属催化剂用于VOCs的催化降解,并研究了贵金属纳米结构的种类和形貌对催化效率的影响,但由于制备工艺的稳定性较差、反应温度较高,难以获得尺寸均匀,结合稳定且成本低廉的VOCs降解催化剂。因此开发一种过程简单的规模化制备负载型贵金属VOCs 降解催化剂的方法是相关领域亟待解决的问题。
本发明提出了一种通过球磨法来制备负载型贵金属VOCs降解催化剂的方法,选用成本较低的多孔结构载体和过渡金属氧化物载体,通过液相球磨法使贵金属负载在基底材料上,通过调节球磨工艺参数和前驱体溶液浓度来控制颗粒尺寸的大小,实现了室温环境下高分散度、结构稳定的负载型贵金属VOCs降解催化剂的大规模合成。
(4)发明内容
1、本发明的目标
本发明提出了一种分散度高、结构稳定的不同载体负载贵金属单原子、团簇或纳米颗粒的 VOCs降解催化剂的制备方法。通过液相球磨将贵金属前驱体溶液还原成纳米结构,并使其均匀且牢固地分散在载体上,从而简单有效地制备负载型贵金属VOCs降解催化剂。这一方法可显著提高VOCs催化氧化的效率,促进催化剂的大规模工业化应用进程。
2、本技术的发明要点
本发明要点如下:
(1)选取合适的溶剂配置质量-体积浓度为10-20mg/mL的载体分散液A,所述载体为可溶解或分散性良好的具有高表面积和孔隙率的惰性材料(如Al2O3、堇青石等)和过渡金属氧化物 (Co3O4、MnO2、Fe3O4以及TiO2等);所述的溶剂为乙醇或异丙醇;
(2)所述的贵金属前驱体溶液B为0.1mol/L的氯铂酸、四氨合硝酸铂、酞菁铂、氯钯酸、氯金酸、乙酰丙酮铑的水溶液;
(3)在室温下,将上述步骤(1)制备的载体分散液A超声分散处理约20min,使其分散均匀,将(2)中所述的贵金属前驱体溶液B分别加入超声处理后的溶液,再充分搅拌吸附约1h;
(4)将搅拌后成分均匀的溶液倒入密封良好的刚玉行星球磨罐中,在300rpm的转速下分别球磨1h、3h,得到样品C、D;
(5)将步骤(4)所得样品C、D进行抽滤并干燥回收,直接得到贵金属单原子、团簇或纳米颗粒负载的用于VOCs降解的催化剂。
本发明提出的球磨法制备负载型贵金属VOCs降解催化剂的方法,其优点在于具有快速高效、产率较高、结构稳定的特点。可以将化学还原得到的纳米级贵金属成分稳定分散在载体中,并通过控制贵金属前驱体浓度和球磨工艺参数来精确调控金属纳米结构的尺寸和形貌,进一步提高VOCs催化氧化效率,促进其大规模工业化应用。
(5)本发明的附图
图1是本发明方法制备的贵金属Pt负载的VOCs降解催化剂的透射电子显微镜图。(a),(b), (c)依次是Pt单原子负载于堇青石(CHC)载体、Pt团簇负载于介孔CeO2载体和Pt纳米颗粒负载于TiO2载体的VOCs降解催化剂。
图2是本发明方法制备的贵金属Pt团簇负载的堇青石(CHC)、介孔CeO2载体催化剂的甲苯催化氧化性能。(a),(b)分别为不同载量Pt团簇负载的堇青石(CHC)、介孔CeO2载体催化剂的甲苯转化率-温度图像。
(6)本发明实施例
以下介绍本发明方法的实施例:
实施例1
贵金属Pt团簇负载的堇青石(CHC)催化剂的制备。
首先,配置载体分散溶液A:100mL 10mg/mL堇青石蜂窝陶瓷粉末溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取800uL的0.1mol/L氯铂酸溶液加入载体CHC分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的灰白色糊状物,经真空干燥后即可得到Pt团簇负载的堇青石(CHC)催化剂。
实施例2
贵金属Au团簇负载的堇青石(CHC)催化剂的制备。
首先,配置载体分散溶液A:100mL 10mg/mL堇青石蜂窝陶瓷粉末溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯金酸(H2AuCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取800uL的0.1mol/L氯铂酸溶液加入载体CHC分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的灰白色糊状物,经真空干燥后即可得到Au团簇负载的堇青石(CHC)催化剂。
实施例3
贵金属Pd团簇负载的堇青石(CHC)催化剂的制备。
首先,配置载体分散溶液A:100mL 10mg/mL堇青石蜂窝陶瓷粉末溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯钯酸(H2PdCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取800uL的0.1mol/L氯钯酸溶液加入载体CHC分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的灰白色糊状物,经真空干燥后即可得到Pd团簇负载的堇青石(CHC)催化剂。
实施例4
贵金属Rh团簇负载的堇青石(CHC)催化剂的制备。
首先,配置载体分散溶液A:100mL 10mg/mL堇青石蜂窝陶瓷粉末溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的乙酰丙酮铑溶液,溶剂为水;将载体分散液A超声处理约 20min,使载体在溶剂中分散均匀。取800uL的0.1mol/L乙酰丙酮铑溶液加入载体CHC分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的灰白色糊状物,经真空干燥后即可得到Rh团簇负载的堇青石(CHC)催化剂。
实施例5
贵金属Pt颗粒负载的堇青石(CHC)催化剂的制备。
首先,配置载体分散溶液A:100mL 10mg/mL堇青石蜂窝陶瓷粉末溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取800uL的0.1mol/L氯铂酸溶液加入载体CHC分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理3h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的灰白色糊状物,经真空干燥后即可得到Pt颗粒负载的堇青石(CHC)催化剂。
实施例6
贵金属Pt单原子负载的介孔CeO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔CeO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体介孔CeO2分散溶液中,并使用磁力搅拌器搅拌30min。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的淡黄色糊状物,经真空干燥后即可得到Pt单原子负载的介孔CeO2催化剂。
实施例7
贵金属Pt团簇负载的介孔CeO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔CeO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体介孔CeO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1.5h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的淡黄色糊状物,经真空干燥后即可得到Pt单原子负载的介孔 CeO2催化剂。
实施例8
贵金属Pt纳米颗粒负载的介孔CeO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔CeO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体介孔CeO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理3h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的淡黄色糊状物,经真空干燥后即可得到Pt纳米颗粒负载的介孔CeO2催化剂。
实施例9
贵金属Au团簇负载的介孔CeO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔CeO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯金酸(H2AuCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯金酸溶液加入载体介孔CeO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1.5h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的淡黄色糊状物,经真空干燥后即可得到Au团簇负载的介孔CeO2催化剂。
实施例10
贵金属Pd团簇负载的介孔CeO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔CeO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯钯酸(H2PdCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯钯酸溶液加入载体介孔CeO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1.5h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的淡黄色糊状物,经真空干燥后即可得到Pd团簇负载的介孔CeO2催化剂。
实施例11
贵金属Rh团簇负载的介孔CeO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔CeO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的乙酰丙酮铑溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L乙酰丙酮铑溶液加入载体介孔CeO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1.5h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的淡黄色糊状物,经真空干燥后即可得到Rh团簇负载的介孔CeO2催化剂。
实施例12
贵金属Pt单原子负载的介孔TiO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔TiO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸(H2PtCl6)溶液加入载体介孔TiO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理0.5h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pt单原子负载的介孔TiO2催化剂。
实施例13
贵金属Pt团簇负载的介孔TiO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔TiO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸(H2PtCl6)溶液加入载体介孔TiO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pt团簇负载的介孔TiO2催化剂。
实施例14
贵金属Pt颗粒负载的介孔TiO2催化剂的制备。
首先,配置载体分散溶液A:50mL10mg/mL介孔TiO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸(H2PtCl6)溶液加入载体介孔TiO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理3h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pt颗粒负载的介孔TiO2催化剂。
实施例15
贵金属Pt团簇负载的介孔MnO2催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔MnO2溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体介孔MnO2分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的黑色糊状物,经真空干燥后即可得到Pt团簇负载的介孔MnO2催化剂。
实施例16
贵金属Pt团簇负载的Al2O3催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL Al2O3溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体Al2O3分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pt团簇负载的Al2O3催化剂。
实施例17
贵金属Pd团簇负载的Al2O3催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL Al2O3溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯钯酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯钯酸溶液加入载体Al2O3分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pd团簇负载的Al2O3催化剂。
实施例18
贵金属Pt团簇负载的介孔Co3O4催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔Co3O4溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体介孔Co3O4分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pt团簇负载的介孔Co3O4催化剂。
实施例19
贵金属Pt团簇负载的介孔Fe3O4催化剂的制备。
首先,配置载体分散溶液A:50mL 10mg/mL介孔Fe3O4溶液,溶剂为乙醇;贵金属前驱体溶液B:0.1mol/L的氯铂酸(H2PtCl6)溶液,溶剂为水;将载体分散液A超声处理约20min,使载体在溶剂中分散均匀。取200uL的0.1mol/L氯铂酸溶液加入载体介孔Fe3O4分散溶液中,并使用磁力搅拌器搅拌1h。将搅拌后成分均匀的溶液倒入刚玉材质内衬的球磨罐中,保持密封良好。设置行星球磨机的转速为300rpm,将上述溶液球磨处理1h。将球磨处理后的混合溶液进行抽滤,得到颜色均匀的白色糊状物,经真空干燥后即可得到Pt团簇负载的介孔Fe3O4催化剂。
Claims (1)
1.一种球磨法制备负载型贵金属VOCs降解催化剂的方法,其特征在于该方法包括以下步骤:
(1)选取合适的溶剂配置质量-体积浓度为10-20mg/mL的载体分散液A,所述载体为可溶解或分散性良好的具有高表面积和孔隙率的惰性材料(如Al2O3、堇青石等)和过渡金属氧化物(Co3O4、MnO2、Fe3O4以及TiO2等);所述的溶剂为乙醇、异丙醇等;
(2)所述的贵金属前驱体溶液B为0.1mol/L的氯铂酸、四氨合硝酸铂、酞菁铂、氯钯酸、氯金酸、乙酰丙酮铑的水溶液;
(3)在室温下,将上述步骤(1)制备的载体分散液A超声分散处理约20min,使其分散均匀,将(2)中所述的贵金属前驱体溶液B分别加入超声处理后的溶液,再充分搅拌吸附约1h;
(4)将搅拌后成分均匀的溶液倒入密封良好的刚玉内衬行星球磨罐中,在300rpm的转速下分别球磨1h、3h,得到样品C、D;
(5)将步骤(4)所得样品C、D进行抽滤并干燥回收,直接得到贵金属单原子、团簇或纳米颗粒负载的用于VOCs降解的催化剂。
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