CN111185166A - 一种高效催化氧化苯的负载型铂钨双金属纳米催化剂 - Google Patents
一种高效催化氧化苯的负载型铂钨双金属纳米催化剂 Download PDFInfo
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Abstract
一种高效催化氧化苯的负载型铂钨双金属纳米催化剂,属于催化化学与纳米科学领域。将PtW双金属纳米粒子负载到γ‑Al2O3载体上,经过焙烧后形成PtW/Al2O3催化剂。制备方法为:采用溶剂热法,将乙酰丙酮铂和羰基钨同时还原,形成PtW双金属纳米粒子,然后采用吸附法将其负载到γ‑Al2O3载体上。将负载后的催化剂先在马弗炉中焙烧,以除去残余有机物,然后在管式炉中600℃下10%H2/Ar气氛中焙烧,形成PtW/Al2O3双金属纳米催化剂。本发明所制备的PtW/Al2O3纳米催化剂制备过程简单,纳米粒子形貌规整,对苯的氧化表现出良好的催化活性,在催化领域具有良好的应用前景。
Description
技术领域
本发明涉及一种铂钨双金属纳米催化剂及其制备方法,具体涉及采用溶剂热合成法制备PtW纳米粒子,采用吸附法将其负载到γ-Al2O3上,经过焙烧形成负载型PtW/Al2O3催化剂,最终达到对苯的高效催化氧化。属于催化化学与纳米科学领域。
背景技术
随着经济的快速发展,大气污染成为难以避免的严重问题,而工业排放的挥发性有机化合物(Volatile Organic Compounds,简称为VOCs)是造成大气污染的主要原因。目前VOCs废气治理技术的相关研究已成为环境保护领域的一个热点。在治理和消除VOCs污染的技术中,催化氧化法被认为是目前最有效的消除方法之一,而催化氧化法的关键在于高活性的催化剂。
贵金属(例如Pd、Pt等)由于其优良的活性而广泛应用于VOCs的催化氧化。但由于贵金属的稀有性、高成本及高温易烧结失活等缺点,限制了贵金属催化剂的应用,人们对双金属催化剂进行了大量研究。利用双金属催化剂中双金属之间存在的协同作用,电子效应等优势,来改善贵金属催化剂所具有的劣势,以及减少贵金属用量,降低催化剂成本,提高催化活性。Saravanan等(G.Saravanan,et al.,Intermetallics,2018,94:179–185)采用浸渍法制备了Al2O3负载的Pt-Fe纳米催化剂,用于苯的催化氧化,苯转化的T90%约为180℃,催化剂在反应后仍保持其结构和形貌。Komatsu等(T.Komatsu,et al.,J.Phys.Chem.C2013,117,10483–10491)研究了液相沉积法制备的Pt-Cu/Al2O3催化剂,发现对CO的催化氧化,PtCu/Al2O3催化剂的活性明显优于Pt/Al2O3催化剂。据我们所知,目前还没有文献和专利报道过溶剂热法制备PtW/Al2O3双金属催化剂用于催化氧化苯的研究。
发明内容
本发明的目的在于利用溶剂热法制备PtW/Al2O3双金属纳米催化剂,用于对苯的催化氧化。
其特征在于,先利用溶剂热合成法制备PtW双金属纳米粒子,再采用吸附法将其负载到γ-Al2O3载体上,经过焙烧形成负载型PtW/Al2O3催化剂。上述样品中金属铂的负载量分别为0.20-0.5wt%。Pt与W的摩尔比为1.3:11-15。
上述的PtW双金属纳米粒子具有形貌规整的立方块状结构,其制备方法主要包括以下几个步骤:
利用溶剂热法制备PtW纳米粒子。具体步骤为:称取乙酰丙酮铂,加入十八烯、油胺、油酸,室温下搅拌溶解20min后加入抗坏血酸,继续搅拌5-10min,然后称取W(CO)6加入混合溶液中,形成混合前驱体溶液,室温下继续搅拌10-20min后装入反应釜中,在180-220℃下烘箱中反应7-10h;将反应后的溶液倒入离心管中,用环己烷和乙醇离心洗涤3-4次,得到PtW双金属纳米粒子。将所制得的PtW纳米粒子均匀分散至10mL环己烷中保存。优选每0.013mmol乙酰丙酮铂,对应2.5mL十八烯,2.5mL油胺,0.5mL油酸,0.28mmol抗坏血酸,继续搅拌5-10min,然后称取0.11-0.15mmol W(CO)6。
采用吸附法,将得到的PtW纳米粒子负载到γ-/Al2O3载体上,经过焙烧得到PtW/Al2O3双金属催化剂。具体步骤为:将一定量的γ-/Al2O3载体加入到含有纳米晶的环己烷溶液中,搅拌12h,离心干燥后得到负载型催化剂。将催化剂放入瓷舟中,在马弗炉中240-280℃下焙烧2-3h,然后转移到管式炉中10%H2/Ar气氛中580-620℃下焙烧2-3h,得到最终的PtW/Al2O3负载型双金属催化剂。
在苯浓度为1000ppm、苯/氧气摩尔比为1/200和空速为40 000mL/(g·h)的反应条件下,PtW/Al2O3催化剂T50%(苯转化率达到50%时所需反应温度)和T90%(苯转化率达到90%时所需反应温度)分别为133℃和140℃。
本发明具有制备过程简单等特征。本发明制备的尤其是PtW/Al2O3催化剂对苯氧化具有优异的催化活性,在苯催化氧化领域具有良好的应用前景。
利用D8 ADVANCE型X射线衍射仪(XRD)、JEOL-2010型透射电子显微镜(TEM)和岛津GC-2014气相色谱(GC)等仪器测定所得催化剂的晶体结构、粒子形貌以及对苯的催化氧化活性。结果表明,采用本发明的方法所制得的各样品均具有较好的结晶度,PtW纳米晶形貌规整,负载型双金属催化剂对苯的催化氧化活性相比较负载型纯铂催化剂显著提高。
附图说明
图1为所制得催化剂的XRD谱图。其中曲线(a)和(b)分别为PtW和Pt纳米粒子(NPs)的XRD谱图,(c)和(d)分别为PtW/Al2O3和对比样品Pt/Al2O3催化剂的XRD谱图。
图2为所制得催化剂的TEM照片。图中(a,b)为PtW NPs的TEM照片,(c)为Pt NPs的TEM照片,(d,e)分别为PtW/Al2O3催化剂的TEM照片,(f)为对比样品Pt/Al2O3催化剂的TEM照片。
图3为所制得PtW/Al2O3和对比样品Pt/Al2O3催化剂对苯催化氧化的活性曲线图。反应条件为:1000ppm苯+20vol%氧气+氮气(平衡气),空速为40000mL/(g h)。
具体实施方式
为了进一步阐述本发明,下面以实施例作详细说明,但发明并不限于以下实施例。
实施例1
称取0.013mmol乙酰丙酮铂,加入2.5mL十八烯,2.5mL油胺,0.5mL油酸,室温下搅拌溶解20min后加入0.28mmol抗坏血酸,继续搅拌5-10min,然后称取0.14mmol W(CO)6加入混合溶液中,形成混合前驱体溶液,室温下继续搅拌10-20min后装入反应釜中,在200℃下烘箱中反应8h。将反应后的溶液倒入离心管中,用环己烷和乙醇离心洗涤3-4次,得到PtW双金属纳米粒子。将所制得的PtW纳米粒子均匀分散至10mL环己烷中保存。
采用吸附法,将得到的PtW双金属纳米粒子负载到γ-Al2O3载体上,经过焙烧过程得到PtW/Al2O3双金属催化剂。具体步骤为:将一定量的/Al2O3载体加入到含有纳米晶的环己烷溶液中,搅拌12h,离心干燥后得到负载型催化剂。将催化剂放入瓷舟中,在马弗炉中250℃下焙烧2h,然后转移到管式炉中10%H2/Ar气氛中600℃下焙烧2h,得到最终的PtW/Al2O3负载型双金属催化剂。
在苯浓度为1000ppm、苯/氧气摩尔比为1/200和空速为40 000mL/(g·h)的反应条件下,该催化剂T50%(苯转化率达到50%时所需反应温度)和T90%(苯转化率达到90%时所需反应温度)分别为133℃和140℃。
Claims (3)
1.一种高效催化氧化苯的PtW/Al2O3双金属纳米催化剂,其特征在于,利用溶剂热法制备PtW双金属纳米粒子,然后将PtW纳米粒子负载在γ-Al2O3载体上,样品中金属铂的负载量分别为0.20-0.5wt%;Pt与W的摩尔比为1.3:11-15。
2.权利要求1所述的高效催化氧化苯的PtW/Al2O3双金属纳米催化剂的制备方法,其特征在于,包括以下步骤:利用溶剂热法制备PtW纳米粒子。具体步骤为:称取乙酰丙酮铂,加入十八烯、油胺、油酸,室温下搅拌溶解20min后加入抗坏血酸,继续搅拌5-10min,然后称取W(CO)6加入混合溶液中,形成混合前驱体溶液,室温下继续搅拌10-20min后装入反应釜中,在180-220℃下烘箱中反应7-10h;将反应后的溶液倒入离心管中,用环己烷和乙醇离心洗涤3-4次,得到PtW双金属纳米粒子。将所制得的PtW纳米粒子均匀分散至10mL环己烷中保存。优选每0.013mmol乙酰丙酮铂,对应2.5mL十八烯,2.5mL油胺,0.5mL油酸,0.28mmol抗坏血酸,继续搅拌5-10min,然后称取0.11-0.15mmol W(CO)6;
采用吸附法,将得到的PtW纳米粒子负载到γ-/Al2O3载体上,经过焙烧得到PtW/Al2O3双金属催化剂。具体步骤为:将一定量的γ-/Al2O3载体加入到含有纳米晶的环己烷溶液中,搅拌12h,离心干燥后得到负载型催化剂。将催化剂放入瓷舟中,在马弗炉中240-280℃下焙烧2-3h,然后转移到管式炉中10%H2/Ar气氛中580-620℃下焙烧2-3h,得到最终的PtW/Al2O3负载型双金属催化剂。
3.按照权利要求1所述的高效催化氧化苯的PtW/Al2O3双金属纳米催化剂的应用,用于苯的催化氧化。
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