CN112225199A - 一种氧化碳材料的制备方法及其应用 - Google Patents
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Abstract
本发明提供一种氧化碳材料的制备方法,将HCl加入到圆底烧瓶中,接着向烧瓶中加入碳纳米管,超声至碳管在溶液中均匀分布,继续搅拌,反应后的产物洗涤至pH为中性,并在烘箱中烘干,命名为HCl‑CNT;将H2O2加入到圆底烧瓶中,接着向烧瓶中加入HCl‑CNT,继续搅拌,反应后的产物用去离子水离心洗涤至中性,烘箱中烘干,制备成氧化碳纳米管。同时公开了其在电催化生产双氧水中的应用,该方法的反应后处理简单,且不会产生额外的废液,且反应机理明确,更有希望大规模应用。
Description
技术领域
本发明涉及一种氧化碳材料的制备方法及其应用,属于氧气电催化领域。
背景技术
过氧化氢(H2O2)是最重要的100种化学物质之一,在化学合成、医药、环境保护和燃料电池方面以每年400万吨的需求迅速增长。目前工业上合成H2O2主要依靠蒽醌法,这是一种多步骤的方法,涉及高耗能的蒸馏过程,有毒废物和危险的H2O2储存运输。此外,直接由氢气(H2)和氧气(O2)合成H2O2是一种可行的方法。然而,混合的H2/O2存在潜在的爆炸性,惰性载气稀释降低了双氧水的选择性和产率。为了解决这些严重的问题,关键在于发展一种高效节能和安全的H2O2生产技术。实际上,可以通过氧气还原反应(ORR)和水氧化反应(WOR)的的二电子的反应路径生成H2O2。
目前的氧还原生产H2O2电催化剂主要是贵金属材料(在酸性环境中)和碳材料(在碱性环境中),其中碳材料部分主要为氧化碳材料。大部分已报道的氧化碳材料,都是在强酸(12 M HCl)或者强碱(6 M KOH)中。反应后的产物需要多次水洗,以除去残余的酸或者碱。此外,反应后的强酸强碱溶液难以处理。
发明内容
针对目前用于氧化碳材料的氧化剂多为强酸强碱,反应后需要多次洗涤和废液难以处理的问题,我们采用30 wt%的H2O2作为氧化剂,在80℃下对碳材料进行氧化处理,以在碳材料表面修饰不同种类的含氧官能团。反应机理如下:碳材料经过浓盐酸处理后,表面残留的Fe催化H2O2生成羟基自由基(·OH)。由于羟基自由基的强氧化能力,第一步先在碳材料表面修饰羟基基团,随后羟基基团被·OH进一步氧化,大部分羟基基团氧化为羰基基团,还有小部分羰基基团被氧化为羧基基团。该方法的反应后处理简单,且不会产生额外的废液,且反应机理明确,更有希望大规模应用。
本发明是通过以下技术方案实现的:
(1)氧化碳材料的制备及表征:我们用碳纳米管作为实际应用对象。(i)将100ml HCl(12 M)加入到圆底烧瓶中,接着向烧瓶中加入1g的碳纳米管,超声10分钟至碳管在溶液中均匀分布,在80℃继续搅拌2h。反应后的产物用去离子水离心洗涤至PH为中性,并在烘箱中60℃过夜烘干,并命名为HCl-CNT。(ii)将20ml 30wt%的H2O2加入到圆底烧瓶中,接着向烧瓶中加入200mg HCl-CNT,在80℃继续搅拌12h,反应后的产物用去离子水离心洗涤至中性,并在烘箱中60℃过夜烘干。同时与其他氧化剂的氧化效果进行对比,采用HNO3和H2SO4/HNO3=3:1作为对比氧化剂,氧化方法同30wt% H2O2的方法。
(2)氧还原生产双氧水的电化学测定:电化学测量采用电化学工作站(CHI760E,CH Instruments)。针对旋转环盘式电极(RRDE)的测量,建立了由RRDE(玻碳(GC)盘+ Pt环)、Hg/HgO参考电极和石墨棒对电极组成的三电极体系。将O2气体通入0.1 M KOH电解液中15分钟。通过线性扫描伏安法(LSV)在0.2 ~ 1.2 V(相对于RHE)中测定H2O2生成活性,扫描速率为20 mV s−1,转速为1600 rpm。在LSV测量期间,Pt环电位保持在1.2 V(相对于RHE)。
有益效果
本发明公开了一种氧化碳材料的制备方法,该方法采用30 wt%的H2O2作为氧化剂,更加环保,操作更为简单。该方法可在碳材料表面修饰更多的羰基基团,进一步提高氧还原生成双氧水的电催化性能。
将制备的氧化碳材料应用于电化学制备双氧水中,双氧水产生量比其他方式产量高。更适于大规模推广应用。
附图说明
图1 碳纳米管的制备机理图;
图2(a,b)氧化碳纳米管的透射电子显微镜图;(c)氧化碳纳米管的X射线衍射图谱;(d)氧化碳纳米管的X射线光电子能谱。
图3(a)不同氧化方式的LSV曲线和(b)对应的双氧水选择性;(c)用30wt% H2O2作为氧化剂,不同反应时间的LSV曲线和对应的(d)双氧水选择性;(e)用30wt% H2O2作为氧化剂,不同反应温度的LSV曲线和(f)对应的双氧水选择性。
图4 不同氧化方式氧化碳纳米管的双氧水产生量。
图5 在实际设备中双氧水的生成过程示意图。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
(1)氧化碳纳米管的制备及表征:(i)将100mlHCl(12 M)加入到圆底烧瓶中,接着向烧瓶中加入1g的碳纳米管,超声10分钟至碳管在溶液中均匀分布,在80℃继续搅拌2h。反应后的产物用去离子水离心洗涤至PH为中性,并在烘箱中60℃过夜烘干,并命名为HCl-CNT。(ii)将20ml 30wt%的H2O2加入到圆底烧瓶中,接着向烧瓶中加入200mg HCl-CNT,在80℃继续搅拌12h,反应后的产物用去离子水离心洗涤至中性,并在烘箱中60℃过夜烘干。利用透射电子显微镜、X射线衍射,X射线光电子能谱表征所制备的氧化碳纳米管。从透射电子显微镜表征结果可以看出碳管的直径约为20nm,表面有凹凸结构。在X射线光电子能谱和530-534ev处为氧官能团的吸收峰。上述实验结果表明我们成功制备了氧化碳纳米管。
(2)氧还原生产双氧水的电化学测定:电化学测量采用电化学工作站(CHI760E,CH Instruments)进行。针对旋转环盘式电极(RRDE)的测量,建立了由RRDE(玻碳(GC)盘+Pt环)、Hg/HgO参考电极和石墨棒对电极组成的三电极体系。用1um氧化铝水溶液悬浮液抛光5 min, 0.05um氧化铝水溶液悬浮液抛光5 min,在去离子水中超声处理30 s。将催化剂与水、2-丙醇和Nafion (5 wt%) (v/v/v = 4/1/0.02)混合,形成4 mg mL−1的悬浮液,制备催化剂油墨。超声处理60分钟后,将6ul催化剂墨水滴干在玻璃碳圆盘上(圆盘面积0.2475cm-2,环形面积0.1866 cm-2)。循环伏安法(CV)在0.2 ~ 1.20 V(相对于RHE)范围内进行,扫描速率为100 mV s−1,扫描频次为40个周期,在此周期内获得稳定的CV响应。然后,在相同的电位范围内,以500 mV s−1的扫描速率电化学清洗Pt环10个周期。将O2气体净化到电解液中15分钟(注意:如果Pt环清洗到ORR测量的时间间隔太长,Pt环的表面钝化可能会低估H2O2的选择性)。通过线性扫描伏安法(LSV)在0.2 ~ 1.2 V(相对于RHE)中测定H2O2生成活性,扫描速率为20 mV s−1,转速为1600 rpm。在LSV期间,Pt环电位保持在1.2 V(相对于RHE)。
为了定量测试双氧水的含量:以nafion 117膜为隔膜,在双室电池中采用双电极系统进行H2O2的电制。阴极室(80 mL)和阳极室(80 mL)在25℃充满相同的电解质。电极的制备方法是将催化剂墨水(250 uL)沉积在一张(1cm×1cm)的镍网上。铂网充当阳极。电解液为0.1M KOH溶液。在阴极连续通氧,以8 mA电流进行H2O2产率测定。为了量化所产生的H2O2,在一定时间采集样品,并与等量的硫酸氧钛溶液(6 g L-1)混合。以硫酸氧钛为指示剂,测定了过氧化氢的产率。用紫外-可见分光光度计(UV-8000, METASH.)检测所生成的络合物溶液,在最大吸收波长为406 nm。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (7)
1.一种氧化碳材料的制备方法,其特征在于,将HCl加入到圆底烧瓶中,接着向烧瓶中加入碳纳米管,超声至碳管在溶液中均匀分布,继续搅拌,反应后的产物洗涤至pH为中性,并在烘箱中烘干,命名为HCl-CNT;将H2O2加入到圆底烧瓶中,接着向烧瓶中加入HCl-CNT,继续搅拌,反应后的产物用去离子水离心洗涤至中性,烘箱中烘干,制备成氧化碳纳米管。
2.根据权利要求1所述的制备方法,其特征在于,所述的HCl的浓度为12 M ,加入的量为100ml,碳纳米管的加入量为1g。
3.根据权利要求1所述的制备方法,其特征在于,所述的加入H2O2为30wt%,加入量为20ml ;HCl-CNT的加入量为200mg,直径为20nm。
4.根据权利要求1所述的制备方法,其特征在于,所述继续搅拌的温度为80℃,12h。
5.一种权利要求1-4之一所述的制备方法制备的氧化碳材料在电催化生产双氧水中的应用。
6.根据权利要求5所述的应用,其特征在于,双氧水的制备方法为:建立了由工作电极、Hg/HgO参比电极和石墨棒对电极组成的三电极体系,将O2气体通入0.1 M KOH电解液中15分钟,制备双氧水;所述的工作电极由负载氧化碳材料的玻碳盘+ Pt环制成。
7.根据权利要求6所述的应用,其特征在于,所述的双氧水的制备方法为:用1um氧化铝水溶液悬浮液抛光5 min, 0.05um氧化铝水溶液悬浮液抛光5 min,在去离子水中超声处理30 s,将催化剂与水、2-丙醇和5 wt%Nafion (v/v/v = 4/1/0.02)混合,形成4 mg mL−1的悬浮液,制备催化剂油墨;超声处理60分钟后,将6ul催化剂墨水滴干在玻璃碳圆盘上,其中圆盘面积0.2475 cm-2,环形面积0.1866 cm-2,循环伏安法在0.2 ~ 1.20 V范围内进行,扫描速率为100 mV s−1,扫描频次为40个周期,在此周期内获得稳定的CV响应;在相同的电位范围内,以500 mV s−1的扫描速率电化学清洗Pt环10个周期,将O2气体净化到电解液中15分钟,制备双氧水。
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