CN111013627A - 一种Cu/OCN复合催化臭氧分解材料及其制备方法与应用 - Google Patents
一种Cu/OCN复合催化臭氧分解材料及其制备方法与应用 Download PDFInfo
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Abstract
本发明属催化技术领域,涉及一种Cu/OCN复合催化臭氧分解材料及其制备方法与应用。所述Cu/OCN复合催化臭氧分解材料包括Cu原子和OCN;所述Cu原子均匀地负载在OCN上;其中,所述Cu/OCN结构为单层片状。本发明的改性方法包括对g‑C3N4进行氧化剥离制备得到OCN以及Cu负载制备Cu/OCN。Cu/OCN样品主体部分为OCN,为层状物质,Cu原子均匀地负载在OCN上。与石墨相g‑C3N4相比,Cu/OCN结构细碎,呈单层片状,比表面积较大,Cu成功负载在OCN上,有助于充分与被催化物质接触,增强催化效果。
Description
技术领域
本发明属催化技术领域,涉及一种Cu/OCN复合催化臭氧分解材料及其制备方法与应用。
背景技术
充当“保护伞”的臭氧位于平流层,而臭氧污染位于对流层,尤其是贴近人们的近地层,这类污染主要源于人类活动的间接排放。城市生活中,机动车尾气,化石燃料的燃烧,工业生产,都会产生氮氧化合物。挥发性有机物的来源就更多了,汽车喷涂,印刷厂油墨挥发,加油站油气挥发,化工行业生产过程,溶液使用等都有影响。虽然来源充分,但从氮氧化合物和挥发性有机物生成臭氧是需要特定气象条件的。据大气办监测数据分析,一年中,夏秋两季臭氧浓度较高,因为,温度升高,太阳辐射增强,是臭氧生成的重要条件,这两种物质会发生一系列的光化学反应,迅速生成臭氧,达到甚至超过污染水平。
对流层的臭氧对人体有很大影响,臭氧会刺激和损害眼睛、呼吸系统等粘膜组织,对人体健康产生负面作用。此外,臭氧对金属及大部分非金属具有强烈的腐蚀作用,会间接的影响一些仪器的精密度,一些生活用品的提前报废等等。
臭氧催化分解是一种新型的臭氧污染处理技术,现今分解臭氧的催化剂有金属氧化物催化剂,负载型催化剂及碳质材料催化剂。金属氧化物催化剂是指以金属氧化物为主要催化活性组分的催化剂,其催化效率的高低取决于金属催化剂的选取及其制备工艺。把主催化剂、助催化剂负载在载体上所制成的催化剂称为负载型催化剂。负载型催化剂的载体,其物理结构和性质往往对催化剂性能有决定性的影响。碳质材料催化臭氧氧化体系具有除污性能强、臭氧利用率高和无金属溶出的特点,应用广泛。但随着循环使用次数的增加,碳表面的碱性基团不断消耗,酚羟基、羧基和羰基等酸性含氧基团持续累积,石墨层电子密度降低,从而降低体系的催化能力。与传统催化剂相比,g-C3N4改性后负载金属原子具有更好的催化效果,且g-C3N4易制得,该催化剂金属利用率高,成本低,污染小,具有广泛的应用价值。
发明内容
针对现有技术的不足,本发明提供一种Cu/OCN复合催化臭氧分解材料及其制备方法与应用,本发明的改性方法包括对g-C3N4进行氧化制备得到OCN以及Cu负载制备Cu/OCN。Cu/OCN样品主体部分为OCN,为层状物质,Cu原子均匀地负载在OCN上。与石墨相g-C3N4相比,Cu/OCN结构细碎,呈单层片状,比表面积较大,Cu成功负载在OCN上,有助于充分与被催化物质接触,增强催化效果。
为实现以上目的,本发明通过以下技术方案予以实现:
一种Cu/OCN复合催化臭氧分解材料,所述Cu原子均匀地负载在OCN上;其中,所述Cu/OCN结构为单层片状。
一种Cu/OCN复合催化臭氧分解材料的制备方法,包括以下步骤:
(1)OCN晶体的制备:将石墨相g- C3N4研磨处理并备用;将所述石墨相g-C3N4加入双氧水中并加热处理,使黄色混合液变色为橙棕色混合液;将橙棕色混合液缓慢加入蒸馏水中,冷却至室温,取出后离心分离,取出沉淀物A,依次经过洗涤、真空干燥后得到O-g-C3N4,即得OCN;
(2)Cu/OCN复合催化臭氧分解材料的制备:将步骤(1)所得的OCN和Cu(NO3)2以0.25wt%~20wt%的质量比Cu(NO3)2混合并溶解于去离子水中,搅拌处理后得混合液;向混合液中加入硼氢化钠并搅拌处理,取出后离心分离,取出沉淀物B,依次经过洗涤、放置于冷冻干燥机中干燥、充分研磨,得到Cu/OCN。
优选地,所述步骤(1)和所述步骤(2)中洗涤用的溶剂均为无水乙醇和超纯水,其中,先用无水乙醇洗涤4次,后用超纯水洗涤四次。
优选地,所述步骤(1)中加热处理温度为90℃,加热处理时间为24h。
本发明所述的Cu/OCN复合催化臭氧分解材料作为催化剂应用于处理空气中的污染物臭氧。
与现有技术相比,本发明具有以下有益效果:
(1)本发明制备工艺简单、条件温和、稳定性好、成本低廉,具有催化效率高、环保节能、无毒无污染等突出优点,符合环境友好要求,具有广泛的运用前景;
(2)通过本发明的制备方法制备的复合催化材料Cu/OCN样品孔隙较多,结构较为蓬松,主体部分为OCN,为层状物质,Cu原子均匀地负载在OCN上。与石墨相g-C3N4相比,Cu/OCN结构细碎,呈层状粉末状,质地轻盈,比表面积较大,Cu成功负载在OCN上,可以充分与被催化物质接触,增强催化效果;
(3)g-C3N4氧化后负载微量Cu,催化剂的性能显著提高。臭氧去除率提高显著,几乎达到100%。可见,Cu/OCN催化分解对空气污染物臭氧的处理具有潜在的应用价值。
附图说明
图1是实施例1制备的 g-C3N4、0-C3N4、0.5Cu-O-C3N4、20Cu-O-C3N4的X射线粉末衍射图;
图2是实施例1制备的0.5Cu/OCN的透射电镜图(TEM);
图3是实施例1中个物质的元素映射图(EDS);
图4是常温下Cu/OCN、Cu/CN催化分解浓度40ppm臭氧的效果图。
具体实施方式
下面通过具体实施方式对本发明作进一步详细说明。但本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限定本发明的范围。实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件按照说明书进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。实施例 1
一种Cu/OCN复合催化臭氧分解材料的制备方法,包括以下步骤:
(1)OCN晶体的制备:称取10g石墨相g-C3N4,仔细研磨,放置备用。将10g石墨相g-C3N4加入200ml双氧水中,90℃加热24h,使黄色混合液变色为橙棕色混合液。将溶液缓慢加入300ml蒸馏水中,冷却至室温,取出后离心分离,取出棕黄色沉淀物,用无水乙醇和超纯水各洗4次。置于真空干燥箱中,真空干燥10h,得到O-g-C3N4,即得OCN;
(2)Cu/OCN复合催化臭氧分解材料的制备:将步骤(1)中所述的OCN和Cu(NO3)2以0.5wt%、2wt%、5wt%、20wt%的质量比Cu(NO3)2混合,并溶解于100ml的去离子水中,搅拌16h。向混合液中加入适量硼氢化钠(硼氢化钠溶于水以缓慢速度滴入混合液中,速度为1ml/min),搅拌18h。取出后离心分离,取出沉淀物,用无水乙醇和超纯水各洗4次,放置于冷冻干燥机中干燥。取出后,充分研磨,得到Cu/OCN。
图1为 g-C3N4、0-C3N4、0.5Cu-O-C3N4、20Cu-O-C3N4的X射线粉末衍射图,从图1可知:0.5Cu-O-C3N4的XRD中无铜和铜氧化物种的特征峰,且13°左右的峰相对于0-C3N4变弱,可知铜是以掺杂的形式进入了氮化碳的晶格中。20Cu-O-C3N4中有Cu单质的峰说明了铜添加量的增多导致了Cu单质的团聚形成了Cu晶体。
图2为 0.5Cu-O-C3N4 OCN的透射电镜图(TEM),从图2可知,所述OCN晶体厚度均匀超薄,Cu/OCN结构蓬松。Cu/OCN主体部分为OCN,为层状物质,其表面未见Cu或者CuOx颗粒存在。
图3为 0.5Cu-O-C3N4的元素映射图(EDS),通过元素映射表征,Cu以非常分散的形式存在Cu原子均匀地负载在OCN上。与石墨相g-C3N4相比,Cu/OCN结构细碎,呈层状粉末状,质地轻盈,比表面积较大,Cu成功负载在OCN上,可以充分与被催化物质接触,增强催化效果。其次氧化过的C3N4存在更多的缺陷,O3可以选择性地攻击缺陷和活性部位,诱发一系列的链式反应(EQs),可以提高O的吸附效率和传质效率。
本实施例制备的Cu/OCN常温处理空气污染物臭氧的去除率见图4。
催化分解臭氧性能评价:在常温下,催化剂投加量为100mg条件下,其中,反应条件如下:臭氧浓度为40ppm,空速为600L∙L-1∙h-1;湿度25%;Cu掺杂量为0.5wt%制备的Cu/OCN催化性能达到最佳。由图4可知,Cu/OCN常温处理空气污染物臭氧的效果明显。
以上所述的具体实施例,对本发明的目的、技术方案和有益效果进行了进一步详细说明,所应理解的是,以上所述仅为本发明的具体实施例而已,并不用于限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种Cu/OCN复合催化臭氧分解材料,其特征在于,所述Cu原子均匀地负载在OCN上;其中,所述Cu/OCN结构为单层片状。
2.根据权利要求1所述的一种Cu/OCN复合催化臭氧分解材料的制备方法,其特征在于,包括以下步骤:
(1)OCN晶体的制备:将石墨相g- C3N4研磨处理并备用;将所述石墨相g-C3N4加入双氧水中并加热处理,使黄色混合液变色为橙棕色混合液;将橙棕色混合液缓慢加入蒸馏水中,冷却至室温,取出后离心分离,取出沉淀物A,依次经过洗涤、真空干燥后得到O-g-C3N4,即得OCN;
(2)Cu/OCN复合催化臭氧分解材料的制备:将步骤(1)所得的OCN和Cu(NO3)2以0.5wt%~20wt%的质量比Cu(NO3)2混合并溶解于去离子水中,搅拌处理后得混合液;向混合液中加入硼氢化钠并搅拌处理,取出后离心分离,取出沉淀物B,依次经过洗涤、放置于冷冻干燥机中干燥、充分研磨,得到Cu/OCN。
3.根据权利要求2所述的一种Cu/OCN复合催化臭氧分解材料的制备方法,其特征在于,所述步骤(1)和所述步骤(2)中洗涤用的溶剂均为无水乙醇和超纯水,其中,先用无水乙醇洗涤4次,后用超纯水洗涤四次。
4.根据权利要求2所述的一种Cu/OCN复合催化臭氧分解材料的制备方法,其特征在于,所述步骤(1)中加热处理温度为90℃,加热处理时间为24h。
5.权利要求1所述的一种Cu/OCN复合催化臭氧分解材料作为催化剂应用于处理空气中的污染物臭氧。
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