CN111992236B - 熔融盐热聚合法制备具有光催化氧化硫化氢气体功能的碳氮催化剂及其制备方法和应用 - Google Patents
熔融盐热聚合法制备具有光催化氧化硫化氢气体功能的碳氮催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种熔融盐热聚法合成具有光催化氧化硫化氢气体功能的碳氮催化剂及其制备方法和应用,属于材料制备及催化脱硫的技术领域,其是将碳氮前驱体和LiCl、KCl组成的混合盐混合后进行研磨,再将所得粉末在氮气气氛下进行热处理,即得到所述的功能化碳氮催化剂材料。利用廉价混合熔盐法合成功能化碳氮催化剂材料,能有效的将硫化氢气体氧化成硫单质,并且具有较高的转换效率和选择性。本发明工艺简单,成本低,可大规模生产,符合实际生产需要,有较大的应用潜力。
Description
技术领域
本发明属于材料制备及催化脱硫技术领域,具体涉及一种熔融盐热聚合法合成具有光催化氧化硫化氢气体功能的碳氮催化剂及其制备方法和应用。
背景技术
硫化氢作为一种有腐蚀性的酸性有毒气体,在冶金工业、低温煤焦化、含硫是由开发与提炼以及化学品加工等过程中大量产生。硫化氢的排放不仅对设备造成损害、对环境造成污染,同时对人体也有损害。随着环境保护法对硫化氢的排放要求越来越高,业界迫切需求发展高效、稳定、低成本的处理硫化氢气体的技术手段。
目前工业中传统的处理硫化氢废气方法可分为干法和湿法两大类。干法是以固体氧化剂或吸附剂来脱硫或直接燃烧;湿法则又可以分为液体吸收法和吸收氧化法两种。工业中常用金属氧化物作为催化剂在高温条件下对硫化氢选择性氧化脱除。但由于硫化氢在高温下易与氧气发生过反应而产生二氧化硫等二次污染物,选择性较低;且反应的选择性氧化是放热反应,因此高温条件下硫化氢的选择性氧化热力学上受到抑制,难以将硫化氢降解至ppb级别。
光催化技术由于其反应条件温和、选择性好等优势而受到关注。现常用的脱硫光催化剂主要为金属氧化物与金属硫化物,例如TiO2、CdS和ZnS等催化剂,但是其转换率、稳定性等仍具有一定的局限性。因此开发一种制备简单、成本低、效率高并稳定性高的脱硫光催化剂材料具有极其重要的意义。碳氮材料主要由C、N等元素组成,廉价易得,通过化学键合构筑结构性碱中心,稳定性良好,结构组成易于调控,具有可调光响应等优点,使其适宜用作硫化氢的深度净化。
发明内容
本发明的目的在于提供一种熔融盐热聚合法合成具有光催化氧化硫化氢气体功能的碳氮催化剂及其制备方法和应用,本发明制备的碳氮催化剂能够高效地实现H2S气体的光催化氧化,可实现低浓度恶臭气体硫化氢的废气治理资源化,且具有较好的选择性和寿命。本发明工艺简单、成本低、效率高,符合实际生产需要,有较大的应用前景。
为实现上述目的,本发明采用如下技术方案:
一种熔融盐热聚合法制备具有光催化氧化硫化氢气体功能的碳氮催化剂的化学式为C3N4。
进一步地,所述碳氮催化剂的比表面积为 40~70 m2·g-1,半晶态物质,能有效地将硫化氢气体光催化氧化为硫单质。
上述熔融盐热聚合法制备具有光催化氧化硫化氢气体功能的碳氮催化剂的制备方法,将碳氮前驱体置于熔融盐中进行热聚合,生成具有光催化氧化硫化氢气体功能的碳氮催化剂。
进一步地,所述碳氮前驱体包括七嗪、5-氨基四氮唑、三聚氰胺、二聚氰胺、尿素中的一种。
上述制备方法具体包括以下步骤:
(1)将碳氮前驱体放入研钵,加入LiCl和KCl的混合盐,混合后研磨均匀;
(2)将步骤(1)所得混合粉末在氮气气氛下,以2~5 ℃/min的速度升温到450~650℃,热处理2-5h,即得具有光催化氧化硫化氢气体功能的碳氮催化剂。
进一步地,步骤(1)所用碳氮前驱体、混合盐的质量比为1:10~5:10;混合盐中LiCl与KCl的质量比为2:1~2:7。
上述熔融盐热聚合法制备具有光催化氧化硫化氢气体功能的碳氮催化剂可以用于选择性将硫化氢气体氧化为硫磺单质。
本发明的有益效果:
(1)本发明提供了一种一步熔盐热处理制备功能化的碳氮催化剂的方法,其将廉价的混合盐与碳氮前驱体在氮气气氛下一起加热反应,利用熔盐模板制备层状碳氮催化剂材料,产率最高可达到88.3%。
(2)该碳氮催化剂吸收光能生成电子-空穴对,与表面的氧气反应生成活性氧基团,进而高效地将硫化氢气体氧化成硫磺单质,并且具有高转化率和较好的稳定性。
(3)本发明的整个工艺过程简单易控制,能耗低、产率高、成本低,符合实际生产需要,有利于大规模的推广。
附图说明
图1为实施例1所得氮化碳催化剂的XRD(X射线粉末衍射)图;
图2为实施例1所得氮化碳催化剂的SEM(扫描电子显微镜)图;
图3为实施例1所得氮化碳催化剂的TEM(透射电子显微镜)图;
图4为实施例1所得碳氮催化剂PHI与现有氮化碳对硫化氢气体光氧化活性图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
1)分别称取一定量的七嗪与LiCl和KCl质量比为9:11的混合盐,混合均匀;其中,七嗪、混合盐的质量比为1:10;
2)将步骤1)所得混合粉末放入马弗炉中,在惰性气体保护下,以2~5 ℃/min的速度升温到550℃,热处理4h后,自然降温至常温,洗去混合盐后即得碳氮光催化剂。
图1为实施例1所得氮化碳催化剂材料的XRD(X射线粉末衍射)图;由XRD图表明制备的产物为聚七嗪酰亚胺(PHI)结构的氮化碳。其中28.2°处的峰,由层状氮化碳材料堆叠引起,表明层间距为0.316 nm。图2为实施例1所得氮化碳催化剂材料的SEM(扫描电子显微镜)图;从图中可以发现,制备的产物呈珊瑚状。图3为实施例1所得氮化碳催化剂材料的TEM(透射电子显微镜)图;从图中可以发现,制备的产物有较好的结晶。图4为实施例1所得碳氮催化剂PHI与现有氮化碳对硫化氢气体光氧化活性图;在20 ppm硫化氢、10 ppm氧气的混合气中,空速为6000 ml/(h·g)的流速下,现有氮化碳对硫化氢的光催化转化率低于1.8%,PHI对硫化氢的光催化转化率可达到99.9%以上,且不产生二氧化硫,证明了PHI光催化脱硫的高效性;同时在100分钟的反应时间内,硫化氢转化率依然维持在99%以上,证明了PHI光催化脱硫的稳定性。
实施例2
1)分别称取一定量的三聚氰胺与LiCl和KCl质量比为4:7的混合盐,混合均匀;其中,二聚氰胺、混合盐的质量比为2:10;
2)将步骤1)所得混合粉末放入马弗炉中,在惰性气体保护下,以2~5 ℃/min的速度升温到600℃,热处理4h后,自然降温至常温,洗去混合盐后即得碳氮光催化剂。
实施例3
1)分别称取一定量的二聚氰胺与LiCl和KCl质量比为1: 1的混合盐,混合均匀;其中,二聚氰胺、混合盐的质量比为1:10;
2)将步骤1)所得混合粉末放入马弗炉中,在惰性气体保护下,以2~5 ℃/min的速度升温到550℃,热处理4h后,自然降温至常温,洗去混合盐后即得碳氮光催化剂。
实施例4
1)分别称取一定量的5-氨基四氮唑与LiCl和KCl质量比为1:1的混合盐,混合均匀;其中,5-氨基四氮唑、混合盐的质量比为2:10;
2)将步骤1)所得混合粉末放入马弗炉中,在惰性气体保护下,以2~5 ℃/min的速度升温到550℃,热处理3h后,自然降温至常温,洗去混合盐后即得碳氮光催化剂。
实施例5
1)分别称取一定量的尿素与LiCl和KCl质量比为9:11的混合盐,混合均匀;其中,尿素、混合盐的质量比为5:10;
2)将步骤1)所得混合粉末放入马弗炉中,在氮气气氛下,以2~5 ℃/min的速度升温到525℃,热处理2h,即得碳氮催化剂。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (1)
1.一种熔融盐热聚合法制备具有光催化氧化硫化氢气体功能的碳氮催化剂用于将硫化氢气体光催化氧化为硫单质的用途,其特征在于:所述碳氮催化剂的化学式为C3N4;所述碳氮催化剂的比表面积为 40~70 m2·g-1,半晶态物质;
所述碳氮催化剂制备方法包括以下步骤:
(1)将碳氮前驱体放入研钵,加入LiCl和KCl的混合盐,混合后研磨均匀;其中碳氮前驱体为七嗪,所用碳氮前驱体、混合盐的质量比为1~10;混合盐中LiCl与KCl的质量比为9:11;
(2)将步骤(1)所得混合粉末在氮气气氛下,以2~5 ℃/min的速度升温到550℃,热处理2-5h,即得具有光催化氧化硫化氢气体功能的碳氮催化剂。
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