CN114682213A - 一种用于吸附氨气的阻燃型活性炭及其制备方法 - Google Patents
一种用于吸附氨气的阻燃型活性炭及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于吸附氨气的阻燃型活性炭及其制备方法,对活性炭首先进行高温处理后,减少表面易氧化的含氧基团,再通过浸渍法将离子液体负载到活性炭上,除去过量溶剂后得到阻燃型活性炭。本发明制备的阻燃型活性炭,有效抑制了在热空气法再生过程中活性炭的氧化放热,降低了因局部过热导致的着火风险,同时具有氨吸附性能良好、制备方法简便、易于工业化等优点。
Description
【技术领域】
本发明涉及一种阻燃型活性炭及其制备方法,特别是涉及一种具有良好氨吸附性能的阻燃型活性炭及其制备方法。
【背景技术】
活性炭因其较大的比表面积和发达的孔隙结构,具有较强的吸附能力,被广泛应用于污水处理、工业尾气净化等方面,如处理含油废水、VOC、脱硫脱硝等。活性炭表面官能团的种类和数量,对其与极性或非极性吸附质相互作用有重要影响。因此,对活性炭进行改性大大增加了其在各个领域的应用价值。常见的改性技术有酸改性、碱改性、负载改性、高温重整改性等。
活性炭的再生方式包括:热再生、超生波再生、微波再生和生物再生等。其中,工业上应用最广泛、最成熟的是热再生,包括热蒸汽再生和热空气再生。由于氨极易溶于水,因此采用热蒸汽加热的方式进行再生会产生大量的氨氮废水,造成二次污染;使用热空气再生时,对于解吸气可以采用与原料气并入净化系统的方式进行处理,相比热蒸汽再生更为环保。因此,热空气法更适合氨吸附工艺中活性炭的再生。
现有活性炭在制备成型过程不可避免地会引入含氧官能团,如酚羟基、内酯基、羧基、羰基等。在净化含氨尾气方面,通过酸改性进一步增加含氧官能团的数量以提高氨吸附量是较为常用的方法。但在热空气法再生过程中,这些含氧官能团会加速活性炭在空气中的氧化,放出大量的热,热量累积可能造成火灾事故。为了降低活性炭的着火风险,并保持良好的氨吸附性能,本发明提供了用于吸附氨气的阻燃型活性炭的制备方法。公开号为CN1517146A的专利在活性炭中加入了阻燃剂,当达到一定温度时阻燃剂分解吸收热量,进而降低温度,达到阻燃效果。但该活性炭并不具备选择性吸附氨气的能力,不适用于净化含氨尾气。本发明所提供的阻燃型活性炭,采用不同的阻燃机理,即抑制活性炭的氧化放热,达到阻燃效果,同时具有良好的氨吸附性能。公开号为CN104162409A的专利对活性炭进行了酸改性,公开号为CN104368307A的专利则是对活性炭进行酸处理后,负载了金属氯化物。酸改性是提高活性炭氨吸附量的常用方法,但并不具备阻燃作用。相反地,酸处理会增加含氧官能团的数量,增加了活性炭在工业应用过程中的着火风险。同时酸改性易造成设备的腐蚀,因其不易分解,再生时还需要更高的温度。本发明所提供的活性炭,除了具有阻燃效果,还通过负载离子液体保持了较高的氨吸附量,相比酸改性更加绿色、环保。公开号为CN110064365A的专利通过将离子液体负载到活性炭上,活性炭的燃点提高了30℃左右,但该活性炭仅适用于吸附有机废气。本发明采用不同的制备工艺、离子液体和阻燃机理,制备了适用于吸附氨气的阻燃型活性炭。
基于离子液体具有难挥发、不易燃、结构可控等优点,在气体吸收和分离纯化等方面得到广泛应用。通过设计离子液体的结构,可以高效地选择性分离混合气体中的氨气。将这类离子液体负载到活性炭上,可以提高活性炭的氨吸附能力。
本发明提供的制备方法对活性炭进行了高温活化处理,并将离子液体负载到活性炭上。由于活性炭表面的含氧基团减少,有效抑制了碳氧化,达到了阻燃的目的;而离子液体的存在则保持了活性炭对氨的吸附能力,满足了工业应用的要求。
【发明内容】
针对活性炭在热空气再生过程中存在着火风险的问题,本发明旨在提供一种具有阻燃效果且氨吸附量较高的活性炭及其制备方法。
本发明选用木质活性炭、椰壳活性炭或煤质活性炭,先对活性炭进行高温处理,再通过浸渍法将离子液体负载到活性炭上,除去过量溶剂后得到用于吸附氨气的阻燃型活性炭。
具体地,本发明通过以下实施例方案实现:
本发明提供的制备方法为:将活性炭进行高温处理后,取一定量干燥后的离子液体溶解于有机溶剂中,缓慢加入一定量活化后的活性炭,室温下搅拌2~48 h。除去过量的溶剂后,真空干燥2~24h,得到负载离子液体的阻燃型活性炭。
本发明所述的离子液体的特征为:阳离子为含有质子氢的烷基咪唑阳离子,如1-丁基咪唑阳离子、1-乙基咪唑阳离子;或含有羟基的季铵类阳离子,如体 N,N-二甲基乙醇铵阳离子。阴离子为含F、O、N的单核阴离子,如硝酸根、氟硼酸根、六氟磷酸根。
本发明所述的有机溶剂的特征为:甲醇、乙醇、异丙醇中的一种或几种的复配溶剂。
本发明的有益效果是:
(1)本发明提供的阻燃型活性炭有效抑制了热空气再生过程中自身的氧化放热,避免了局部过热导致的着火危险。同时,在贮藏和运输过程中,大大降低了活性炭与空气接触后自燃的危险性;
(2)本发明提供的阻燃型活性炭具有较高的氨吸附量;
(3)本发明采用的焙烧法、浸渍法操作简便,原料价格低廉,所需设备简单,成本较低且易于工业化。
因此,本发明所提供的阻燃型活性炭,在热空气再生过程中的安全性高,避免了火灾事故的发生;同时其吸附性能能够满足净化含氨尾气的要求,制备方法较为简单。
【具体实施方式】
下面结合具体实例进一步阐述本发明。
实施例1:
在400℃、氮气气氛下,将活性炭在管式炉中焙烧12h。取1g[Bim]NO3溶解在35mL乙醇中,缓慢加入9g焙烧后的活性炭,室温下搅拌24h。80℃旋蒸2h,转速40rpm,压力10kpa。除去大量乙醇后,80℃真空干燥24h,真空度 -90kpa,得到负载量10wt%的阻燃型活性炭1。
实施例2:
在400℃、氮气气氛下,将活性炭在管式炉中焙烧12h。取1g[Eim]NO3溶解在35mL乙醇中,缓慢加入9g焙烧后的活性炭,室温下搅拌24h。80℃旋蒸2h,转速40rpm,压力10kpa。除去大量乙醇后,80℃真空干燥24h,真空度 -90kpa,得到负载量10wt%的阻燃型活性炭2。
通过DSC(差示扫描量热法)对不同活性炭进行测试,测试条件:空气气氛,空气气速50mL/min,升温速率10℃/min,测试温度25℃~160℃,观察有无放热峰出现,结果见附图2;通过U型管对负载前后活性炭的氨吸附量进行评价(如附图3),测试方法为称重法,测试条件:30℃水浴,氨气气速50mL/min,评价结果见附图4、表1。
DSC结果表明,3种活性炭在120℃前均出现不同大小的吸热峰,主要是由于部分未除尽的水脱附造成的。当温度继续升高,改性前活性炭出现明显的放热迹象,说明空气气氛下活性炭表面基团被氧化并放出热量;改性后活性炭的曲线则相对平稳,说明自身氧化得到有效的抑制。
评价结果表明,改性后活性炭的氨吸附量明显高于改性前,吸附饱和时间无明显滞后,氨吸附效果良好。
表1负载前后活性炭的氨吸附量评价结果
【附图说明】
附图1是阻燃型活性炭的制备流程图。
附图2是不同活性炭的DSC测试结果。
附图3是活性炭的氨吸附量评价装置图。
附图4是不同活性炭的穿透曲线评价结果。
Claims (10)
1.一种用于吸附氨气的阻燃型活性炭及其制备方法,对活性炭进行高温处理后,通过浸渍法将离子液体负载到活性炭上,除去过量溶剂后真空干燥,最终得到阻燃型活性炭。本发明制备的阻燃型活性炭,有效抑制了在热空气法再生过程中活性炭的氧化放热,降低了因局部过热导致的着火风险,同时具有氨吸附性能良好、制备方法简便、易于工业化等优点。
2.如权利要求1所述的制备方法为:将活性炭进行高温处理后,取一定量干燥后的离子液体溶解于有机溶剂中,缓慢加入一定量处理后的活性炭,室温下搅拌2~48h。除去过量的溶剂后,真空干燥2~24h,得到负载离子液体的阻燃型活性炭。
3.如权利要求1所述的高温处理为:惰性气氛下,如氮气、氦气、氩气等,300℃~800℃焙烧2~24h。
4.如权利要求1所述的离子液体和活性炭的质量比为1:1.5至1:9。
5.如权利要求1所述的活性炭和有机溶剂的质量比为1:3至1:5。
6.如权利要求1所述的除去过量溶剂的方法为:80~100℃旋转蒸发1~6h,转速10~100rpm,压力10kpa~100kpa。
7.如权利要求1所述的真空干燥的温度为:80~120℃,压力10kpa~100kpa。
8.如权利要求1所述的活性炭的特征为:木质活性炭、椰壳活性炭或煤质活性炭。
9.如权利要求1所述的离子液体的特征为:阳离子为含有质子氢的烷基咪唑阳离子,如1-丁基咪唑阳离子、1-乙基咪唑阳离子;或含有羟基的季铵类阳离子,如N,N-二甲基乙醇铵阳离子。阴离子为含F、O、N的单核阴离子,如硝酸根、氟硼酸根、六氟磷酸根。
10.如权利要求1所述的有机溶剂特征为:甲醇、乙醇、异丙醇中的一种或几种的复配溶剂。
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