CN115055160A - 一种用于双吸附硫化氢与甲硫醇活性炭的制备方法 - Google Patents
一种用于双吸附硫化氢与甲硫醇活性炭的制备方法 Download PDFInfo
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Abstract
本发明涉及恶臭气体吸附技术领域,具体涉及一种用于双吸附硫化氢与甲硫醇的活性炭及制备方法。本发明以椰壳为碳源,将预处理后的椰壳粉末与碱性助剂进行高温碳化得炭化料,将炭化料在高锰酸钾溶液中浸渍活化,制备得到用于同时吸附硫化氢和甲硫醇的活性炭。本发明提供的制备方法操作简便,原料获取容易,可工业生产。制备得到的活性炭比表面积增大,表面碱性基团增加,饱和硫容量更高,对于填埋气中的主要恶臭组分无机硫(硫化氢)和有机硫(甲硫醇)能有良好的共吸附作用。
Description
技术领域
本发明涉及恶臭气体吸附技术领域,具体涉及一种用于双吸附硫化氢与甲硫醇活性炭的制备方法。
背景技术
随着工业发展水平不断提高,恶臭污染也随着排放的增加而日趋严重。垃圾处理场所产生的大气污染物主要为挥发性有机物,其中的硫化物恶臭气体对人体健康存在危害。近年来,由于社会经济的发展和环境保护的加强,垃圾场的建设越来越多,社会对恶臭污染物的处理要求也越来越多,如何有效去除垃圾填埋场周围的空气恶臭污染物,成为广泛关注的热点问题。
填埋场挥发出来的恶臭气体中常同时存在硫化氢和甲硫醇等有害物,对周边环境造成恶劣的影响,而现有的处理手段往往是通过使用活性炭与分子筛等吸附剂同时发挥吸附作用,活性炭具有发达的孔隙结构、较大的比表面积和丰富的表面化学基团,是一类特异性吸附能力较强的炭材料,其表面化学改性的性质也有利于对填埋气中特定恶臭组分的定向吸附,并降低对其他组分的吸附。但是目前市面上的改性活性炭通常只对其中一种气体有较好的吸附效果,要吸附多种气体只能将多种改性活性炭组合使用,从而会提高成本,因此需要开发一种能够同时对无机硫和有机硫有效吸附的活性炭材料。
发明内容
为了克服上述现有技术的不足,本发明的目的是提供一种用于双吸附硫化氢与甲硫醇活性炭的制备方法,本发明采用碱性助剂和高锰酸钾改性活性炭的方法,制备得到的活性炭比表面积增大,表面碱性基团增加,饱和硫容量更高,对于填埋气中的主要恶臭组分无机硫(硫化氢)和有机硫(甲硫醇)能有良好的共吸附作用。
为了实现上述目的,本发明所采用的技术方案是:
本发明提供了一种用于双吸附硫化氢与甲硫醇活性炭的制备方法,该方法包括以下步骤:
S1、将预处理后的椰壳粉末与碱性助剂混合后,在保护气体气氛下进行高温炭化反应,得到炭化料;
S2、将炭化料在KMnO4溶液中浸渍4~8h得到用于双吸附硫化氢和甲硫醇的活性炭吸附剂。
优选地,步骤1中,所述预处理为将椰壳粉末浸于水中,后升温至100~120℃搅拌300~400min,过滤烘干后得到预处理后的椰壳粉末。
优选地,步骤1中,所述碱性助剂包括为KHCO3、NaHCO3、CH3COOK、CH3COONa的至少一种。进一步地,碱性助剂为KHCO3。
优选地,步骤1中,所述椰壳粉末的粒径小于0.85mm。
优选地,步骤1中,椰壳粉末与碱性助剂的混合质量比为(1~4):1。进一步地,椰壳粉末与碱性助剂的混合质量比为(1~2):1。
优选地,步骤1中,所述高温炭化反应的详细步骤为以升温速率3~5℃/min,升温至300~350℃反应1~2h;然后以升温速率1~3℃/min,升温至750~850℃反应2~3h。进一步地,所述高温炭化反应的详细步骤为以升温速率3℃/min,升温至300℃反应1h;然后以升温速率1℃/min,升温至750℃反应2h。
优选地,步骤1中,所述保护气体为N2或CO2。进一步地,所述保护气体为CO2。
优选地,步骤2中,浸渍的KMnO4的质量浓度为0.5~7%。
优选地,步骤2中,浸渍后进行洗涤干燥。
本发明还提供了采用上述的制备方法制备得到的种用于双吸附硫化氢与甲硫醇活性炭,所述生物炭应用于吸附硫。所述生物炭应用于特定吸附硫化氢与甲硫醇。
与现有技术相比,本发明的有益效果是:
本发明提供了一种用于双吸附硫化氢与甲硫醇活性炭的制备方法,采用椰壳粉末与碳酸氢钠共同高温炭化的方法,碳酸氢钠高温分解生成碳酸钠、水汽和二氧化碳,碳酸钠可以提高对无机硫的吸附效率,水汽和二氧化碳则有助于提升生物炭的孔隙率,进一步升温可增大比表面积和丰富孔隙;采用高锰酸钾溶液浸渍能增加碱性位点,提高对有机硫的吸附效率;经过改性的活性炭比表面积增大,表面碱性基团增加,饱和硫容量更高,对于填埋气中的主要恶臭组分无机硫(硫化氢)和有机硫(甲硫醇)能有良好的共吸附作用。
附图说明
图1为生物炭的电镜扫描图,其中a为C5;b为C6;c为C3。
具体实施方式
下面对本发明的具体实施方式作进一步说明。在此需要说明的是,对于这些实施方式的说明用于帮助理解本发明,但并不构成对本发明的限定。此外,下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
下述实施例中的实验方法,如无特殊说明,均为常规方法,下述实施例中所用的试验材料,如无特殊说明,均为可通过常规的商业途径购买得到。
实施例1改性活性炭C1的制备
(1)将20g椰壳进行烘干,用配备了20目筛网的锤磨机研磨得到粒径小于0.85mm的椰壳粉末;
(2)预处理:将椰壳粉末浸于去离子水中,升温至110℃后连续搅拌350min,过滤后烘干得到预处理后的椰壳粉末;
(3)将10g预处理后的椰壳粉末与99%纯度的KHCO3固体粉末按质量比为1:1的比例混合,置于管式炉中,在通入流量为50ml/min的氮气气氛下炭化,以3℃/min的升温速率升到300℃后反应1h,然后以1℃/min的升温速率升到750℃后反应2小时,后冷却至室温得到炭化料;
(4)将5g炭化料置于100ml的质量浓度为1%的KMnO4溶液中,在25℃下搅拌浸渍6h;
(5)将浸渍后的炭化料用去离子水进行抽滤洗涤至滤液为中性,放入干燥箱中在100℃条件下干燥10h,制备得到改性活性炭,记作C1。
实施例2改性活性炭C2的制备
制备方法同实施例1,与实施例1不同的是,椰壳粉末与99%纯度的KHCO3固体粉末按质量比为4:1的比例混合,制备得到改性活性炭,记为C2。
实施例3改性活性炭C3的制备
制备方法同实施例1,与实施例1不同的是,炭化采用的保护气体为二氧化碳,制备得到改性活性炭,记为C3。
实施例4改性活性炭C4的制备
制备方法同实施例1,与实施例1不同的是,KMnO4溶液的浓度为0.5%,制备得到改性活性炭,记为C4。
对比例1改性活性炭C5的制备
制备方法同实施例1,与实施例1不同的是,没有添加KHCO3固体粉末,制备得到活性炭,记为C5。
对比例2改性活性炭C6的制备
制备方法同实施例1,与实施例1不同的是,没有浸渍在高锰酸钾溶液,制备得到活性炭,记为C6。
实施例1改性生物炭的结构表征和组合吸附剂的吸附能力测试
(1)结构表征
对C1~C6进行电镜扫描分析,扫描图如图1所示,从图中观察到C5的表面的孔隙分布不均匀;而C6的表面形态相对平坦无孔;C3的表面具有丰富的孔隙结构,且C1、C2和C4的电镜扫描结果与C3相同。
对C1~C6采用全自动比表面积与孔径分析仪测定活性炭的比表面积、孔容和孔径分布,不同生物炭的比表面积和孔容如表1所示:
表1不同生物炭的比表面积和孔容表征结果
从表1得出,通过对比C3与C1发现炭化过程中通入二氧化碳比通氮气的比表面积与孔容都大幅提高;通过对比C1、C2和C4发现减少KHCO3助剂量和减少KMnO4浸渍量后比表面积与孔容下降;C5在炭化时不加入碱性助剂后没有热解二氧化碳,比表面积与孔容都大幅降低;C6不进行KMnO4浸渍后比表面积与孔容降低,表明KHCO3助剂量和KMnO4浸渍量与比表面积与孔容正相关,而且二氧化碳能增加生物炭的比表面积与孔容。
(2)生物炭的吸附能力测试
对C1~C6进行硫化氢和甲硫醇的双吸附性能测试:在常温状态下,使用质量流量控制计以300ml/min的气体流量将混合气通过装有5g活性炭的吸附剂床层,混合气体为3000ppm的硫化氢和1000ppm甲硫醇的混合气,在出口处采用气相色谱仪测得出口硫化氢和甲硫醇的浓度,根据下列公式计算脱硫化氢效率和脱甲硫醇效率:
脱硫化氢效率=(入口硫化氢浓度-出口硫化氢浓度)/入口硫化氢浓度×100%;
脱甲硫醇效率=(入口甲硫醇浓度-出口甲硫醇浓度)/入口甲硫醇浓度×100%。
各生物炭的脱硫化氢和甲硫醇效率如如表2所示:
表2不同生物炭的脱硫化氢和甲硫醇效率
C1 | C2 | C3 | C4 | C5 | C6 | |
出口硫化氢浓度(ppm) | 804 | 885 | 726 | 846 | 1485 | 852 |
出口甲硫醇浓度(ppm) | 319 | 346 | 274 | 333 | 326 | 579 |
脱硫化氢效率(%) | 72.3% | 70.5% | 75.8% | 71.8% | 50.5% | 71.6% |
脱甲硫醇效率(%) | 68.1% | 65.4% | 72.6% | 66.7% | 67.4% | 42.1% |
从表2得出,通过对比C3与C1发现炭化过程中通入二氧化碳比通氮气的脱硫化氢和甲硫醇效率提高;通过对比C1、C2和C4发现减少KHCO3助剂量和减少KMnO4浸渍量后脱硫化氢和甲硫醇效率下降;C5在炭化时不加入碱性助剂后脱硫化氢效率大幅下降,脱甲硫醇效率影响不大;C6不进行KMnO4浸渍后脱甲硫醇效率大幅下降,脱硫化氢效率影响不大,表明经碱性助剂和高锰酸钾改性后,活性炭能够实现良好的共吸附硫化氢和甲硫醇作用,且对比发现通入二氧化碳炭化反应能提高吸附效率和提高饱和硫容量。
综上所述,本发明将椰壳粉末与碳酸氢钠在保护气体气氛下高温炭化,使生物炭比表面积增大和孔隙丰富,提高对无机硫硫化氢的吸附效率,且通入二氧化碳炭化更有助于提高生物炭性能;用高锰酸钾溶液浸渍增加碱性位点,提高对有机硫甲硫醇的吸附;经过改性的活性炭对硫化氢和甲硫醇能够实现良好的共吸附作用,且饱和硫容量更高,能同时特定吸附两种含硫组分(硫化氢和甲硫醇),降低吸附成本。
以上对本发明的实施方式作了详细说明,但本发明不限于所描述的实施方式。对于本领域的技术人员而言,在不脱离本发明原理和精神的情况下,对这些实施方式进行多种变化、修改、替换和变型,仍落入本发明的保护范围内。
Claims (8)
1.一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,包括以下步骤:
S1、将预处理后的椰壳粉末与碱性助剂混合后,在保护气体气氛下进行高温炭化反应,得到炭化料;
S2、将炭化料在KMnO4溶液中浸渍4~8h得到用于双吸附硫化氢和甲硫醇的活性炭吸附剂。
2.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤1中,所述预处理为将椰壳粉末浸于水中,后升温至100~120℃搅拌300~400min,过滤烘干后得到预处理后的椰壳粉末。
3.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤1中,所述椰壳粉末的粒径小于0.85mm。
4.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤1中,椰壳粉末与碱性助剂的混合质量比为(1~4):1。
5.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤1中,所述碱性助剂为KHCO3、NaHCO3、CH3COOK、CH3COONa的至少一种。
6.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤1中,所述高温炭化反应的详细步骤为以升温速率3~5℃/min,升温至300~350℃反应1~2h;然后以升温速率1~3℃/min,升温至750~850℃反应2~3h。
7.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤1中,所述保护气体为N2或CO2。
8.根据权利要求1的一种用于双吸附硫化氢和甲硫醇的活性炭吸附剂的制备方法,其特征在于,步骤2中,KMnO4的质量浓度为0.5~7%。
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