CN109502583A - 一种改性活性炭的制备方法 - Google Patents

一种改性活性炭的制备方法 Download PDF

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CN109502583A
CN109502583A CN201811445764.6A CN201811445764A CN109502583A CN 109502583 A CN109502583 A CN 109502583A CN 201811445764 A CN201811445764 A CN 201811445764A CN 109502583 A CN109502583 A CN 109502583A
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黄宇
彭仕琪
朱丹丹
赵全喜
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Jiangsu Zhongke Ruina Environmental Technology Co.,Ltd.
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Abstract

本发明公开了一种改性活性炭的制备方法，通过有机酸和过渡金属离子两步改性法，制备出的活性炭表面羧基基团增多，使过渡金属离子与活性炭表面结合力加强，有效改善金属离子分散性；同时羧基的还原性，可将金属离子还原为金属单质或低价态金属离子，显著提高其对低浓度甲苯的吸附性能。本发明操作流程简单，成本低，可制成活性炭滤芯等防护产品推广应用。

Description

一种改性活性炭的制备方法
技术领域
本发明涉及挥发性有机气体处理技术领域，尤其涉及一种改性活性炭的制备方法。
背景技术
挥发性有机化合物(VOCs)是普遍存在于室内外环境空气中的污染物，主要来源于工业过程及机动车排放的有机废气。其中，甲苯因其有毒、反应活性高、易致癌及易诱发基因突变等特性，近年来引发人们的广泛关注。目前，处理VOCs最常见的方法是吸附法，尤其是处理环境中低浓度的VOCs。活性炭吸附法因其成本低、效率高被证明为较适宜的有机气体处理方法。目前较为常用的活性炭改性方法为无机酸/碱、有机酸、负载过渡元素金属离子或微波改性等。活性炭的制备条件、孔隙度、表面化学性质决定了活性炭对有机气体的吸附性能。
有机酸改性可以提高活性炭表面的酸性含氧基团，对甲醛及其他挥发性有机气体的吸附具有明显的改善作用；单一过渡金属改性也可以提高活性炭对甲苯的单位吸附量，但操作步骤繁琐，且能耗较高，工业化生产难度大。将两种改性方法相结合是一种提高活性炭吸附甲苯的行之有效的方法。
发明内容
本发明主要提供一种结合有机酸以及过渡金属两种方式的改性活性炭的制备方法，制备的改性活性炭对低浓度甲苯具有较高的吸附性能。
一种改性活性炭的制备方法，包括以下步骤：
S1将活性炭用去离子水洗涤至上清液澄清，使活性炭表面杂质被充分去除，然后置于干燥箱中进行干燥，得到预处理的活性炭；
S2将S1预处理后的活性炭置于有机酸溶液中，在恒温水浴振荡器中进行振荡，之后用去离子水进行清洗，最后进行真空干燥，得到有机酸处理过的活性炭；
S3将步骤S2经有机酸处理过的活性炭置于过渡金属盐溶液中，在恒温水浴振荡器中进行振荡，之后用去离子水进行清洗，最后进行真空干燥，即得改性活性炭。
进一步具体的，所述S2中有机酸为草酸、柠檬酸、马来酸、富马酸、琥珀酸或酒石酸中的其中一种。
进一步具体的，所述S3中过渡金属盐为钴盐、铁盐、铜盐或锰盐中的其中一种，同时所述的过渡金属盐为氯盐。
进一步具体的，所述S1中干燥箱的温度控制在80～100℃，时间控制在20h～28h。
进一步具体的，所述S2以及S3中恒温水浴振荡器的温度为50～70℃，振荡频率为90～110r/min，振荡时间为2～4h。
进一步具体的，所述S2以及S3中真空干燥温度为70～90℃，时间控制在20h～28h。
进一步具体的，所述的有机酸溶液浓度为0.5mol/L，所述有机酸溶液与活性炭的液固比是8:1～16:1。
进一步具体的，所述的过渡金属盐溶液，其浓度为0.5～1mol/L；所述过渡金属盐溶液与活性炭的液固比是8:1～16:1。
本发明提供了一种改性活性炭的制备方法，制备出的活性炭表面羧基基团增多，通过羧基配位作用，使过渡金属离子与活性炭表面结合力加强，有效改善金属离子分散性；同时羧基的还原性可将金属离子还原为金属单质或低价态金属离子，显著提高其对低浓度甲苯的吸附性能；且所得改性活性炭孔隙结构发达，比表面积为312.4m2/g，总孔容为0.05cm3/g，平均孔径为3.3nm，对低浓度甲苯具有较高的吸附性能，操作流程简单，成本较低，适用场合广泛，可制成活性炭滤芯等防护产品推广应用。
附图说明
图1为本发明改性活性炭和未改性活性炭的扫描电镜图。
图2为本发明改性活性炭和未改性活性炭的N2吸附等温曲线。
图3为本发明改性活性炭和未改性活性炭的甲苯消除效果图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细的说明。
将活性炭用去离子水洗涤3～5次至上清液澄清，使活性炭表面杂质被充分去除，然后置于80～100℃的干燥箱中时间控制在20h～28h，优选地，所述干燥箱的温度为80℃，时间为24h，得到预处理的活性炭。
根据有机酸溶液与活性炭的液固比8:1～16:1，将预处理后的活性炭置于0.5mol/L的有机酸溶液中，优选地，有机酸为草酸、柠檬酸、马来酸、富马酸、琥珀酸或酒石酸中的其中一种，在50～70℃的恒温水浴振荡器中以90～110r/min振荡2h～4h后，用去离子水洗涤5次，最后70～90℃真空干燥20～28h，优选地，有机酸溶液与活性炭的液固比为16:1，恒温水浴振荡器温度为60℃，震荡频率为110r/min，震荡时间为2h，真空干燥温度为80℃，干燥时间为24h。
根据过渡金属盐溶液与活性炭液固比8:1～16:1，将经有机酸处理过的活性炭置于过渡金属盐溶液中，优选地，过渡金属盐为钴盐、铁盐、铜盐或锰盐中的其中一种，且为氯盐，过渡金属盐溶液浓度为0.5～1mol/L。在50～70℃恒温水浴振荡器中以90～110r/min振荡2h～4h后，用去离子水洗涤5次，最后70～90℃真空干燥20～28h，优选地，过渡金属盐溶液与活性炭液固比为16:1，恒温水浴振荡器温度为60℃，震荡频率为110r/min，震荡时间为2h，真空干燥温度为80℃，干燥时间为24h，即得改性活性炭。
实施例：
将活性炭用去离子水洗涤3～5次至上清液澄清，使活性炭表面杂质被充分去除，然后置于80℃的干燥箱中24h，得到预处理的活性炭；根据有机酸溶液与活性炭的液固比16:1，将预处理后的活性炭置于0.5mol/L的草酸溶液中，在60℃的恒温水浴振荡器中以110r/min振荡2h后，用去离子水洗涤5次，最后80℃真空干燥24h；根据过渡金属盐溶液与活性炭液固比16:1，将经有机酸处理过的活性炭置于0.5mol/L氯化锰溶液中，在60℃恒温水浴振荡器中以110r/min振荡2h后，用去离子水洗涤5次，最后80℃真空干燥24h，即得改性活性炭。
下面给出具体的实验分析。
(1)形貌分析
图1为改性活性炭(a)和未改性活性炭(b)的扫描电镜图，通过扫描电镜对活性炭进行形貌表征，可以看出改性活性炭保留了原有活性炭的大孔道结构，在改性活性炭表面可以检测到含量很高的锰元素。
(2)孔结构分析
通过全自动比表面积及孔隙分析仪对活性炭进行孔结构分析，从而得到相应的比表面积、孔径分布、孔容等信息(表1)。图2是改性活性炭和未改性活性炭对N2的吸附等温曲线，分析结果可知，改性活性炭样品的孔径增大，比表面积和孔容减小。
表1比表面积及孔径分布表
(3)甲苯吸附实验及结果
图3为改性活性炭和未改性活性炭的甲苯消除效果图(测试条件：温度25℃，甲苯初始浓度为270ppb，气体流量为1L/min，改性/未改性活性炭用量0.1g)，从中可以看出，采用有机酸和负载过渡金属离子两步改性法得到的改性活性炭对甲苯具有较高的去除能力。将两步改性法得到的改性活性炭与传统的无机酸/碱、有机酸或过渡金属离子改性活性炭进行比较，我们采用类似的方法制备了HNO3、NaOH、有机酸以及过渡金属离子改性活性炭，并对其甲苯吸附性能进行研究，如表2所示，可以明显看出，两步改性法得到的改性活性炭对甲苯具有最高的去除能力，表明采用有机酸和负载过渡金属离子两步改性法，可以显著提高活性炭对甲苯的吸附性能。
表2不同方法制备的改性活性炭对甲苯的去除率
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种改性活性炭的制备方法，其特征在于：该方法包括以下步骤：
S1将活性炭用去离子水洗涤至上清液澄清，使活性炭表面杂质被充分去除，然后置于干燥箱中进行干燥，得到预处理的活性炭；
S2将S1预处理后的活性炭置于有机酸溶液中，在恒温水浴振荡器中进行振荡，之后用去离子水进行清洗，最后进行真空干燥，得到有机酸处理过的活性炭；
S3将S2经有机酸处理过的活性炭置于过渡金属盐溶液中，在恒温水浴振荡器中进行振荡，之后用去离子水进行清洗，最后进行真空干燥，即得改性活性炭。
2.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述S2中有机酸为草酸、柠檬酸、马来酸、富马酸、琥珀酸或酒石酸中的其中一种。
3.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述S3中过渡金属盐为钴盐、铁盐、铜盐或锰盐中的其中一种，同时所述的过渡金属盐为氯盐。
4.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述S1中干燥箱的温度控制在80～100℃，时间控制在20h～28h。
5.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述S2以及S3中恒温水浴振荡器的温度为50～70℃，振荡频率为90～110r/min，振荡时间为2～4h。
6.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述S2以及S3中真空干燥温度为70～90℃，时间控制在20h～28h。
7.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述的有机酸溶液浓度为0.5mol/L。
8.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述有机酸溶液与活性炭的液固比是8:1～16:1。
9.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述的过渡金属盐溶液，其浓度为0.5～1mol/L。
10.根据权利要求1所述的改性活性炭的制备方法，其特征在于：所述过渡金属盐溶液与活性炭的液固比是8:1～16:1。
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