CN109455715B - 一种石墨烯改性的憎水活性炭的制备方法 - Google Patents
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Abstract
本发明提出一种石墨烯改性的憎水活性炭的制备方法,包括以下步骤:将果壳粉末与ZnCl2‑HCl溶液混合均匀;加入石墨烯,同时加入自制分散剂,所述自制分散剂为聚乙烯吡咯烷酮和木质素磺酸钠的混合水溶液,在超声仪中超声30‑60min,使得石墨烯与果壳粉末混合均匀并均匀地分散在溶液中,反应、干燥,之后研磨、压片、碳化;碳化结束后冷却至室温,用蒸馏水多次洗涤样品至产物呈中性,干燥后即得石墨烯改性的憎水活性炭。本发明的制备方法制得的石墨烯改性的憎水活性炭吸水率低且导热系数是普通商业活性炭的3‑5倍。
Description
技术领域
本发明涉及一种石墨烯改性的憎水活性炭的制备方法。
背景技术
活性炭因具有发达的空隙结构和巨大的比表面积,在挥发性有机气体(VOCs)及其它环境污染物处理方面占有非常重要的地位,但在应用中也仍存在一些难以解决的难题。普通的活性炭因其活化过程中,活性炭表面会产生一些亲水性的基团,导致活性炭具有一定的亲水性,这就会导致在湿度较大的环境中活性炭对VOCs等有机污染物的吸附能力大大降低。因此适当提高活性炭的憎水性对于增加活性炭的应用范围具有十分重要的意义。
发明内容
本发明的目的在于提出一种石墨烯改性的憎水活性炭的制备方法,制得的石墨烯改性的憎水活性炭吸水率低且导热系数是普通商业活性炭的3-5倍。
本发明提出一种石墨烯改性的憎水活性炭的制备方法,包括以下步骤:
S1、将硬质果壳清洗干净、晾干,用粉碎机粉碎、过筛得到200目以下的果壳粉末;
S2、将果壳粉末与ZnCl2-HCl溶液混合均匀,其中ZnCl2的添加量为果壳粉末质量的1-4倍;加入果壳粉末质量的5%-50%的石墨烯,同时加入自制分散剂,所述自制分散剂为聚乙烯吡咯烷酮和木质素磺酸钠的混合水溶液,聚乙烯吡咯烷酮和木质素磺酸钠的总添加量为果壳粉末质量的0.05%-0.5%,其中,聚乙烯吡咯烷酮和木质素磺酸钠的质量比为4:1-4:3;在超声仪中超声30-60min,使得石墨烯与果壳粉末混合均匀并均匀地分散在溶液中,然后将混合溶液在60-80℃搅拌反应3h,待反应结束后将反应产物干燥;
S3、随后将干燥后的混合物进行研磨、压片,装进耐高温的器皿内置于节能管式炉中进行碳化;
S4、碳化结束后冷却至室温,用蒸馏水多次洗涤样品至产物呈中性,干燥后即得石墨烯改性的憎水活性炭。
进一步的,所述的ZnCl2-HCl溶液的浓度为0.1-0.5g/mL。
进一步的,所述的自制分散剂的浓度为5g/L。
进一步的,S3所述的碳化的条件如下:由室温以4-10℃/min的速率升温至400~750℃,并维持4h~8h,此过程一直通入氮气。
进一步的,所述的硬质果壳包括椰子壳、杏核壳、核桃壳、桃壳。
本发明的有益效果:
1、在活化过程中通过加入石墨烯对活性炭进行改性,制得的活性炭憎水性增加,可保证在湿度较大的环境下,活性炭不会因为吸附水而降低对VOCs的吸附效率。
2、由于石墨烯在ZnCl2-HCl溶液不易分散,制备过程中加入了自制分散剂,自制分散剂是浓度为5g/L的聚乙烯吡咯烷酮(PVP)和木质素磺酸钠(SLS)混合溶液,能使石墨烯能够均匀的分散在活性炭中。
3、所制得憎水性活性炭,其导热系数是普通商业活性炭的3-5倍,有利于其再生并能保证在较高温度下吸附床和脱附床的传热性。
具体实施方式
如下结合具体实施例,对本申请方案作进一步描述:
实施例1
一种石墨烯改性的憎水活性炭的制备方法,包括以下步骤:
S1、将硬质果壳清洗干净、晾干,用粉碎机粉碎、过筛得到200目以下的果壳粉末;所述硬质果壳包括椰子壳、杏核壳、核桃壳、桃壳。
S2、称取100克果壳粉末与350mL浓度为0.3g/mL的ZnCl2-HCl溶液混合均匀,加入30克的石墨烯,同时加入20mL自制分散剂,所述自制分散剂为聚乙烯吡咯烷酮(PVP)和木质素磺酸钠(SLS)混合溶液,浓度为5g/L,混合溶液中的聚乙烯吡咯烷酮和木质素磺酸钠的质量比为4:1;在超声仪中超声30-60min,使得石墨烯与果壳粉末混合均匀并均匀地分散在溶液中,然后将混合溶液在60-80℃搅拌反应3h,待反应结束后将反应产物干燥。
S3、随后将干燥后的反应产物进行研磨、压片,装进耐高温的器皿内置于节能管式炉中进行碳化;由室温以4-10℃/min的速率升温至650℃,并维持4h~8h,此过程一直通入氮气。
S4、碳化结束后冷却至室温,用蒸馏水多次洗涤样品至产物呈中性,干燥后即得石墨烯改性的憎水活性炭。
实施例2
一种石墨烯改性的憎水活性炭的制备方法,包括以下步骤:
S1、将硬质果壳清洗干净、晾干,用粉碎机粉碎、过筛得到200目以下的果壳粉末;所述硬质果壳包括椰子壳、杏核壳、核桃壳、桃壳。
S2、称取100克果壳粉末与600mL浓度为0.5g/mL的ZnCl2-HCl溶液混合均匀,加入20克的石墨烯,同时加入20mL自制分散剂,所述自制分散剂为PVP和木质素磺酸钠(SLS)混合溶液,浓度为5g/L,混合溶液中的聚乙烯吡咯烷酮和木质素磺酸钠的质量比为4:3;在超声仪中超声30-60min,使得石墨烯与果壳粉末混合均匀并均匀地分散在溶液中,然后将混合溶液在60-80℃搅拌反应3h,待反应结束后将反应产物干燥。
S3、随后将干燥后的反应产物进行研磨、压片,装进耐高温的器皿内置于节能管式炉中进行碳化;由室温以4-10℃/min的速率升温至600℃,并维持4h~8h,此过程一直通入氮气。
S4、碳化结束后冷却至室温,用蒸馏水多次洗涤样品至产物呈中性,干燥后即得石墨烯改性的憎水活性炭。
实施例3
一种石墨烯改性的憎水活性炭的制备方法,包括以下步骤:
S1、将硬质果壳清洗干净、晾干,用粉碎机粉碎、过筛得到200目以下的果壳粉末;所述硬质果壳包括椰子壳、杏核壳、核桃壳、桃壳。
S2、称取100克果壳粉末与1000mL浓度为0.2g/mL的ZnCl2-HCl溶液混合均匀,加入10克的石墨烯,同时加入10mL自制分散剂,所述自制分散剂为PVP和木质素磺酸钠(SLS)混合溶液,浓度为5g/L,混合溶液中的聚乙烯吡咯烷酮和木质素磺酸钠的质量比为4:2;在超声仪中超声30-60min,使得石墨烯与果壳粉末混合均匀并均匀地分散在溶液中,然后将混合溶液在60-80℃搅拌反应3h,待反应结束后将反应产物干燥。
S3、随后将干燥后的反应产物进行研磨、压片,装进耐高温的器皿内置于节能管式炉中进行碳化;由室温以4-10℃/min的速率升温至400~750℃,并维持4h~8h,此过程一直通入氮气。
S4、碳化结束后冷却至室温,用蒸馏水多次洗涤样品至产物呈中性,干燥后即得石墨烯改性的憎水活性炭。
将上述实施例1-3制得的石墨烯改性的憎水活性炭进行测试,结果如下表:
上述实施例1-3制得的憎水活性炭吸水率较市售的商品活性炭大大降低,即憎水性增加,可保证在湿度较大的环境下,活性炭不会因为吸附水而降低对VOCs的吸附效率。此外,上述实施例所制得憎水活性炭,其导热系数是普通商业活性炭的3-5倍,有利于其再生并能保证在较高温度下吸附床和脱附床的传热性。
上述优选实施方式应视为本申请方案实施方式的举例说明,凡与本申请方案雷同、近似或以此为基础作出的技术推演、替换、改进等,均应视为本专利的保护范围。
Claims (4)
1.一种石墨烯改性的憎水活性炭的制备方法,其特征在于,包括以下步骤:
S1、将硬质果壳清洗干净、晾干,用粉碎机粉碎、过筛得到200目以下的果壳粉末;
S2、将果壳粉末与ZnCl2-HCl溶液混合均匀,其中ZnCl2的添加量为果壳粉末质量的1-4倍;加入果壳粉末质量的5%-50%的石墨烯,同时加入自制分散剂,所述自制分散剂为聚乙烯吡咯烷酮和木质素磺酸钠的混合水溶液,聚乙烯吡咯烷酮和木质素磺酸钠的总添加量为果壳粉末质量的0.05%-0.5%,其中,聚乙烯吡咯烷酮和木质素磺酸钠的质量比为4:1-4:3;在超声仪中超声30-60min,使得石墨烯与果壳粉末混合均匀并均匀地分散在溶液中,然后将混合溶液在60-80℃搅拌反应3h,待反应结束后将反应产物干燥;
S3、随后将干燥后的混合物进行研磨、压片,装进耐高温的器皿内置于节能管式炉中进行碳化,碳化的条件如下:由室温以4-10℃/min的速率升温至400~750℃,并维持4h~8h,此过程一直通入氮气;
S4、碳化结束后冷却至室温,用蒸馏水多次洗涤样品至产物呈中性,干燥后即得石墨烯改性的憎水活性炭。
2.根据权利要求1所述的石墨烯改性的憎水活性炭的制备方法,其特征在于,所述的ZnCl2-HCl溶液的浓度为0.1-0.5g/mL。
3.根据权利要求1所述的石墨烯改性的憎水活性炭的制备方法,其特征在于,所述的自制分散剂的浓度为5g/L。
4.根据权利要求1所述的石墨烯改性的憎水活性炭的制备方法,其特征在于,所述的硬质果壳包括椰子壳、杏核壳、核桃壳、桃壳。
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