CN115475604A - 一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法 - Google Patents
一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法 Download PDFInfo
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Abstract
本发明为解决目前传统生物质活性炭吸附性能单一、吸附效率低的问题,提出一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法。制造方法具有软木活性炭制备、软木活性炭氧化处理、氨基碳量子点制备、复合多功能吸附剂制备的步骤。本发明效益是:本发明的制造方法生产出的复合多功能吸附剂具有均匀的蜂窝状结构、超薄的碳纳米片壁层、高比表面积、良好的层级多孔结构、丰富的氨基官能团和含氧官能团,为多类污染物的高效吸附提供了良好的结构和表面化学基础;该多功能吸附剂对重金属离子和有机染料具有多类型、高效吸附性能,具体表现为高吸附容量、快吸附速度以及优异的再生性能。
Description
技术领域
本发明涉及一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法。
背景技术
工业的快速发展造成了各种污染物的大量排放,由此产生的水污染已经成为一个日益严重的世界性环境问题。许多技术已被开发用于处理含重金属离子和染料的废水,如吸附、膜过滤、离子交换、高级氧化等。其中,吸附法具有效率高、成本低、操作简单、无二次污染的特点,被认为是最有潜力的废水处理途径。目前,已有一系列用于水处理的吸附剂,包括有机聚合物、沸石、粘土、金属有机骨架等。然而,以上材料往往具有性能单一、成本高、吸附效率低、不可再生、不可生物降解等缺点,从而阻碍了其广泛应用。因此,开发一种可持续的、环保的、高效的多功能吸附剂以净化环境废水具有重要意义。
活性炭具有物化稳定性高、比表面积大、孔结构优良、制备简便等优点,是目前最具潜力也是应用最广泛的吸附剂。由于经济、可再生、资源丰富等特点,木材、竹材、椰壳、秸秆等生物质被广泛用于制备活性炭。然而,大多数生物质具有无序的孔隙结构和复杂的化学组成,不利于其在热解过程中的微观结构发展,从而限制了生物质基活性炭对污染物的高效吸附。探索具有高结构均一性的新型生物质碳前体和适宜的活化策略是获得高性能活性炭的关键。
未改性的活性炭对高浓度金属离子的吸附性能往往不理想,具体表现为吸附容量低以及吸附选择性差,引入特定官能团是提高活性炭对金属离子吸附性能的有效策略。
发明内容
本发明为解决现有活性炭吸附技术中存在的一系列缺陷,从而提出一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,如附图1所示。本发明制备得到的复合多功能吸附剂对重金属离子和有机染料均表现出优异的吸附性能,包括高吸附容量、快吸附速度以及良好的再生性能。
所述的制造方法中包括以下步骤:
步骤一、软木活性炭制备:采用两步热解活化法制备软木活性炭;
步骤二、软木活性炭预处理:利用硝酸对软木活性炭进行氧化处理;
步骤三、氨基碳量子点制备:采用水热法制备氨基修饰的碳量子点;
步骤四、将步骤二中氧化处理的软木活性炭置于一定浓度氨基碳量子点溶液中,搅拌反应;悬浮液过滤,取固体产物烘干,最终得到基于软木活性炭及氨基碳量子点的复合多功能吸附。
进一步,步骤一中软木活性炭制备方法如下:将软木原料研磨过筛;将筛分后的软木粉末置于真空管式热解炉中,在氮气氛围下热解炭化,待冷却至室温后取出固体产物,为软木生物炭;将软木生物炭与固体KOH混合,后将混合物置于真空管式热解炉中,在氮气氛围下加热活化,待冷却至室温后取出固体产物,用盐酸溶液及蒸馏水清洗产物至中性pH,烘干得到软木活性炭。
进一步,所述热解炭化工艺为:升温速率10℃/min,热解温度450-750℃,保温时间0.5-2.0h;所述加热活化工艺为:软木生物炭与KOH质量比1:3-5,升温速率10℃/min,活化温度650-850℃,保温时间0.5-2.0h。
进一步,步骤二中软木活性炭预处理过程如下:将软木活性炭置于硝酸溶液中,室温下搅拌混合均匀;将混合物置于水热反应釜中,加热反应,冷却后取出固体产物,用蒸馏水清洗并烘干得到氧化软木活性炭。
进一步,所述硝酸溶液浓度为3-5M,加热反应温度为120℃,保温时间为2h。
进一步,步骤三中氨基碳量子点制备方法如下:将柠檬酸与支化聚乙烯亚胺置于蒸馏水中,室温下搅拌混合均匀;将混合溶液置于水热反应釜中,加热反应,冷却至室温后,反应溶液经透析和冷冻干燥得到氨基碳量子点。
进一步,所述柠檬酸与支化聚乙烯亚胺施加比为1:3,加热反应温度为180℃,保温时间为6h。
进一步,步骤四中复合多功能吸附剂制备方法如下:将氧化软木活性炭、N-羟基琥珀醯亚胺、N-羟基硫代琥珀醯亚胺置于醋酸缓冲液中,室温下搅拌均匀;将10ml的氨基碳量子点溶液加入上述混合液,40℃搅拌反应,固体产物经蒸馏水清洗、烘干,最终得到复合多功能吸附剂。
进一步,所述氨基碳量子点溶液浓度为0.1-4wt%,40℃搅拌反应时间为12h。
与目前现有技术相比,本发明有益效果在于:经过本发明的制造方法生产出的基于软木活性炭和氨基碳量子点的复合多功能吸附剂具有均匀的蜂窝状结构、超薄的碳纳米片壁层、高比表面积、良好的层级多孔结构、丰富的活性官能团,为多类型污染物的高效吸附提供了良好的结构及表面化学基础;该多功能吸附剂对重金属离子和有机染料均具有较高的吸附容量和吸附速度,优于许多其他类型吸附剂;此外,该多功能吸附剂还具有良好的再生性能、高的物化稳定性以及优异的生物相容性,展现出巨大的工业化应用潜力。
附图说明
附图1是本发明基于软木活性炭及氨基碳量子点的复合多功能吸附剂的制备工艺流程图;
具体实施方式
下面结合实施案例对本发明作进一步描述和说明,但并不因此而限定本发明的保护范围。
实施案例:
一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,包括以下步骤:
步骤一、软木活性炭制备:将软木颗粒研磨过筛,取40-60目备用;将软木颗粒置于真空管式热解炉中,在300ml/min氮气流氛围下,以10℃/min的升温速率由室温升至550℃,保温1h,待冷却至室温后取出固体产物,即为软木生物炭;将软木生物炭与固体KOH以质量比1:5混合,利用研钵充分研磨,后将混合物置于真空管式热解炉中,在300ml/min氮气流氛围下,以10℃/min的升温速率由室温升至850℃,保温2h,待冷却至室温后取出固体产物,用0.1M盐酸溶液及蒸馏水清洗产物至中性pH,80℃烘干得到软木活性炭;
步骤二、软木活性炭氧化处理:将0.2g软木活性炭置于60ml的5M硝酸溶液中,室温下搅拌混合均匀;将混合物置于水热反应釜中,120℃反应2h,冷却后取出固体产物,用蒸馏水清洗至中性pH,80℃烘干得到氧化活性炭;
步骤三、氨基碳量子点制备:将1g柠檬酸和3g支化聚乙烯亚胺置于25ml蒸馏水中,室温下搅拌混合均匀;将混合溶液置于水热反应釜中,180℃反应6h;冷却至室温后,反应溶液用蒸馏水透析2天,冷冻干燥得到氨基碳量子点;
步骤四、基于软木活性炭及氨基碳量子点的复合多功能吸附剂制备:将0.2g硝酸氧化活性炭、0.24gN-羟基琥珀醯亚胺、0.06gN-羟基硫代琥珀醯亚胺置于pH=3的醋酸缓冲液中,室温下搅拌1h;将10ml0.1%wt的氨基碳量子点溶液加入上述混合液,40℃搅拌反应12h;固体产物用蒸馏水清洗,80℃烘干得到复合多功能吸附剂。
本实施案例的效果是:制造的复合多功能吸附剂具有蓬松的蜂窝状结构,超薄的碳纳米片壁层(~200nm),高比表面积(1088.97m2/g),良好的层级多孔结构,丰富的氨基和含氧基团;多功能吸附剂独特的结构和表面化学性质使其对Pb(Ⅱ)(231.48mg/g,10min)和RhB(1734.55mg/g,180min)均具有较高的吸附容量和吸附速度;此外,其还表现出良好的再生性能,连续5次吸附-解吸循环后,对Pb(Ⅱ)和RhB的再吸收效率分别达到82%和70%。
以上所述仅是本发明的优选实施方式,本发明的保护范围并不仅限于上述实施案例。凡属于发明思路下的技术方案均属于本发明的保护范围。应该指出,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的改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,包括以下步骤:
步骤一、软木活性炭制备:采用两步热解活化法制备软木活性炭;
步骤二、软木活性炭预处理:利用硝酸对软木活性炭进行氧化处理;
步骤三、氨基碳量子点制备:采用水热法制备氨基修饰的碳量子点;
步骤四、将步骤二中氧化处理的软木活性炭置于一定浓度氨基碳量子点溶液中,搅拌反应;悬浮液过滤,取固体产物烘干,最终得到基于软木活性炭及氨基碳量子点的复合多功能吸附。
2.根据权利要求1所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,步骤一中活性炭制备方法如下:将软木原料研磨过筛;将筛分后的软木粉末置于真空管式热解炉中,在氮气氛围下热解炭化,待冷却至室温后取出固体产物,为软木生物炭;将软木生物炭与固体KOH混合,后将混合物置于真空管式热解炉中,在氮气氛围下加热活化,待冷却至室温后取出固体产物,用盐酸溶液及蒸馏水清洗产物至中性pH,烘干得到软木活性炭。
3.根据权利要求2所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,热解炭化工艺为:升温速率10℃/min,热解温度450-750℃,保温时间0.5-2.0h;所述加热活化工艺为:软木生物炭与KOH质量比1:3-5,升温速率10℃/min,活化温度650-850℃,保温时间0.5-2.0h。
4.根据权利要求1所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,步骤二中软木活性炭氧化处理过程如下:将软木活性炭置于硝酸溶液中,室温下搅拌混合均匀;将混合物置于水热反应釜中,加热反应,冷却后取出固体产物,用蒸馏水清洗并烘干得到氧化软木活性炭。
5.根据权利要求4所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,硝酸浓度为3-5M,加热温度120℃,反应时间2h。
6.根据权利要求1所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,步骤三中氨基碳量子点制备方法如下:将柠檬酸与支化聚乙烯亚胺置于蒸馏水中,室温下搅拌混合均匀;将混合溶液置于水热反应釜中,加热反应,冷却至室温后,反应溶液经透析和冷冻干燥得到氨基碳量子点。
7.根据权利要求6所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,柠檬酸与支化聚乙烯亚胺施加比为1:3,加热温度180℃,反应时间6h。
8.根据权利要求1所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,步骤四中复合多功能吸附剂制备方法如下:将氧化软木活性炭、N-羟基琥珀醯亚胺、N-羟基硫代琥珀醯亚胺置于醋酸缓冲液中,室温下搅拌均匀;将10ml的氨基碳量子点溶液加入上述混合液,40℃搅拌反应,固体产物经蒸馏水清洗、烘干,最终得到复合多功能吸附剂。
9.根据权利要求8所述一种基于软木活性炭及氨基碳量子点的复合多功能吸附剂制造方法,其特征在于,氨基碳量子点溶液浓度为0.1-4wt%,40℃搅拌反应12h。
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