CN106268719A - 一种负载四氧化三铁微粒的改性活性炭制备方法 - Google Patents
一种负载四氧化三铁微粒的改性活性炭制备方法 Download PDFInfo
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Abstract
本发明涉及一种负载四氧化三铁微粒的改性活性炭制备方法,属于资源综合利用技术领域。将FeCl2、FeCl3和固体NaOH混合均匀,然后在氮气气氛中微波加热至温度为180~220℃进行焙烧熔融50~90min,熔融结束后冷却至50℃得到熔融液;向熔融液中依次加入十二烷基苯磺酸钠、以紫茎泽兰原料制备的活性炭混合均匀,在温度为40℃、超声波辅助条件下进行负载,负载结束后加入热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭。本发明制备得到的负载四氧化三铁微粒的改性活性炭性能较好,碘吸附值能到达1100~2200mg/g。
Description
技术领域
本发明涉及一种负载四氧化三铁微粒的改性活性炭制备方法,属于资源综合利用技术领域。
背景技术
四氧化三铁,俗称氧化铁黑、磁铁、吸铁石、黑铁,为具有磁性的黑色晶体,故又称为磁性氧化铁。此物质溶于酸溶液,不溶于水、碱溶液及乙醇、乙醚等有机溶剂。通常用作颜料和抛光物质,也可用于制造录音磁带和电讯器材。传统制备四氧化三铁颗粒的方法主要有沉淀法、水热(溶剂热)法、微乳化法、溶胶-凝胶法,而新兴的制备方法诸如微波法、热解羰基前躯体法、超声法、空气氧化法、热解-还原法、多元醇还原法等因极具发展前景从而已经成为学者们研究的热点。在制备四氧化三铁颗粒或者对其改性负载的过程中,新型的表面活性剂、制备体系也都有所突破,其中表面活性剂例如SDS(十二烷基苯磺酸钠)、PEG(聚乙二醇)、CTAB(十六烷基三甲基溴化铵)、柠檬酸、油酸等被应用广泛,制备体系也相继出现乙醇-水体系、正丙醇-水、丙二醇-水体系等。
活性炭作为炭材料中性能优良的多孔介质的一种,已经被广泛地应用于诸多的工业领域,例如气相与液相的分离、纯化,废水、废气、废染料的吸附处理,做各种催化剂的载体,或者因其优良的导电性能而作为超级电容器等。随着人类社会的发展,活性炭的应用范围越来越广泛,需求量也越来越大,针对不同领域的研究,要求活性炭具有相应的吸附性能,这就对活性炭吸附性能的要求也越来越高,而单纯由原材料制备的多孔活性炭,很难满足于特定领域的特定处理,针对这样的现象,研究者们将其他具有相应功能但又因其自身结构条件限制而无法独立应用的有机物或者无机物通过某种手段负载于活性炭表面,从而使得活性炭性能有了极大的飞跃。针对废水废气中各种金属离子的吸收,本发明所制备的改性活性炭均可进行有效吸附。
本发明以紫茎泽兰作原料制备的原活性炭含碳量高,孔结构分布均匀,负载四氧化三铁颗粒后并不影响其结构性能,相反的这种改性活性炭的吸附性能更加优越专一,从而避免了活性炭泛而吸收不精的现象。由于微波焙烧熔融四氧化三铁颗粒的过程中有产物水蒸气生成,随着后续裂解,反应会朝着逆方向进行从而对熔融过程不利,故在此过程中通入氮气以保持平衡分压,提高反应效率。改性后的活性炭比表面积和未改性的活性炭比表面积差别不大,孔结构也相似,只是在活性炭表面上增加了四氧化三铁颗粒,这种具有磁性的被负载质对废水中各种金属回收利用极为有利。本发明所使用的未改性活性炭比表面积位2587m2/g,改性后活性炭比表面积2443 m2/g,相比较而言,后者比表面积有稍微的降低,这是因为有些许四氧化三铁颗粒进入了活性炭孔洞所致,也从侧面说明成功负载四氧化三铁颗粒为有效吸附废水中各种金属离子这一突出环境问题提供了一个切实可行的方法。
申请人在专利号为200910273073.7的专利里,公开了一种“微波法制备四氧化三铁纳米片的方法”,这种方法是以采用可溶性三价铁盐为原材料,用乙二醇配置成铁盐溶液,往其中加入醋酸钠和表面活性剂,搅拌均匀后利用微波辐照生成四氧化三铁,产物经过滤和洗涤后空气中常温干燥即得到四氧化三铁纳米片材料。上述发明与本发明相比,上述方法采用乙二醇溶解铁盐的过程并无其他辅助操作流程,因为乙二醇能与金属作用形成的醇盐是一元醇盐,如将此醇盐(例如乙二醇一钠)在氢气流中加热到180~200℃则可形成乙二醇二钠,而本实验采用简单的二价和三价铁盐的碱化,直接在200℃下微波加热进行熔盐裂解,从而避免了上述辅助操作;
申请人在专利号为201510792930.X的专利里,公开了一种 “改性活性炭负载铈吸附剂的制备方法”,这种方法包括以下步骤:(1)将粒径0.27~0.83mm的颗粒椰壳活性炭用去离子水洗涤多次;(2)放入干燥箱于110℃下干燥12h,记作AC;(3)分别用一定浓度的HCl,HNO3,H2O2,NH3·H2O对AC进行表面氧化改性,洗涤至中性。上述发明与本发明相比:上述方法采用酸碱逐一对活性炭进行表面改性,流程繁琐,且改性过程中未对氨气做回收处理;而本发明通过添加表面活性剂十二烷基苯磺酸钠,充分利用超声波准确的声能来对活性炭进行均匀负载,同样达到了精准的负载效果。
发明内容
针对上述现有技术存在的问题及不足,本发明提供一种负载四氧化三铁微粒的改性活性炭制备方法。本发明制备得到的负载四氧化三铁微粒的改性活性炭性能较好,碘吸附值能到达1100~2200mg/g。本发明通过以下技术方案实现。
一种负载四氧化三铁微粒的改性活性炭制备方法,包括以下具体步骤:
(1)将FeCl2、FeCl3和固体NaOH按照摩尔比为1:1:4~6混合均匀,然后在氮气气氛中微波加热至温度为180~220℃进行焙烧熔融,熔融结束后冷却至50℃得到熔融液;
(2)步骤(1)得到的熔融液,按照质量比为10~30:10~30:50~150依次加入十二烷基苯磺酸钠、以紫茎泽兰原料制备的活性炭混合均匀,在温度为40℃、超声波辅助条件下进行负载,负载结束后加入热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭.
所述步骤(2)中超声波功率为300~600W。
所述步骤(2)中离心振荡器转速为300r/min。
所述步骤(2)中真空干燥箱真空度为0.005~0.01MPa。
本发明的有益效果是:
(1)本方法选取的负载基体活性炭是通过活化外来入侵物种紫茎泽兰而得到的,从而该活性炭生产成本低廉,即负载基体的成本不高,这就为改性提供了必要的可能性;
(2)本方法采用微波加热焙烧碱化的二价和三价铁盐,一步到位制备了四氧化三铁颗粒的离子液体,选择裂解温度200℃,高温对阴阳离子晶格的损坏,也使后续缓慢冷却更容易;
(3)本方法采取通入氮气的方式,以氮气的平衡分压维持了反应方程的平衡,并使其尽量朝着生成四氧化三铁的方向进行;
(4)本方法采取蒸馏水对制备的改性活性炭进行多次洗涤,可使部分熔融的氯化钠溶解;
(5)本方法采取超声波辅助常温负载,充分利用了其方向性和穿透性;
(6)本方法采取真空干燥避免了改性活性炭在干燥过程中的氧化,从而保证了改性活性炭的得率;
(7)目前常规的技术只是致力于如何制备结构优良、吸附性能良好的活性炭,但是对于改性技术的研究并不深远,本方法针对特定被吸附质进行活性炭的改性则具有良好前景。
(8)本方法采取回收利用的原则,回收滤液中氯化钠;
(9)本发明制备得到的负载四氧化三铁微粒的改性活性炭性能较好,碘吸附值能到达1100~2200mg/g。
附图说明
图1是本发明实施例1以紫茎泽兰为原料制备的活性炭FT-IR图;
图2是本发明实施例1制备得到的负载四氧化三铁颗粒的改性活性炭FT-IR图;
图3是本发明实施例1以紫茎泽兰为原料制备的活性炭扫描电镜图;
图4是本发明实施例1制备得到的负载四氧化三铁颗粒的改性活性炭扫描电镜图。
具体实施方式
下面结合附图和具体实施方式,对本发明作进一步说明。
本发明实施例中比表面积采用全自动物理化学吸附仪(Autosorb-1-C,康塔公司)测定,碘吸附值根据国家标准GB/T12496.10-1999测定。
实施例1
该负载四氧化三铁微粒的改性活性炭制备方法,包括以下具体步骤:
(1)将10molFeCl2、FeCl3和固体NaOH按照摩尔比为1:1:5混合均匀,然后在氮气气氛中微波加热至温度为200℃进行焙烧熔融70min,熔融结束后冷却至50℃得到熔融液;
(2)取步骤(1)得到的20g熔融液,按照质量比为20:10:100依次加入十二烷基苯磺酸钠(10g)、以紫茎泽兰原料制备的活性炭(100g),在温度为40℃、超声波辅助条件下进行负载40min,负载结束后加入100ml热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭。其中超声波功率为300W,离心振荡器转速为300r/min,真空干燥箱真空度为0.005MPa。
经上述步骤负载制备得到的负载四氧化三铁微粒的改性活性炭碘吸附值为2146mg/g。
上述以紫茎泽兰原料制备的活性炭FT-IR图如图1所示,制备得到的负载四氧化三铁颗粒的改性活性炭FT-IR图如图2所示,以紫茎泽兰为原料制备的活性炭扫描电镜图如图3所示,负载四氧化三铁颗粒的改性活性炭扫描电镜图如图4所示。从图可以看出改性前后活性炭表面官能团有显著差异,证明已将四氧化三铁微粒负载在改性活性炭上。
实施例2
该负载四氧化三铁微粒的改性活性炭制备方法,包括以下具体步骤:
(1)将10molFeCl2、FeCl3和固体NaOH按照摩尔比为1:1:6混合均匀,然后在氮气气氛中微波加热至温度为220℃进行焙烧熔融90min,熔融结束后冷却至50℃得到熔融液;
(2)取10g步骤(1)得到的熔融液,按照质量比为30:30:150依次加入十二烷基苯磺酸钠、以紫茎泽兰原料制备的活性炭,在温度为40℃、超声波辅助条件下进行负载50min负载结束后加入100ml热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭。其中超声波功率为600W,离心振荡器转速为300r/min,真空干燥箱真空度为0.01MPa。
经上述步骤负载制备得到的负载四氧化三铁微粒的改性活性炭碘吸附值为1753mg/g。
实施例3
该负载四氧化三铁微粒的改性活性炭制备方法,包括以下具体步骤:
(1)将10molFeCl2、FeCl3和固体NaOH按照摩尔比为1:1:4混合均匀,然后在氮气气氛中微波加热至温度为180℃进行焙烧熔融50min,熔融结束后冷却至50℃得到熔融液;
(2)取10g步骤(1)得到的熔融液,按照质量比为10:10:50依次加入十二烷基苯磺酸钠、以紫茎泽兰原料制备的活性炭,在温度为40℃、超声波辅助条件下进行负载30min,负载结束后加入100ml热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭。其中超声波功率为500W,离心振荡器转速为300r/min,真空干燥箱真空度为0.008MPa。
经上述步骤负载制备得到的负载四氧化三铁微粒的改性活性炭碘吸附值为1146mg/g。
实施例4
该负载四氧化三铁微粒的改性活性炭制备方法,包括以下具体步骤:
(1)将10molFeCl2、FeCl3和固体NaOH按照摩尔比为1:1:4.5混合均匀,然后在氮气气氛中微波加热至温度为190℃进行焙烧熔融60min,熔融结束后冷却至50℃得到熔融液;
(2)向步骤(1)得到的熔融液中按照质量比为15:10:100依次加入十二烷基苯磺酸钠、以紫茎泽兰原料制备的活性炭,在温度为20℃、超声波辅助条件下进行负载35min,负载结束后加入100ml热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭。其中超声波功率为400W,离心振荡器转速为300r/min,真空干燥箱真空度为0.006MPa。
经上述步骤负载制备得到的负载四氧化三铁微粒的改性活性炭碘吸附值为1473mg/g。
以上结合附图对本发明的具体实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下做出各种变化。
Claims (4)
1.一种负载四氧化三铁微粒的改性活性炭制备方法,其特征在于包括以下具体步骤:
(1)将FeCl2、FeCl3和固体NaOH按照摩尔比为1:1:4~6混合均匀,然后在氮气气氛中微波加热至温度为180~220℃进行焙烧熔融50~90min,熔融结束后冷却至50℃得到熔融液;
(2)将步骤(1)得到的熔融液,按照质量比为10~30:10~30:50~150依次加入十二烷基苯磺酸钠、以紫茎泽兰原料制备的活性炭混合均匀,在温度为40℃、超声波辅助条件下进行负载30~50min,负载结束后加入热蒸馏水,离心振荡去掉上清液,过滤并将滤渣在真空干燥箱中进行干燥,得到负载四氧化三铁微粒的改性活性炭。
2.根据权利要求1所述的负载四氧化三铁微粒的改性活性炭制备方法,其特征在于:所述步骤(2)中超声波功率为300~600W。
3.根据权利要求1所述的负载四氧化三铁微粒的改性活性炭制备方法,其特征在于:所述步骤(2)中离心振荡器转速为300r/min。
4.根据权利要求1所述的负载四氧化三铁微粒的改性活性炭制备方法,其特征在于:所述步骤(2)中真空干燥箱真空度为0.005~0.01MPa。
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