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CN112705166A - 一种氨水改性桉木活性炭吸附剂的制备方法及应用 - Google Patents

一种氨水改性桉木活性炭吸附剂的制备方法及应用 Download PDF

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CN112705166A
CN112705166A CN202110009900.2A CN202110009900A CN112705166A CN 112705166 A CN112705166 A CN 112705166A CN 202110009900 A CN202110009900 A CN 202110009900A CN 112705166 A CN112705166 A CN 112705166A
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eucalyptus
activated carbon
ammonia water
drying
carbon adsorbent
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卢泽
曾惠婷
张康
石清亮
张华�
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Guilin University of Technology
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Abstract

本发明公开了一种氨水改性桉木活性炭吸附剂的制备方法及应用。将桉木粉末浸泡在磷酸溶液中，浸泡后的桉木粉末放置于马弗炉内高温热解、冷却、洗涤；过滤、干燥、研磨过筛，得到桉木活性炭；将所得桉木活性炭，置于乙二醇中，经过超声波处理，再加入氨水，磁力搅拌，所得均一的混合液装入到反应釜中，干燥、冷却、洗涤；过滤、干燥、研磨过筛，得到氨水改性桉木活性炭吸附剂。本发明先采用磷酸活化法制备活性炭，再进行氨水改性，工艺流程简单，条件易行；负载氨基后的复合桉木活性炭相较于原始活性炭，能够通过静电吸附、氢键作用和氧化还原作用，大大增强对水溶液中Cr(VI)的去除能力；所制备吸附剂可广泛应用于工矿企业含Cr(VI)废水的处理工序。

Description

一种氨水改性桉木活性炭吸附剂的制备方法及应用
技术领域
本发明涉及一种氨水改性桉木活性炭吸附剂的制备方法及应用，利用桉木为主要材料，研究了氨水改性桉木活性炭吸附剂的制备方法及其对铬的吸附应用。属于材料制备与水处理领域。
背景技术
随着工业活动的快速发展，大量含有重金属的工业废水被排放到环境中，由于其不可生物降解的特性和潜在的致癌性，引起了严重的环境问题。其中，工业废水中含有的铬是一种主要的有毒污染物。微量的铬就可引起严重的生理或神经损伤。铬主要存在于两种价态:Cr(III)和Cr(VI)，并且Cr(VI)类物质由于毒性大、迁移率高，比Cr(III)类物质的危害性大得多。目前，各种传统或现代技术已被用于处理含Cr(VI)的重金属废水，包括还原，离子交换，反渗透，膜分离，电凝和吸附等方法。在这些方法中，吸附法被认为是一种成本较低、效率较高的处理低浓度重金属污染水的方法。
桉木富含纤维素、半纤维素和木质素，经过热解后会产生多孔结构，有利于对水中Cr(VI)的吸附去除，而且桉木生长周期短，作为制备活性炭的原材料可以有效地降低生产成本。
在无氧条件下对桉木通过热化学裂解生产的活性炭具有多孔结构、表面积、表面官能团和矿物组分等特点，是一种适合于去除水溶液中污染物的吸附剂。以其环保、经济、高效的优点受到越来越多的关注。但与改性的复合活性炭相比，原始活性炭的比表面积更小，官能团更少，对污染物的吸附能力有限。为提高活性炭的吸附能力，选择了氨水对活性炭进行修饰处理的改性方法。近年来，许多研究人员使用负载氨基的复合材料来改善吸附剂对金属离子的吸附。在酸性条件下，氨基易于质子化形成正电荷基团，提高了复合材料的零电荷点。通过静电吸附、氧化还原以及氨基基团与Cr(VI)离子的氢键作用，可以提高Cr(VI)在水溶液中的去除率。因此，为了提高活性炭的吸附能力，如何把氨基基团负载在活性炭上进行改性，是目前研究的一个热点问题。因此，以桉木为主要原料，制备氨水改性桉木活性炭吸附剂及其应用具有较为有利的发展前景。
发明内容
本发明的目的是为了解决原始活性炭对水溶液中Cr(VI)的去除效果有限的问题，提出采用磷酸活化法制备桉木活化炭，接着用氨水对其进行改性将氨基基团负载于活性炭表面，制备氨水改性桉木活性炭吸附剂，从而提高对Cr(VI)的吸附能力。
目前，广泛使用吸附铬的吸附材料包括有天然吸附剂(沸石、黏土、泥煤、煤灰等)，人工合成碳基吸附剂(活性炭、生物炭、污泥碳、碳纳米管、氧化石墨烯等)，金属基吸附剂(纳米零价铁、金属氧化物纳米材料等)。这些材料中发挥吸附功效的主要成分比较单一。为了解决当前吸附剂吸附容量低，吸附能力有限的缺点，以及充分利用广西丰富的林业资源——桉木资源，本发明提供一种对铬具有较大吸附能力的吸附材料——氨水改性桉木活性炭吸附剂的制备方法。由此方法制备获得的氨水改性桉木活性炭吸附剂的比表面积为1654.38m2/g，在pH＝2的条件下吸附初始浓度为300mg/L的Cr(VI)溶液，平衡吸附量为260mg/g，对Cr(VI)溶液的去除率达到85.67％。
具体步骤为：
(1)将桉木锯成块，切成薄片，清洗并干燥后，置于粉碎机中粉碎并过30目筛，得到桉木粉末备用。
(2)称取10g步骤(1)所得桉木粉末浸泡于40mL的质量百分比浓度为40％的磷酸溶液中，室温条件下浸泡8～10h。
(3)将步骤(2)所得的浸泡后的桉木粉末放置于200mL坩埚中，置于马弗炉内，在500℃～600℃条件下热解1～2h，升温速率为10℃/min。
(4)将步骤(3)所得产物冷却至室温，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤。
(5)将步骤(4)所得产物置于培养皿中，放在60℃～80℃的烘箱中烘18～24h，然后研磨并过200目筛，获得桉木活性炭。
(6)于100mL烧杯中加入0.5g步骤(5)所得桉木活性炭，再加入60mL乙二醇，置于超声波清洗器中超声20～30min后，再加入20～30mL氨水，置于磁力搅拌器中搅拌(1100rpm)30～45min，所得均一的混合液装入到100mL聚四氟乙烯内衬的反应釜中，置于鼓风干燥箱中200℃条件下反应10～12h。
(7)将步骤(6)所得产物自然冷却，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤。
(8)将步骤(7)所得产物置于培养皿中，在60℃～80℃条件下干燥18～24h，过200目筛，得到氨水改性桉木活性炭吸附剂。
(9)上述制得的氨水改性桉木活性炭吸附剂应用于对水溶液中Cr(VI)的吸附去除。
本发明利用桉木作为主要原材料，降低了生产成本；采用磷酸活化法制备活性炭，再进行氨水改性，工艺流程简单，条件易行；负载氨基后的复合桉木活性炭相较于原始活性炭，能够通过静电吸附、氢键作用和氧化还原作用，大大增强对水溶液中Cr(VI)的吸附能力；所制备吸附剂可广泛应用于工矿企业含Cr(VI)废水的处理工序。
附图说明：
图1为本发明实施例制得的5000倍数下改性前后桉木活性炭SEM对比图谱。
图2为本发明实施例制得的改性前后桉木活性炭及氨水改性桉木活性炭吸附剂吸附Cr(VI)的FT-IR对比图谱。
图3为本发明实施例制得的改性前后桉木活性炭及氨水改性桉木活性炭吸附剂吸附Cr(VI)的XPS对比图谱。
图4为本发明实施例制得的改性前后桉木活性炭在不同的pH条件下，对溶液中Cr(VI)吸附量的变化对比图谱。
图5为本发明实施例制得的改性前后桉木活性炭在不同的吸附剂量条件下，对溶液中Cr(VI)吸附量及去除率的变化对比图谱。
图6为本发明实施例制得的改性前后桉木活性炭在不同的吸附时间条件下，对溶液中Cr(VI)吸附量及去除率的变化对比图谱。
图7为本发明实施例制得的改性前后桉木活性炭在不同的溶液浓度及温度条件下，对溶液中Cr(VI)吸附量的变化对比图谱。
具体实施方式
实施例：
(1)将桉木锯成块，切成薄片，清洗并干燥后，置于粉碎机中粉碎并过30目筛，得到桉木粉末备用。
(2)称取10g步骤(1)所得桉木粉末浸泡于40mL的质量百分比浓度为40％的磷酸溶液中，室温条件下浸泡10h。
(3)将步骤(2)所得的浸泡后的桉木粉末放置于200mL坩埚中，置于马弗炉内，在500℃条件下热解1h，升温速率为10℃/min。
(4)将步骤(3)所得产物冷却至室温，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤。
(5)将步骤(4)所得产物置于培养皿中，放在60℃的烘箱中烘24h，然后研磨并过200目筛，获得桉木活性炭。
(6)于100mL烧杯中加入0.5g步骤(5)所得桉木活性炭，再加入60mL乙二醇，置于超声波清洗器中超声20min后，再加入20mL氨水，置于磁力搅拌器中搅拌(1100rpm)30min，所得均一的混合液装入到100mL聚四氟乙烯内衬的反应釜中，置于鼓风干燥箱中200℃条件下反应10h。
(7)将步骤(6)所得产物自然冷却，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤。
(8)将步骤(7)所得产物置于培养皿中，在60℃条件下干燥24h，过200目筛，得到氨水改性桉木活性炭吸附剂。
(9)将本实施例制得的氨水改性桉木活性炭吸附剂应用于对水溶液中Cr(VI)的吸附去除。
(10)称取一定量本实施例制得的改性前后的桉木活性炭于100mL离心管中，采用25mL移液管向离心管中加入25mL、一定浓度、一定pH的Cr(VI)溶液，置于气浴振荡器中，在一定温度、200r/min转速条件下振荡混合一定时间后，用0.45μm滤膜过滤，用分光光度计测Cr(VI)剩余浓度，以考察经过氨水改性前后桉木活性炭的吸附能力变化，以及不同条件对吸附能力的影响。结果如图4、5、6、7所示。可以看出，本实施例制备得到的氨水改性桉木活性炭在pH＝3条件下，采用0.025g吸附剂处理25mL 300mg/L Cr(VI)溶液时，大约为720min后达到吸附平衡，温度升高在一定程度上促进对Cr(VI)的去除。相较原始活性炭而言，氨水改性桉木活性炭对Cr(VI)的去除能力显著提高。
采用新型热场发射扫描电镜(SEM，SU5000，日本日立)分析氨水改性桉木活性炭吸附剂的表面形貌，结果见图1；物相结构与元素组成则采用美国热电尼高力仪器公司470FTIR型FT-IR傅里叶红外光谱分析仪和美国热力公司ESCALAB 250Xi型X射线衍射仪进行测试，结果见图2和图3。

Claims (2)

1.一种氨水改性桉木活性炭吸附剂的制备方法，其特征在于具体步骤为：
(1)将桉木锯成块，切成薄片，清洗并干燥后，置于粉碎机中粉碎并过30目筛，得到桉木粉末备用；
(2)称取10g步骤(1)所得桉木粉末浸泡于40mL的质量百分比浓度为40％的磷酸溶液中，室温条件下浸泡8～10h；
(3)将步骤(2)所得的浸泡后的桉木粉末放置于200mL坩埚中，置于马弗炉内，在500℃～600℃条件下热解1～2h，升温速率为10℃/min；
(4)将步骤(3)所得产物冷却至室温，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤；
(5)将步骤(4)所得产物置于培养皿中，放在60℃～80℃的烘箱中烘18～24h，然后研磨并过200目筛，获得桉木活性炭；
(6)于100mL烧杯中加入0.5g步骤(5)所得桉木活性炭，再加入60mL乙二醇，置于超声波清洗器中超声20～30min后，再加入20～30mL氨水，置于100rpm磁力搅拌器中搅拌30～45min，所得均一的混合液装入到100mL聚四氟乙烯内衬的反应釜中，置于鼓风干燥箱中200℃条件下反应10～12h；
(7)将步骤(6)所得产物自然冷却，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤；
(8)将步骤(7)所得产物置于培养皿中，在60℃～80℃条件下干燥18～24h，过200目筛，得到氨水改性桉木活性炭吸附剂。
2.一种如权利要求1所述的氨水改性桉木活性炭吸附剂的应用，其特征在于，所述氨水改性桉木活性炭吸附剂应用于对水中Cr(VI)的吸附去除。
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