CN106378098A - 一种磁性DMG@Fe3O4吸附剂的制备及对镍的吸附应用 - Google Patents

一种磁性DMG@Fe3O4吸附剂的制备及对镍的吸附应用 Download PDF

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CN106378098A
CN106378098A CN201610890343.9A CN201610890343A CN106378098A CN 106378098 A CN106378098 A CN 106378098A CN 201610890343 A CN201610890343 A CN 201610890343A CN 106378098 A CN106378098 A CN 106378098A
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dmg
magnetic
adsorbent
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magneto separate
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李燕
张以河
魏琴
马洪敏
王维
王欢
杨学英
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University of Jinan
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

本发明公开了一种磁性DMG@Fe3O4吸附剂的制备及对镍的吸附应用。利用DMG和磁性Fe3O4合成了一种磁性DMG@Fe3O4吸附剂。将所合成的磁性DMG@Fe3O4吸附剂应用于重金属Ni2+离子的吸附，吸附效果良好，吸附量可达2000mg/g，解吸附条件温和，再生性强，可重复利用。

Description

一种磁性DMG@Fe3O4吸附剂的制备及对镍的吸附应用
技术领域
本发明属于水处理技术领域，特别涉及一种磁性丁二酮肟DMG/Fe3O4吸附剂的制备方法及在水处理中对重金属Ni2+离子吸附的应用技术。
背景技术
化学的进步为人类带来巨大益处的同时，也对环境造成了污染。重金属废水对环境的污染随城市和工业的发展日趋严重。世界卫生组织(WHO)所属的国际癌症研究机构(IARC)公布的39种(类)对人致癌物质中，镍被列为其中之一。为控制镍对人的危害，世界上许多国家已制定了镍的排放标准。随着人们对镍的危害认识的逐步加深，以及人们认识到镍是一种宝贵的资源，有必要加以回收利用。再加上一些地区或行业制定了镍的排放标准，所以对镍的治理及回收利用，变废为宝，越来越得到重视。目前去除水体系中的镍有化学沉淀、化学还原、离子交换、膜分离、生物絮凝等多种方法。这些方法，有的会产生大量的含镍废渣，易造成二次污染，有的处理效果较差。近几年，一些新的吸附材料被应用于含镍废水的处理，如纳米碳管、生物膜等，但是这些材料成本较高。膜分离、生物凝絮等多种方法因成本相对较高或不可再生，或容易造成二次污染，在应用方面受到限制。
吸附法处理重金属离子废水受到越来越多的重视。目前常用的吸附剂可分为腐植酸类吸附剂、碳类吸附剂、矿物吸附剂、高分子吸附剂、生物材料吸附剂、介孔SiO2材料等。吸附法的本质是依靠吸附剂来吸附处理重金属离子其特征是吸附剂具有丰富的孔道结构和高比表面积，因此研制高效选择性好的新型吸附剂极为迫切。上述吸附剂在分离上存在这样或那样的弊端。磁性材料的出现弥补了这一不足。本发明制备了一种磁性DMG/Fe3O4吸附剂，可轻松地利用磁分离分离吸附剂和溶液。本发明将制备的磁性DMG/Fe3O4吸附剂应用于Ni2+离子的吸附，吸附量大，再生性好，可反复使用。
发明内容
本发明的目的之一是制备了一种磁性DMG/Fe3O4吸附剂。
本发明的目的之二是将所制备的磁性DMG/Fe3O4吸附剂，用于重金属Ni2+的吸附。
本发明的技术方案如下：
1. 一种磁性DMG@Fe3O4吸附剂的制备，其特征在于，包括以下步骤：
称取用共沉淀法合成的四氧化三铁1g，置于浓度10~20g/L的十六烷基三甲基溴化铵CTMAB溶液100mL中，于80oC水浴加热搅拌10~12h，冷却至室温，磁分离，用蒸馏水多次洗涤颗粒，至无Br-，50oC真空干燥12h，研磨；将干燥研磨好的颗粒浸于100mL 1~3 mg/mL丁二酮肟乙醇溶液中，于60oC搅拌50~80min，静置老化，50~80min。磁分离，用乙醇和水多次洗涤，于60oC真空干燥24h，研磨，过筛制得磁性DMG@Fe3O4吸附剂。
2. 如权利要求1所述的制备方法制备的磁性DMG@Fe3O4吸附剂对镍的吸附应用，步骤如下：
(1) 吸附：称取磁性DMG@Fe3O4吸附剂0.1g置于100mL锥形瓶中；加入20.00mL10.00mg/mL的镍溶液，边摇边逐滴加入1mol/LNaOH溶液，采用磁分离分离吸附后吸附剂，用酸度计准确测量磁分离后溶液的pH8.50~11.50，并取清夜，用原子吸收法测定Ni2+的浓度，依据溶液中Ni2+离子的初始浓度c 0和吸附后溶液中Ni2+的浓度c e计算Ni2+离子的去除率；
(2) 解吸附：将吸附Ni2+后的磁性DMG/Fe3O4置于锥形瓶中，滴加1~2 mol/L HCl溶液至磁性DMG/Fe3O4上，充分搅拌，磁分离，用蒸馏水洗涤，滤液定容，稀释，用原子吸收法测定Ni2 +，磁分离后的固体为再生的磁性DMG@Fe3O4。
本发明的有益成果
(1) 本发明得到的磁性DMG/Fe3O4具有良好的磁性；是一种新型的具有磁性的吸附剂材料，具有良好的化学性能，对Ni2+的吸附量可达2000mg/g，易再生，可反复使用。
(2) 本发明磁性DMG/Fe3O4吸附剂的制备过程简单，条件易于控制，易操作，生产成本低。
(3) 本发明磁性DMG/Fe3O4吸附剂对Ni2+吸附效率高，吸附率和分离速度快，解吸附简单，只需NaOH和HCl即可实现Ni2+的吸附和解吸附，可实现含镍污水中镍离子的回收利用。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外还应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明做各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1 一种磁性DMG@Fe3O4吸附剂的制备
称取用共沉淀法合成的四氧化三铁1g，置于浓度10g/L的十六烷基三甲基溴化铵CTMAB溶液100mL中，于80oC水浴加热搅拌10h，冷却至室温，磁分离，用蒸馏水多次洗涤颗粒，至无Br-，50oC真空干燥12h，研磨；将干燥研磨好的颗粒浸于100mL 1mg/mL丁二酮肟乙醇溶液中，于60oC搅拌50min，静置老化，50min。磁分离，用乙醇和水多次洗涤，于60oC真空干燥24h，研磨，过筛制得磁性DMG@Fe3O4吸附剂。
实施例2 一种磁性DMG@Fe3O4吸附剂的制备
称取用共沉淀法合成的四氧化三铁1g，置于浓度15g/L的十六烷基三甲基溴化铵CTMAB溶液100mL中，于80oC水浴加热搅拌11h，冷却至室温，磁分离，用蒸馏水多次洗涤颗粒，至无Br-，50oC真空干燥12h，研磨；将干燥研磨好的颗粒浸于100mL 2 mg/mL丁二酮肟乙醇溶液中，于60oC搅拌60min，静置老化，60min。磁分离，用乙醇和水多次洗涤，于60oC真空干燥24h，研磨，过筛制得磁性DMG@Fe3O4吸附剂。
实施例3 一种磁性DMG@Fe3O4吸附剂的制备
称取用共沉淀法合成的四氧化三铁1g，置于浓度20g/L的十六烷基三甲基溴化铵CTMAB溶液100mL中，于80oC水浴加热搅拌12h，冷却至室温，磁分离，用蒸馏水多次洗涤颗粒，至无Br-，50oC真空干燥12h，研磨；将干燥研磨好的颗粒浸于100mL 3 mg/mL丁二酮肟乙醇溶液中，于60oC搅拌80min，静置老化， 80min。磁分离，用乙醇和水多次洗涤，于60oC真空干燥24h，研磨，过筛制得磁性DMG@Fe3O4吸附剂。
实施例4 磁性DMG@Fe3O4吸附剂对镍的吸附
称取磁性DMG@Fe3O4吸附剂0.1g置于100mL锥形瓶中；加入20.00mL 10.00mg/mL的镍溶液，边摇边逐滴加入1mol/LNaOH溶液，采用磁分离分离吸附后吸附剂，用酸度计准确测量磁分离后溶液的pH8.50，并取清夜，用原子吸收法测定Ni2+的浓度，依据溶液中Ni2+离子的初始浓度c 0和吸附后溶液中Ni2+的浓度c e计算Ni2+离子的去除率。
实施例5 磁性DMG@Fe3O4吸附剂对镍的吸附
称取磁性DMG@Fe3O4吸附剂0.1g置于100mL锥形瓶中；加入20.00mL 10.00mg/mL的镍溶液，边摇边逐滴加入1mol/LNaOH溶液，采用磁分离分离吸附后吸附剂，用酸度计准确测量磁分离后溶液的pH10.50，并取清夜，用原子吸收法测定Ni2+的浓度，依据溶液中Ni2+离子的初始浓度c 0和吸附后溶液中Ni2+的浓度c e计算Ni2+离子的去除率为100%，吸附量为2000mg/g。
实施例6 磁性DMG@Fe3O4吸附剂吸附镍后的解吸附
将吸附Ni2+后的磁性DMG/Fe3O4置于锥形瓶中，滴加1 mol/L HCl溶液至磁性DMG/Fe3O4上，充分搅拌，磁分离，用蒸馏水洗涤，滤液定容，稀释，用原子吸收法测定Ni2+，磁分离后的固体为再生的磁性DMG@Fe3O4。
实施例7
磁性DMG@Fe3O4吸附剂吸附镍后的解吸附
将吸附Ni2+后的磁性DMG/Fe3O4置于锥形瓶中，滴加1.5 mol/L HCl溶液至磁性DMG/Fe3O4上，充分搅拌，磁分离，用蒸馏水洗涤，滤液定容，稀释，用原子吸收法测定Ni2+，磁分离后的固体为再生的磁性DMG@Fe3O4。
实施例8
磁性DMG@Fe3O4吸附剂吸附镍后的解吸附
将吸附Ni2+后的磁性DMG/Fe3O4置于锥形瓶中，滴加2mol/L HCl溶液至磁性DMG/Fe3O4上，充分搅拌，磁分离，用蒸馏水洗涤，滤液定容，稀释，用原子吸收法测定Ni2+，磁分离后的固体为再生的磁性DMG@Fe3O4。

Claims (2)

1.一种磁性DMG@Fe3O4吸附剂的制备，其特征在于，包括以下步骤：
称取用共沉淀法合成的四氧化三铁1g，置于浓度10~20g/L的十六烷基三甲基溴化铵CTMAB溶液100mL中，于80oC水浴加热搅拌10~12h，冷却至室温，磁分离，用蒸馏水多次洗涤颗粒，至无Br-，50oC真空干燥12h，研磨；将干燥研磨好的颗粒浸于100mL 1~3 mg/mL丁二酮肟乙醇溶液中，于60oC搅拌50~80min，静置老化，50~80min，磁分离，用乙醇和水多次洗涤，于60oC真空干燥24h，研磨，过筛制得磁性DMG@Fe3O4吸附剂。
2.如权利要求1所述的制备方法制备的磁性DMG@Fe3O4吸附剂对镍的吸附应用，步骤如下：
（1）吸附：称取磁性DMG@Fe3O4吸附剂0.1g置于100mL锥形瓶中；加入20.00mL 10.00mg/mL的镍溶液，边摇边逐滴加入1mol/LNaOH溶液，采用磁分离分离吸附后吸附剂，用酸度计准确测量磁分离后溶液的pH8.50~11.50，并取清夜，用原子吸收法测定Ni2+的浓度，依据溶液中Ni2+离子的初始浓度c 0和吸附后溶液中Ni2+的浓度c e计算Ni2+离子的去除率；
（2）解吸附：将吸附Ni2+后的磁性DMG/Fe3O4置于锥形瓶中，滴加1~2 mol/L HCl溶液至磁性DMG/Fe3O4上，充分搅拌，磁分离，用蒸馏水洗涤，滤液定容，稀释，用原子吸收法测定Ni2+，磁分离后的固体为再生的磁性DMG@Fe3O4。
CN201610890343.9A 2016-10-13 2016-10-13 一种磁性DMG@Fe3O4吸附剂的制备及对镍的吸附应用 Pending CN106378098A (zh)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103331142A (zh) * 2013-07-11 2013-10-02 南京工业大学 一种磁性吸附剂、制备方法及其在燃料油脱硫中的应用

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103331142A (zh) * 2013-07-11 2013-10-02 南京工业大学 一种磁性吸附剂、制备方法及其在燃料油脱硫中的应用

Non-Patent Citations (2)

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KAMYAR KHOSHNEVISAN，ET AL.: "Preparation and Characterization of CTAB-Coated Fe3O4 Nanoparticles", 《SYNTHESIS AND REACTIVITY IN INORGANIC, METAL-ORGANIC, AND NANO-METAL CHEMISTRY》 *
翟云会，罗鹏煜: "丁二酮肟掺杂磁性Fe3O4离子吸附剂的制备", 《纳米加工工艺》 *

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