CN113023818A - 一种水净化材料 - Google Patents

一种水净化材料 Download PDF

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CN113023818A
CN113023818A CN202110272198.9A CN202110272198A CN113023818A CN 113023818 A CN113023818 A CN 113023818A CN 202110272198 A CN202110272198 A CN 202110272198A CN 113023818 A CN113023818 A CN 113023818A
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water
water purification
mno
hollow mesoporous
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高琴
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Yishui Hongyu Environmental Science And Technology Center
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Yishui Hongyu Environmental Science And Technology Center
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    • 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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0222—Compounds of Mn, Re
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • 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
    • 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
    • B01J20/28014—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 form

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

本申请涉及一种水净化材料，其采用如下步骤制备：(1)制备中空介孔SiO2，将Fe3+、Fe2+两种盐溶液均匀混合，随后加入一定量的CTAB作为表面活性剂，向其中加入中空介孔SiO2，超声处理以使得铁盐充分进入SiO2中空孔隙中，滴加氨水80‑100℃水浴加热反应一定时间，反应产物用蒸馏水和乙醇交替洗涤3次，得到负载有Fe3O4的中空介孔SiO2；(2)将步骤(1)制备得到的复合材料分散于乙二醇溶液中，随后加入醋酸锰和氯酸钠搅拌均匀，转移到水热釜中，在150‑190℃溶剂热反应10‑15h；冷却到室温，洗涤干燥，得到Fe3O4/SiO2/MnO2的复合材料，MnO2作为棒状材料包覆于Fe3O4/SiO2外周围，该复合材料对水中重金属离子与有机染料分子具有优异的吸附性能，并满足水净化材料的各项要求。

Description

一种水净化材料
技术领域
本发明涉及水处理技术领域，具体涉及一种Fe3O4/SiO2/MnO2的复合材料及其制备方法和应用。
背景技术
随着社会的快速发展，我国的工业化城市化速度不断加快，对城市河道的水环境造成了很大的破坏，水质问题和生态问题愈发严重，污染水体中含有大量的重金属离子，对生态平衡和人类健康均造成很大的威胁。目前水污染治理的方法包括化学沉淀法、生物修复法和吸附法等。吸附法工艺简单、成本较低、并且能够循环利用，已被证明是去除废水中包括钴离子在内的重金属离子去除的有效方法。
磁性纳米材料是重要的水污染处理材料之一，但是其在水溶液中容易聚集，在酸性条件容易反应而产生新的污染。而且很多材料制备成本高、效率低、耗时长；而且目前的磁性吸附材料大多只能单一吸附污染物，应用范围小，因此，开展可降解、高效吸附多种污染物的新型磁性复合材料的研究具有重要的意义。
发明内容
发明目的：提供一种水净化材料及其制备方法，以解决背景技术中所涉及的问题。
(1)制备中空介孔SiO2，将Fe3+、Fe2+两种盐溶液均匀混合，随后加入一定量的CTAB作为表面活性剂，向其中加入中空介孔SiO2，超声混合以使得Fe3+、Fe2+充分进入中空介孔SiO2孔隙中，接着滴加氨水80-100℃水浴加热反应一定时间，反应产物用蒸馏水和乙醇交替洗涤3次，得到负载有Fe3O4的中空介孔SiO2；
(2)将步骤(1)制备得到的复合材料分散于乙二醇溶液中，随后加入醋酸锰和氯酸钠搅拌均匀，转移到水热釜中，在150-190℃溶剂热反应10-15h；冷却到室温，洗涤干燥，得到Fe3O4/SiO2/MnO2的复合材料，MnO2作为棒状材料包覆于Fe3O4/SiO2外周围。
优选的，Fe3O4和中空介孔SiO2的摩尔比为1：(0.4-2)；
优选的，溶剂热的反应温度为150-190℃；
优选的，溶剂热反应时间为10-15h；
优选的，MnO2和Fe3O4/SiO2质量比为1：(0.4-4)。
技术效果
本发明利用中空介孔的二氧化硅负载纳米磁性Fe3O4，有效避免纳米Fe3O4的团聚问题，Fe3O4纳米颗粒具有极高的稳定性和分散性；利用Fe3O4的分离性能，利于吸附剂材料与水的分离及材料的回收再利用；采用溶剂热法制备得到纳米棒状的MnO2包覆Fe3O4/SiO2，一方面其具有较大的比表面积，提高了材料吸附性能，另一方面，可以对Fe3O4/SiO2形成保护作用；可作为高效的吸附剂应用于污水的处理，具有广阔的应用前景。
附图说明
附图1为本申请Fe3O4/SiO2/MnO2的复合材料的SEM图
具体实施方式
实施例1
(1)按FeCl2·4H2O、FeCl3·6H2O、中空介孔SiO2、CTAB质量比1.5：1：1：0.2称量混合，超声1h，滴加氨水，80℃水浴加热反应2h，反应产物用蒸馏水和乙醇交替洗涤3次，得到负载有Fe3O4的中空介孔SiO2；
(2)将步骤(1)制备得到的复合材料，醋酸锰和氯酸钠以质量比为1：1：0.8的比例加入100ml的乙二醇中，的搅拌均匀，转移到水热釜中，在150℃溶剂热反应10h；冷却到室温，洗涤干燥，得到Fe3O4/SiO2/MnO2的复合材料，MnO2作为棒状材料包覆于Fe3O4/SiO2外周围。
实施例2
(1)按FeCl2·4H2O、FeCl3·6H2O、中空介孔SiO2、CTAB质量比1.5：1：1.5：0.2称量混合，超声1h，滴加氨水，80℃水浴加热反应1h，反应产物用蒸馏水和乙醇交替洗涤3次，得到负载有Fe3O4的中空介孔SiO2；
(2)将步骤(1)制备得到的复合材料，醋酸锰和氯酸钠以质量比为1：1：0.8的比例加入100ml的乙二醇中，的搅拌均匀，转移到水热釜中，在160℃溶剂热反应10h；冷却到室温，洗涤干燥，得到Fe3O4/SiO2/MnO2的复合材料，MnO2作为棒状材料包覆于Fe3O4/SiO2外周围。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (5)

1.一种水净化材料，其采用如下步骤制备：
(1)制备中空介孔SiO2，将Fe3+、Fe2+两种盐溶液均匀混合，随后加入一定量的CTAB作为表面活性剂，向其中加入中空介孔SiO2，超声1-2h，滴加氨水80-100℃水浴加热反应一定时间，反应产物用蒸馏水和乙醇交替洗涤3次，得到负载有Fe3O4的中空介孔SiO2；
(2)将步骤(1)制备得到的复合材料分散于乙二醇溶液中，随后加入醋酸锰和氯酸钠搅拌均匀，转移到水热釜中，在150-190℃溶剂热反应10-15h；冷却到室温，洗涤干燥，得到Fe3O4/SiO2/MnO2的复合材料，MnO2作为纳米棒状材料包覆于Fe3O4/SiO2外周围。
2.根据权利要求1所述的一种水净化材料，Fe3O4和中空介孔SiO2的摩尔比为1：(0.4-2)。
3.根据权利要求1-3所述的一种水净化材料，溶剂热的反应温度为150-190℃。
4.根据权利要求1所述的一种水净化材料，溶剂热反应时间为10-15h。
5.根据权利要求1所述的一种水净化材料，MnO2和Fe3O4/SiO2质量比为1：(0.4-4)。
CN202110272198.9A 2021-03-12 2021-03-12 一种水净化材料 Withdrawn CN113023818A (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113617329A (zh) * 2021-08-18 2021-11-09 上海海洋大学 一种介孔Fe3O4复合吸附剂的一步制备及其在治理含As(Ⅲ)水溶液中的应用
CN115814770A (zh) * 2022-12-12 2023-03-21 南通大学 一种磁性多孔纳米二氧化硅流体的制备方法及应用
CN115814770B (zh) * 2022-12-12 2024-06-04 南通大学 一种磁性多孔纳米二氧化硅流体的制备方法及应用

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113617329A (zh) * 2021-08-18 2021-11-09 上海海洋大学 一种介孔Fe3O4复合吸附剂的一步制备及其在治理含As(Ⅲ)水溶液中的应用
CN115814770A (zh) * 2022-12-12 2023-03-21 南通大学 一种磁性多孔纳米二氧化硅流体的制备方法及应用
CN115814770B (zh) * 2022-12-12 2024-06-04 南通大学 一种磁性多孔纳米二氧化硅流体的制备方法及应用

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