CN108176362A - 一种稳定的铁锰氧化物制备方法 - Google Patents

一种稳定的铁锰氧化物制备方法 Download PDF

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CN108176362A
CN108176362A CN201810163193.0A CN201810163193A CN108176362A CN 108176362 A CN108176362 A CN 108176362A CN 201810163193 A CN201810163193 A CN 201810163193A CN 108176362 A CN108176362 A CN 108176362A
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iron
manganese oxides
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activated carbon
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张福彪
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Rucheng Three Xin Electrochemical Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204Inorganic carriers, supports or substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234Inorganic material layers
    • B01J20/3236Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

Abstract

本发明涉及一种稳定的铁锰氧化物制备方法,包括以下步骤:步骤一、制备FeCl2溶液和KMnO4溶液,混合得到混合溶液,然后在混合溶液中加入活性炭搅拌;步骤二、将混合溶液的pH调节到7‑7.5,然后通入交流电5‑10min;步骤三、过滤混合溶液得到固体产物,干燥碾碎后即得成品。本发明的制备方法简易,环境友好,易于工业化生产,制得的生物炭稳定化铁锰氧化物与生物炭或铁锰氧化物吸附剂相比,对有机污染物的吸附性能得到提高。

Description

一种稳定的铁猛氧化物制备方法
技术领域
[0001]本发明涉及环境功能材料领域,特别涉及一种稳定的铁锰氧化物制备方法。
背景技术
[0002]铁锰氧化物是一种绿色和经济的氧化剂,可用于去除多种环境污染物。由于其相 对较大的表面积和高活性,近年来铁锰氧化物已广泛应用于控制水和土壤污染,已成为一 项重要的环境修复技术。然而,由于其较大的表面能量和强烈的磁场吸引力,铁锰氧化物易 于聚集。此外,当在水中分散成纳米颗粒时,将铁锰氧化物从悬浮液中回收是相当困难的。 这些缺点限制它进一步的环境应用。因此,通过适当的方法将铁锰氧化物负载在活性炭的 表面,使其不易聚集,提高稳定性和吸附性能。
发明内容
[0003]有鉴于此,本发明的目在于提供一种吸附性能良好、稳定性高的稳定的铁锰氧化 物制备方法。本发明制备方法简易,环境友好,制作快速,易于工业化生产,制得的生物炭稳 定化铁锰氧化物与生物炭或铁锰氧化物吸附剂相比,对有机污染物的吸附性能得到提高。
[0004] 本发明的目的可以通过以下技术方案来实现:
[0005] 一种稳定的铁锰氧化物制备方法,包括以下步骤:
[0006]步骤一、制备FeCl2溶液和KMn〇4溶液,混合得到混合溶液,然后在混合溶液中加入 活性炭搅拌;
[0007]步骤二、将混合溶液的pH调节到7-7.5,然后通入交流电5-lOmin;
[0008]步骤三、过滤混合溶液得到固体产物,干燥碾碎后即得成品。
[0009]进一步的改进,所述步骤一中,FeCl2溶液浓度为1 • 785毫摩尔/L; KMn04溶液浓度为 0.85毫摩尔/L。
[0010]进一步的改进,所述FeCl2溶液与KMn04溶液的体积比为1〇〇: 70。
[0011]进一步的改进,所述活性炭与混合溶液的固液比为100:170mg/ml。
[0012]进一步的改进,所述交流电的频率为5〇Hz,交流电电流为〇.卜〇 • 3A。
[0013]进一步的改进,所述固体产物在80°C温度下烘干。
[0014] 进一步的改进,所述活性炭通过稻壳和/或秸秆制成。
[0015]所述的活性炭是以农业废弃物稻壳和秸秆为原料,粉碎至粒径小于0• 147mm并过 100目筛,经在氮气环境下限氧热解方法制得;
[0016] 活性炭的表面积为176m2/g,孔容为0• 17cm3/g;
[0017] 所述的使用磁力搅拌器搅拌,磁力搅拌速度为16〇rpm。
[0018] 本发明制备的活性炭稳定化铁锰氧化物材料直接以农业废弃物稻壳和秸秆为原 料,在FeCl2和KMn04溶液中,将铁锰氧化物沉降在活性炭上。
[0019] 与现有技术相比,本发明具有以下特点:
[0020] 1 •本发明以农业废弃物稻壳和猜杆为原料,制备方法简单,成本低廉;
[0021] 2 •本发明制得的活性炭稳定化铁锰氧化物在水溶液中不易聚集,作为吸附剂,容 易集中回收再利用;
[0022]
[0023] 3.制备方法简单可行,生产速度快周期短,不需要复杂的化工设备,能够实现工业 化生产。
[0024]
附图说明
[0025]图1是本发明实施例1的活性炭稳定化铁锰氧化物的扫描电镜示意图和能谱分析 图;
[0026]图2是本发明实施例1的活性炭稳定化铁锰氧化物在不同初始浓度下处理有机污 染物雌二醇;
[0027]图3是本发明实施例1的活性炭稳定化铁锰氧化物在不同时间下处理有机污染物 雌二醇;
具体实施方式
[0028]以下将结合说明书附图和具体实施例对本发明做进一步详细说明。
[0029] 实施例1:
[0030] 一种本发明所述的活性炭稳定化铁锰氧化物的具体制备方法如下:
[0031]首先制备两种储备溶液,S卩100mL l_785raM FeCl2和70mL0.85mM KMn〇4混合。再将 l〇〇mg活性炭加入到混合溶液中,磁力搅拌20min。,接着用1M NaOH慢慢调节pH值到7.0〜 7 • 5,并继续磁力搅拌30分钟。之后,通入交流电5-10min,交流电的频率为50Hz,交流电电流 为0.1-0.3A,然后过滤。在将固体从水中分离出来后,用去离子水反复清洗材料直到pH为中 性,并在80°C温度中干燥24h,之后用辗钵捣碎干燥材料。
[0032]制备得到的活性炭稳定化铁锰氧化物材料,在扫描电镜下观察,如图1所示,可以 看到表面有纳米颗粒负载在活性炭的表面。能谱定量分析,可以看到活性炭稳定化铁锰氧 化物材料上存在铁元素和锰元素。
[0033] 实施例2:
[0034]本发明的活性炭稳定化铁锰氧化物材料处理水体中的有机污染物雌二醇,包括以 下步骤:
[0035] 分别取0_2〜8mg/L有机污染物雌二醇溶液lOOmL于锥形瓶中,每个锥形瓶中加入 5mg该材料后,置于水浴恒温振荡器中,在25°C条件下反应。24h后,每个锥形瓶分别取1〇眺 溶液进行离心,离心后通过0 • 45um滤膜过滤,取滤液于离心管中。采用荧光风光光度计检测 反应后的溶液浓度。结果如图2所示,在不同有机污染物雌二醇初始浓度条件下,该材料对 水体中有机污染物雌二醇具有较高吸附能力。在初始浓度为〇.2mg/L的条件下具有1.85mg/ g的吸附量,并随初始浓度增加而增加,到8mg/L的条件下该吸附剂的吸附量达到52.22mg/ g〇
[0036] 实施例3:
[0037]本发明的活性炭稳定化铁锰氧化物材料处理水体中有机污染物雌二醇,包括以下 步骤:
[0038]将〇_〇lg该材料加入到lOOmL的6mg/L的有机污染物雌二醇溶液中,置于水浴恒温 振荡器中,在25°C条件下反应。在不同的间隔时间点分别取l〇mL溶液进行离心,离心后通过 〇. 45WI1滤膜过滤,取滤液于离心管中。采用荧光分光光度计检测反应后的溶液浓度。不同时 间下的吸附量结果以及和铁锰氧化物,原始活性炭的对比如附图3所示,活性炭稳定化铁锰 氧化物对水体中有机污染物雌二醇的吸附量随着时间的增加不断增加。在lOmin到200min 之间,吸附量快速增加,并在400min以后开始达到饱和。这说明活性炭稳定化铁锰氧化物材 料能够快速吸附处理水体中有机污染物雌二醇。并且和铁锰氧化物,原始活性炭相比,活性 炭稳定化铁锰氧化物的吸附容量得到提升。
[0039]以上仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例, 与本发明构思无实质性差异的各种工艺方案均在本发明的保护范围。

Claims (7)

1.一种稳定的铁锰氧化物制备方法,包括以下步骤: 步骤一、制备FeCh溶液和KMn〇4溶液,混合得到混合溶液,然后在混合溶液中加入活性 炭搅拌; 步骤二、将混合溶液的pH调节到7-7.5,然后通入交流电5-l〇min; 步骤三、过滤混合溶液得到固体产物,干燥碾碎后即得成品。
2. 如权利要求1所述的稳定的铁锰氧化物制备方法,其特征在于,所述步骤一中,FeCl2 溶液浓度为1 • 785毫摩尔/L; KMn04溶液浓度为0 •85毫摩尔/L。
3. 如权利要求2所述的稳定的铁锰氧化物制备方法,其特征在于,所述FeCl2溶液与 !«11〇4溶液的体积比为1〇〇:7〇。
4. 如权利要求3所述的稳定的铁猛氧化物制备方法,其特征在于,所述活性炭与混合溶 液的固液比为1〇〇: 170mg/ml。
5. 如权利要求1所述的稳定的铁猛氧化物制备方法,其特征在于,所述交流电的频率为 50Hz,交流电电流为〇. 1 -〇.3A。
6. 如权利要求1所述的稳定的铁猛氧化物制备方法,其特征在于,所述固体产物在8〇°C 温度下烘干。 _
7. 如权利要求1所述的稳定的铁猛氧化物制备方法,其特征在于,所述活性炭通过稻壳 和/或秸杆制成。
CN201810163193.0A 2017-11-13 2018-02-26 一种稳定的铁锰氧化物制备方法 Pending CN108176362A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174000A (zh) * 2018-10-17 2019-01-11 南方科技大学 一种用于雌酮污染土壤的原位固定剂及其制备方法和应用
CN110125159A (zh) * 2018-12-12 2019-08-16 浙江省农业科学院 一种铁锰基生物炭对镉锑复合土壤的钝化效果的优化工艺

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101507928A (zh) * 2009-03-23 2009-08-19 华南理工大学 一种铁锰复合氧化物催化剂及其制备方法和应用
CN104888704A (zh) * 2015-05-21 2015-09-09 桂林理工大学 桑杆活性炭/铁锰氧化物复合吸附剂的制备方法
CN104971752A (zh) * 2014-04-03 2015-10-14 南京工大环境科技有限公司 适用于催化氧化工艺的磁性催化剂及其制备方法和应用
CN106669727A (zh) * 2016-12-28 2017-05-17 华南理工大学 一种活化过硫酸盐处理印染废水的污泥碳化改性磁性纳米材料的制备方法与应用
CN106669614A (zh) * 2017-01-18 2017-05-17 湖南大学 Ctab表面活化粘土矿物负载纳米金属氧化物的制备及其用途
CN107551998A (zh) * 2017-09-23 2018-01-09 湖南大学 一种生物炭稳定化铁锰氧化物的制备方法和应用

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101507928A (zh) * 2009-03-23 2009-08-19 华南理工大学 一种铁锰复合氧化物催化剂及其制备方法和应用
CN104971752A (zh) * 2014-04-03 2015-10-14 南京工大环境科技有限公司 适用于催化氧化工艺的磁性催化剂及其制备方法和应用
CN104888704A (zh) * 2015-05-21 2015-09-09 桂林理工大学 桑杆活性炭/铁锰氧化物复合吸附剂的制备方法
CN106669727A (zh) * 2016-12-28 2017-05-17 华南理工大学 一种活化过硫酸盐处理印染废水的污泥碳化改性磁性纳米材料的制备方法与应用
CN106669614A (zh) * 2017-01-18 2017-05-17 湖南大学 Ctab表面活化粘土矿物负载纳米金属氧化物的制备及其用途
CN107551998A (zh) * 2017-09-23 2018-01-09 湖南大学 一种生物炭稳定化铁锰氧化物的制备方法和应用

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
QIMENG NING ET AL.: "Fabrication of hydrochar functionalized Fe-Mn binary oxide nanocomosites:characterization and 17β-estradiol removal", 《RSC ADVANCES》 *
于敏娜等: "ZnFe2O4、MnFe2O4铁氧体纳米粒子的制备、表征及磁性能", 《化工进展》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174000A (zh) * 2018-10-17 2019-01-11 南方科技大学 一种用于雌酮污染土壤的原位固定剂及其制备方法和应用
CN110125159A (zh) * 2018-12-12 2019-08-16 浙江省农业科学院 一种铁锰基生物炭对镉锑复合土壤的钝化效果的优化工艺

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