CN108479692A - 一种磁性壳聚糖膨润土复合材料的制备方法 - Google Patents

一种磁性壳聚糖膨润土复合材料的制备方法 Download PDF

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CN108479692A
CN108479692A CN201810379816.8A CN201810379816A CN108479692A CN 108479692 A CN108479692 A CN 108479692A CN 201810379816 A CN201810379816 A CN 201810379816A CN 108479692 A CN108479692 A CN 108479692A
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bentonite
chitosan
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cts
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娄大伟
明明
连丽丽
吕进义
王希越
张�浩
高文秀
祝波
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Jilin Institute of Chemical Technology
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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
    • B01J20/02—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
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur

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  • Organic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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Abstract

本发明属于无机复合材料与技术领域，具体涉及一种功能化磁性壳聚糖膨润土复合材料的制备方法。以Fe3O4为基板，与壳聚糖膨润土通过超声复合制得带有磁性的功能化壳聚糖复合材料。该材料具有稳定的化学性质，分散性好，吸附能力强，制作过程环保无污染，可用于污水中刚果红的吸附。本发明所涉及的方法简单，原料易得，适合于不同样品中染料的吸附与去除，具有广阔的应用前景。

Description

一种磁性壳聚糖膨润土复合材料的制备方法
技术领域
本发明属于无机复合材料与技术领域，具体涉及一种新型磁性壳聚糖膨润土纳米材料的制备，此材料可应用于水中刚果红的吸附。
技术领域
壳聚糖作为一种天然的可再生资源，有良好的生物降解性、无毒、较好的抗菌能力以及对染料的吸附能力等。但是壳聚糖的溶解性比较差，而且固液分离难，单独使用壳聚糖作为吸附剂对水中阴离子印染废水处理效果不高且无法从跟本上解决染料的污染问题。
以天然膨润土作为基体负载壳聚糖制备新型的壳聚糖/膨润土复合吸附剂，一方面可以降低膨润土在废水中的高膨胀高悬浮等特性、另一方面解决了壳聚糖密度小、易漂浮，难于与溶液中污染物接触的问题。目前所制备的膨润土/壳聚糖复合吸附剂大体分为两种，一种为壳聚糖负载在膨润土表面，另一种为壳聚糖插层到膨润土内。本研究采用微波作为能源将壳聚糖修饰于膨润土表面，为了解决吸附剂固液分离的问题，与具有超顺磁性的Fe3O4通过超声复合得到磁性壳聚糖膨润土复合材料。通过这种方法得到了一种廉价无污染的吸附材料，并在吸附印染废水中刚果红显示了独特的优势。
发明内容
本发明提供的用于吸附染料刚果红的功能化磁性纳米粒子，其具体制备方法如下：
（1）将一定质量的壳聚糖加入到乙酸溶液中溶解后搅拌均匀，加入膨润土搅拌均匀成浆糊，使膨润土充分润湿之后倒进坩埚里，放入微波炉，使用中火微波一定时间。使用研钵研成粉末，制得壳聚糖膨润土复合材料（CTS-B）;
(2) 取CTS-B加入50 mL的去离子水充分混合，再加入Fe3O4超声20min，利用外加磁场使复合材料与溶液分离，用水和乙醇各洗涤3次放入真空干燥箱烘干、研细，制得壳聚糖修饰的磁性膨润土（CTS-B-Fe3O4）。
本发明制备的磁性纳米粒子具有合成简单、成本低、吸附能力强等优点，可用于印染废水中刚果红的吸附。
附图说明
图1是制得的磁性纳米粒子傅里叶红外光谱图片。
图2是不同浓度吸附剂对染料吸附效果的影响图片。
具体实施方式
磁性纳米粒子制备实施例：
将0.6 g壳聚糖加入到8 mL的5 %的乙酸溶液中溶解后搅拌均匀，加入6.5 g的膨润土搅拌均匀成浆糊，使膨润土充分润湿之后倒进坩埚里，放入微波炉，使用中火微波10 min。使用研钵研成粉末。取CTS-B功能化复合膨润土0.6 g加入50 ml的去离子水再加入0.5 g的Fe3O4超声20min使其混合均匀，利用磁性分离，用水和乙醇各洗涤3次放入真空干燥箱40 ℃烘干、研细。
磁性纳米粒子的应用实例:
配置 50mL的浓度分别为20 mg/L、30 mg/L、40 mg/L的刚果红溶液，加入0.03g壳聚糖/膨润土吸附剂，振荡至吸附平衡，用722分光光度计测定吸光度。

Claims (8)

1.一种吸附染料刚果红的壳聚糖修饰的膨润土磁性材料的制备方法，其特征在于，制备出壳聚糖复合膨润土（CTS-B），与Fe3O4混合，超声制得功能化磁性纳米材料，具体制备方法如下：
(1) 将一定质量的壳聚糖加入到5 %的乙酸溶液中溶解后搅拌均匀，加入膨润土搅拌均匀成浆糊，使膨润土充分润湿之后倒进坩埚里，放入微波炉，使用中火微波一定时间，使用研钵研成粉末，制得功能化复合膨润土（CTS-B）；
(2) 取CTS-B功能化复合膨润土加入50 ml的去离子水，再加入Fe3O4超声20min使其混合均匀，利用磁性分离，用水和乙醇各洗涤3次放入真空干燥箱烘干、研细。
2.按照权利要求书1中(1)所述的制备方法，其特征在于：壳聚糖的质量为0.3~0.5 g。
3.按照权利要求书1中(1)所述的制备方法，其特征在于：乙酸溶液的体积为5~10mL。
4.按照权利要求书1中(1)所述的制备方法，其特征在于：膨润土的质量为5~10 g。
5.按照权利要求书1中(1)所述的制备方法，其特征在于：微波的时间为5~10 min。
6.按照权利要求书1中(2)所述的制备方法，其特征在于：TS-B功能化复合膨润土的质量为0.6~1g。
7.按照权利要求书1中(2)所述的制备方法，其特征在于：Fe3O4的质量为0.5g。
8.按照权利要求书1中(2)所述的制备方法，其特征在于：真空干燥箱的烘干温度为40~70℃。
CN201810379816.8A 2018-04-25 2018-04-25 一种磁性壳聚糖膨润土复合材料的制备方法 Pending CN108479692A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111359658A (zh) * 2018-12-26 2020-07-03 广西大学 一种有机修饰磁性膨润土负载的花状BiOBr及其制备方法和应用
CN111468067A (zh) * 2020-04-27 2020-07-31 吉林化工学院 一种金属氧化物NiO的制备和应用

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111359658A (zh) * 2018-12-26 2020-07-03 广西大学 一种有机修饰磁性膨润土负载的花状BiOBr及其制备方法和应用
CN111468067A (zh) * 2020-04-27 2020-07-31 吉林化工学院 一种金属氧化物NiO的制备和应用

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