CN110523381A - 一种有机磷吸附剂的制备方法和该吸附剂的应用 - Google Patents
一种有机磷吸附剂的制备方法和该吸附剂的应用 Download PDFInfo
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Abstract
本发明公开了一种尿素官能团化磁性吸附材料Urea‑Fe3O4@LDH的制备及其在吸附去除水中有机磷的应用,属于水污染控制技术领域。该Urea‑Fe3O4@LDH的制备,首先利用共沉淀法和水热法结合制备磁性核壳结构Fe3O4@LDH,然后运用将尿素官能团负载在Fe3O4@LDH的表面,得到Urea‑Fe3O4@LDH。本发明提供的吸附材料表面含尿素基团,可用于水中有机磷的高效去除,并且利用磁铁能快速从水中分离。
Description
技术领域
本发明属于水污染控制技术领域,涉及一种有机磷吸附剂的制备方法和利用Urea-Fe3O4@LDH吸附有机磷的方法。
背景技术
有机磷(OP)是一类化学物质,根据与中心P原子相连的官能团不同而具有不同的化学性质,主要包括除草剂,杀虫剂,有机磷阻燃剂等,这类物质都是以含有磷原子的有机酯化合物为基础,具有毒性、生物积累性和持久性。大多数有机磷使用后仍留在生态系统中,并可在许多环境介质中检测到,如水、土壤和大气,直接或间接地对生态环境和人类安全构成了巨大威胁;此外,已经在许多植物和动物中检测到有机磷,特别是蔬菜、水果、牛奶等食品中,它们通过人体内的食物链积聚。因此,开发有效的材料是去除水中有机磷的重要挑战。
为了从水体中有效去除有机磷,需要开发具有高效快速吸附能力的材料。尿素对有机磷污染物具有显着的选择性。尿素作为活性位点的基团通过鉴定P=O吸附有机磷污染物,尿素供体和P=O受体可在反应中形成氢键。在水中,带有尿素衍生基团的吸附剂可以通过NH-CO-NH和P=O之间产生静电吸引或氢键结合,这有利于快速和选择性地去除水中的有机磷污染物。
此外,吸附剂的分离和回收是将它们用于去除水和废水处理中的污染物的另一个重要因素。Fe3O4磁性纳米粒子具有生物相容性,无毒,易与水溶液分离的特性。同时核壳结构被证实是防止Fe3O4聚集和氧化的有效方法。层状双氢氧化物(LDHs)因其丰富的羟基,非凡的离子交换能力和简单的制备而备受关注。本发明成功制备了Fe3O4@LDH核壳材料和Urea-Fe3O4@LDH,能够高效快速吸附有机磷污染物,并且在反应中表现出良好的分离能力。
发明内容
本发明的目的在于提供一种利用Urea-Fe3O4@LDH高效快速吸附有机磷并快速从水中分离的方法。
本发明利用共沉淀法和水热法制备磁性核壳结构Fe3O4@LDH,然后利用LDH表面的羟基将尿素官能团负载在Fe3O4@LDH的表面,得到磁性吸附材料Urea-Fe3O4@LDH。该吸附剂表面NH-CO-NH基团具有良好的吸附作用,并且具有顺磁性,采用磁铁即能够实现快速简单分离。
Urea-Fe3O4@LDH的制备方法,包括以下步骤:
Ⅰ.Fe3O4@LDH的制备:
(1)将Fe3O4纳米颗粒超声分散在30mL去离子水中,与NaOH和Na2CO3混合均匀;
(2)在搅拌下滴加15mL Mg(NO3)2·6H2O和Al(NO3)3·9H2O混合溶液(Mg2+/Al3+=3/1),搅拌20min,保持pH=10,取出上清液并加入乙二醇,搅拌10min;
(3)将混合物移入反应釜110℃保持12h;
(4)将得到的固体洗涤至中性,在60℃下干燥,研磨过筛得到Fe3O4@LDH粉末。
Ⅱ.Urea-Fe3O4@LDH的制备:
(1)将Fe3O4@LDH分散在100mL乙醇中,加入3-氨丙基三乙氧基硅烷,在80℃下回流10h,洗涤干燥后得到NH2-Fe3O4@LDH;
(2)将得到的材料分散到四氢呋喃中,加入对甲苯基异氰酸酯,室温下搅拌24h;
(3)用乙醇和水洗涤,在60℃下干燥,得到Urea-Fe3O4@LDH。
进一步的研究上述制备得到的Urea-Fe3O4@LDH在吸附去除水中磷酸三苯酯上的应用。
Urea-Fe3O4@LDH吸附磷酸三苯酯的吸附性能研究,磷酸三苯酯浓度为1.9mg/L,称取3mg/L吸附剂Urea-Fe3O4@LDH,搅拌速度为200rpm,吸附时间为6h,吸附完成后利用磁铁分离,测定剩余溶液中磷酸三苯酯的浓度。
(1)pH对Urea-Fe3O4@LDH吸附磷酸三苯酯的影响:使用HNO3或NaOH调节pH为3.0-8.0。
(2)离子强度对Urea-Fe3O4@LDH吸附磷酸三苯酯的影响:利用0.001M,0.01M和0.1MNaNO3模拟离子强度的影响,同时研究在不同pH下NaNO3的影响。
(3)有机物对Urea-Fe3O4@LDH吸附磷酸三苯酯的影响:腐植酸模拟有机物,腐植酸浓度在0-200mg/L,调节pH=7.5。
与现有技术相比,本发明具有如下优点:
本发明以尿素作为官能团,Fe3O4@LDH核壳材料为载体,制备Urea-Fe3O4@LDH吸附磷酸三苯酯,具有快速高效吸附的特性,并且能快速从水中分离。LDH作为壳层材料可以很好地负载官能团,并且减少离子强度对吸附磷酸三苯酯的影响。
附图说明
图1为材料Fe3O4,LDH,Fe3O4@LDH和Urea-Fe3O4@LDH的XRD图;
图2为实施例1中材料Fe3O4,LDH,Fe3O4@LDH和Urea-Fe3O4@LDH吸附磷酸三苯酯的去除率;
图3为实施例2中Urea-Fe3O4@LDH在不同pH下的吸附量;
图4为实施例3中Urea-Fe3O4@LDH在不同离子强度下的吸附量;
图5为实施例4中Urea-Fe3O4@LDH去除有机磷污染物乐果。
具体实施方式
本发明提供了一种利用制备的吸附剂Urea-Fe3O4@LDH吸附有机磷污染物磷酸三苯酯的应用,下面结合附图和实施例对本发明做进一步说明。
实施例1:材料Fe3O4,LDH,Fe3O4@LDH和Urea-Fe3O4@LDH吸附磷酸三苯酯的去除研究
磷酸三苯酯浓度为1.9mg/L,取溶液500mL置于烧杯中,分别加入3mg/L的Fe3O4,LDH,Fe3O4@LDH和Urea-Fe3O4@LDH,混合均匀,搅拌速度为200rpm,搅拌6h,利用磁铁进行分离,使用高效液相色谱测定溶液中磷酸三苯酯的浓度,并计算得到Urea-Fe3O4@LDH对磷酸三苯酯的去除率。
Fe3O4,LDH和Fe3O4@LDH去除率约为40%,吸附至少6h达到平衡,同时Urea-Fe3O4@LDH去除率可达90%以上,在2h时内可达平衡。具体如图2所示。
实施例2:材料Urea-Fe3O4@LDH去除磷酸三苯酯在不同pH下的吸附性能
磷酸三苯酯浓度为1.9mg/L,取溶液500mL置于烧杯中,使用HNO3或NaOH调节pH为3.0、4.0、5.0、6.0、7.0、8.0,称取3mg/L吸附剂Urea-Fe3O4@LDH,搅拌速度为200rpm,吸附时间为6h,吸附完成后利用磁铁分离,并计算得到Urea-Fe3O4@LDH对磷酸三苯酯的吸附量。
研究不同pH条件下Urea-Fe3O4@LDH去除TPhP的吸附量。随着pH值从3.0增加到5.5,Urea-Fe3O4@LDH对TPhP的吸附量逐渐增加;pH>5.5时,TPhP的吸附量缓慢降低。具体如图3所示。
实施例3:材料Urea-Fe3O4@LDH去除磷酸三苯酯在不同离子强度下的吸附性能
研究离子强度对Urea-Fe3O4@LDH吸附磷酸三苯酯的影响,磷酸三苯酯浓度为1.9mg/L,取溶液500mL置于烧杯中,使用HNO3或NaOH调节pH,在不同pH下(3.0、4.0、5.0、6.0、7.0、8.0)加入0.001M,0.01M和0.1M NaNO3,模拟离子强度的影响,同时研究在不同pH下NaNO3的影响。称取3mg/L吸附剂Urea-Fe3O4@LDH,搅拌速度为200rpm,吸附时间为6h,利用磁铁分离,测定剩余溶液中磷酸三苯酯的浓度,计算磷酸三苯酯的吸附量。
研究不同离子强度条件下Urea-Fe3O4@LDH对TPhP的吸附量。在未添加离子时,吸附量高,引入NaNO3后,吸附量降低,例如pH=5.时,Urea-Fe3O4@LDH对TPhP的吸附量为550mg/g,当离子强度增加到0.1M时,在相同的pH值条件下,对TPhP吸附量为464mg/L,吸附去除率减小约12%。溶液中NaNO3浓度从0.001M上升至0.1M时,对Urea-Fe3O4@LDH吸附TPhP效率影响较小。在不同pH下变化量均较小。具体如图4所示。
实施例4:材料Urea-Fe3O4@LDH去除有机磷农药乐果的效果研究
考察Urea-Fe3O4@LDH吸附有机磷农药乐果的去除率,利用乐果标准溶液配置,浓度为2.0mg/L,称取3mg/L吸附剂Urea-Fe3O4@LDH,搅拌速度为200rpm,吸附时间为6h,利用磁铁分离,测定剩余溶液中乐果的浓度,计算乐果的去除率。
研究了Urea-Fe3O4@LDH对乐果的去除率,吸附时间为6h。Urea-Fe3O4@LDH去除率可达到85%,在4h时内完成吸附。具体如图5所示。
上述实施例对本发明的技术方案进行了详细说明。显然,本发明并不局限于所描述的实施例。基于本发明中的实施例,熟悉本技术领域的人员还可据此做出多种变化,但任何与本发明等同或相类似的变化都属于本发明保护的范围。
Claims (10)
1.一种尿素官能团化磁性吸附材料Urea-Fe3O4@LDH的制备方法,其特征在于,包括以下步骤:
(1)Fe3O4@LDH的制备:将Fe3O4纳米颗粒超声分散在去离子水中,与NaOH和Na2CO3混合均匀,在搅拌下滴加Mg(NO3)2·6H2O和Al(NO3)3·9H2O混合溶液,搅拌,保持pH=10;静置后,取出上清液并加入乙二醇,搅拌,将混合物进行水热反应,将得到的固体洗涤至中性,干燥后,研磨得到Fe3O4@LDH粉末;
(2)Urea-Fe3O4@LDH的制备:将步骤(1)所得Fe3O4@LDH分散在乙醇中,加入3-氨丙基三乙氧基硅烷,回流,洗涤干燥后得到NH2-Fe3O4@LDH;将得到的材料分散到四氢呋喃中,加入对甲苯基异氰酸酯,进行后处理,得到Urea-Fe3O4@LDH。
2.根据权利要求1所述的方法,其特征在于,步骤(1)中所述混合溶液的Mg2+/Al3+=3/1。
3.根据权利要求1所述的方法,其特征在于,步骤(1)中所述水热反应在反应釜内于110℃,保持12h进行反应。
4.根据权利要求1所述的方法,其特征在于,步骤(1)中所述干燥的温度是60℃。
5.根据权利要求1所述的方法,其特征在于,步骤(2)中所述回流在80℃下进行10h。
6.根据权利要求1所述的方法,其特征在于,步骤(2)中所述后处理包括在室温下进行搅拌24h,使用乙醇和水进行洗涤,在60℃进行干燥。
7.使用权利要求1所述方法制备的Urea-Fe3O4@LDH吸附有机磷的应用,其特征在于,将Urea-Fe3O4@LDH吸附剂加入有机磷溶液中,调节pH,搅拌,吸附完成后利用磁铁分离。
8.根据权利要求7所述的应用,其特征在于,所述有机磷溶液是磷酸三苯酯或乐果。
9.根据权利要求7所述的应用,其特征在于,所述调节pH使用HNO3或NaOH调节pH为3.0-8.0。
10.根据权利要求7所述的应用,其特征在于,所述搅拌的时间为6h。
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