CN116603503A - 一种壳聚糖凝胶包裹载钙活性炭的除磷微粒及其制备方法 - Google Patents
一种壳聚糖凝胶包裹载钙活性炭的除磷微粒及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种壳聚糖凝胶包裹载钙活性炭的除磷微粒及其制备方法,属于环境材料制备技术领域。所述制备方法包括以下步骤:活性炭粉与氢氧化钙混合得到载钙活性炭,所述载钙活性炭与壳聚糖和醋酸形成混合溶液,将所述混合溶液加入到氢氧化钠与无水乙醇的混合溶液中形成凝胶,所述凝胶再与戊二醛交联固化,经洗涤、烘干和研磨,得到除磷微粒。所述除磷微粒具有稳定性强、能重复利用和制备工艺简单等特点,用于废水中磷的去除,效果表现优异。
Description
技术领域
本发明公开了一种壳聚糖凝胶包裹载钙活性炭的除磷微粒及其制备方法,属于环境材料制备技术领域。
背景技术
活性炭是一种高度多孔的吸附材料,由于其具有较高的表面积和孔隙度,因此在许多领域都有广泛的应用。活性炭可以用于净化自来水、废水和工业水。它可以去除异味、有机污染物和重金属等有害物质,以提高水的质量。活性炭常用于废水的深度处理过程,但是,活性炭单独应用深度除磷效果不佳,通常需要对活性炭进行改性来优化其除磷性能。传统金属氧化物和氢氧化物被广泛用于提高传统吸附剂的磷吸附性能,其中Ca(OH)2作为一种来源广泛、廉价易得的改性剂用于磷去除研究中。而通过钙盐改性的活性炭存在吸附效果差和结构不稳定等问题。
发明内容
针对现有技术的不足,本发明的目的在于提供一种壳聚糖凝胶包裹载钙活性炭的除磷微粒及其制备方法,用于解决活性炭对于水体中磷吸附效率低以及改性后结构不稳定等问题。具体地,本发明的目的可以通过以下技术方案实现:
活性炭经预处理得到活性炭粉;
所述活性炭粉、氢氧化钙和去离子水混合,经恒温振荡、真空抽滤和烘干,得到载钙活性炭;
所述载钙活性炭加入到溶解有壳聚糖的醋酸溶液中形成混合溶液;
所述混合溶液加入到含有氢氧化钠和无水乙醇的溶液中,形成凝胶;
所述凝胶与戊二醛混合,经固化、洗涤、烘干和研磨,得到除磷微粒。
进一步地,所述活性炭粉、氢氧化钙和去离子水的重量比包括1:0.37:10。
进一步地,所述恒温振荡是在温度为25℃、转速为180rpm/min的条件下处理24h。
进一步地,所述活性炭粉、氢氧化钙和去离子水混合后的烘干温度为105℃。
进一步地,所述醋酸的质量浓度为2%。
进一步地,所述氢氧化钠的浓度为3mol/L。
进一步地,所述氢氧化钠和无水乙醇的体积比为3:1。
进一步地,所述凝胶和戊二醛混合后烘干的温度为65℃。
进一步地,所述洗涤是用去离子水洗涤至pH值为7。
进一步地,所述除磷微粒的结构包括活性炭表面结合钙离子,壳聚糖包裹所述表面带有钙离子的活性炭。
进一步地,所述除磷微粒在废水中的加入量为每一升废水加入0.2~0.6g。
本发明的有益效果:
(1)本发明采用壳聚糖凝胶包裹法,有效固定了载钙活性炭的有效成分,能够得到有效和稳定的除磷微粒,制作方法简单有效。
(2)本发明制备的壳聚糖凝胶包裹载钙活性炭微粒,集中了壳聚糖、活性炭、钙的优点,吸收速率快,且对于磷的吸附容量大。
(3)本发明制备的除磷微粒,在废水中应用后,通过酸解吸再生并循环利用,除磷率依然能保持在80%以上,表明除磷微粒的重复利用效果良好,节约资源和成本。
(4)本发明的除磷微粒在浓度0.2g/L~0.6g/L时,除磷效率高的同时,能保持所述除磷微粒的吸附能力,综合利用率最高。
附图说明
图1为实施例1中的活性炭微观图。
图2为实施例1的除磷微粒微观图。
图3为实施例2除磷微粒和粉末活性炭的吸附动力学曲线图:图中,Ca-PAC@CTS表示本发明的除磷微粒,RawPAC表示活性炭。
图4为实施例3的吸附材料投加量对除磷微粒吸附磷酸盐的效果图。
图5为实施例4经过5次循环利用的除磷微粒对磷酸盐去除率的效果图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清晰、完整地描述,显然,所描述的实施例仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创新性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
一种壳聚糖凝胶包裹载钙活性炭的除磷微粒及其制备方法,包括以下步骤:
(1)称取10g活性炭至于100mL去离子水中,置于恒温摇床(温度25℃,转速180rpm/min)中振荡24h后取出,经真空抽滤后,置于105℃烘干,得到预处理后的活性炭粉,储存备用。
(2)称取10g预处理后的活性炭粉和3.7g氢氧化钙,加入100mL去离子水后置于恒温摇床中,以25℃、180rpm/min的转速振荡24h后取出,经真空抽滤后,置于105℃烘箱中烘干,得到载钙活性炭。
(3)称取3g壳聚糖溶于100mL质量浓度为2%的醋酸溶液中,待完全溶解后加入9g载钙活性炭,充分搅拌1h以实现完全混合。
(4)配置400mL的混合溶液(3mol/L的氢氧化钠溶液300mL+100mL无水乙醇),将步骤(3)得到的混合溶液缓慢加入溶液中形成凝胶,接着加入4mL戊二醛交联固化1h,用去离子水洗涤至中性后置于65℃烘箱中烘干,用研磨机研磨多次后得到除磷微粒,除磷微粒的结构如图2所示,实验中用到的活性炭结构如图1所示。
实施例2:
一种壳聚糖凝胶包裹载钙活性炭的除磷微粒的应用,包括以下步骤:
称取0.01g除磷微粒于100mL锥形瓶中,锥形瓶中加入100mL浓度为1mg/L的KH2PO4溶液(调节pH=7±0.1),封紧锥形瓶塞后置于恒温振荡器中以180rpm/min的转速在25℃恒温下振荡24h后,测定溶液中剩余的磷浓度。从图3可以看出,吸附均在2h内达到平衡。同时,可以看出吸附过程大致分为两个阶段:在第一阶段约30分钟内,除磷微粒吸附了溶液中80%以上的磷酸盐;第二阶段吸附效率逐渐缓慢直至吸附达到平衡。图3显示了除磷微粒和活性炭粉的吸附动力学曲线,可以看出活性炭粉本身吸附磷酸盐的速度就比较快,这可能是由于活性炭粉自身具有较大的比表面积和发达的孔隙结构,能够提供大量吸附位点,但原始活性炭粉的吸附容量较低。在引入壳聚糖和钙改性之后,除磷微粒表面的静电吸引作用和引入的羟基也增加了与磷酸盐配体交换的活性位点,因此除磷微粒对磷酸盐的去除可以在较短时间内达到平衡,显著提升了磷吸附容量。
实施例3:
一种壳聚糖凝胶包裹载钙活性炭的除磷微粒的应用,包括以下步骤:
分别称取0.01~0.1g的除磷微粒于100mL锥形瓶中,锥形瓶中加入100mL浓度为1mg/L的KH2PO4溶液(调节pH=7±0.1),封紧锥形瓶塞后置于恒温振荡器中以180rpm/min的转速在25℃恒温下振荡24h后,测定溶液中剩余的磷浓度,得到投加量与磷吸附容量的关系图。吸附材料投加量对除磷微粒吸附磷酸盐的影响如图4所示。随着除磷微粒的投加量从0.4g/L增加到1.0g/L,除磷微粒对磷酸盐的吸附量从1.875mg-P/g逐渐减小到0.94mg-P/g,而溶液中磷酸盐的去除率从77.44%增大到93.48%。用互穿网络水凝胶吸附磷酸盐时发现随着水凝胶的投加量从0.05g增加到0.25g时,吸附剂对磷酸盐的吸附量从16.51mg-P/g减小到7.76mg-P/g,而溶液中磷酸盐的去除率从41.01%增加到95.37%。随着除磷微粒投加量的增加,溶液中提供了更多的吸附位点,因此磷酸盐的去除率随之增加。但除磷微粒投加量的过度也会造成部分吸附位点被覆盖,吸附位点之间产生竞争,所以单位质量的除磷微粒的吸附能力随着吸附剂投加量的增大而降低,因此,除磷微粒在浓度0.2g/L~0.6g/L时,除磷效率高的同时,能保持所述除磷微粒的吸附能力,综合利用率最高。
实施例4:
一种壳聚糖凝胶包裹载钙活性炭的除磷微粒的应用,包括以下步骤:
吸附试验完成后,将吸附后的微颗粒材料经真空抽滤后,用去离子水清洗若干次,置于60℃烘箱中干燥。称取0.1g吸附剂于100mL锥形瓶中,加入100mL浓度为0.01~0.05M的稀H2SO4溶液,在180rpm/min和25℃的条件下振荡0.5h。反应结束后,测定上清液中的磷浓度,实现吸附剂再生。使用回收的固体残留物重新制备除磷微粒,经过5个解吸-再制备-再利用的循环,结果如图5所示,除磷微粒对磷酸盐的去除率仍保持在80%左右,表明经稀硫酸解吸后剩余的固体残余物,被回收再次制备成除磷微粒,依然具有很高的吸附性能,重复利用效果良好,能节约资源和成本。
以上所述的实施例对本发明的技术方案和有益效果进行了详细说明,应理解的是以上所述仅为本发明的具体实施例,并不用于限制本发明。凡在本发明的原则范围内所做的任何修改、补充和等同替换等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种除磷微粒,其特征在于,所述除磷微粒的原料包括:活性炭粉、氢氧化钙、去离子水、壳聚糖、醋酸、氢氧化钠、无水乙醇和戊二醛。
2.根据权利要求1所述的除磷微粒,其特征在于,所述活性炭粉、氢氧化钙和去离子水的重量比为1:0.37:10。
3.根据权利要求1所述的除磷微粒,其特征在于,所述微粒的结构包括活性炭表面结合钙离子,壳聚糖包裹所述表面结合钙离子的活性炭。
4.一种除磷微粒的制备方法,其特征在于,所述方法包括以下步骤:
活性炭经预处理得到活性炭粉;
所述活性炭粉、氢氧化钙和去离子水混合,经恒温振荡、真空抽滤和烘干,得到载钙活性炭;
所述载钙活性炭加入到溶解有壳聚糖的醋酸溶液中形成混合溶液;
所述混合溶液加入到含有氢氧化钠和无水乙醇的溶液中,形成凝胶;
所述凝胶与戊二醛混合,经固化、洗涤、烘干和研磨,得到除磷微粒。
5.根据权利要求4所述的方法,其特征在于,所述氢氧化钠的浓度为3mol/L。
6.根据权利要求4所述的方法,其特征在于,所述氢氧化钠和无水乙醇的体积比为3:1。
7.根据权利要求4所述的方法,其特征在于,所述洗涤是用去离子水洗涤至pH值为7。
8.根据权利要求4所述的方法,其特征在于,所述凝胶与戊二醛混合后烘干的温度为65℃。
9.通过权利要求4~8任一所述方法获得的除磷微粒。
10.权利要求1、2、3或9任一所述的除磷微粒在废水除磷中的应用,其特征在于,所述除磷微粒在废水中的加入量为每一升废水加入0.2~0.6g。
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