CN111533360A - 一种含铬废水的处理方法 - Google Patents
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Abstract
本发明公开了一种含铬废水的处理方法,包括如下步骤:步骤一)、取六价铬废水并调节pH值为1.0~7.0;步骤二)、向六价铬废水中加入磁性复合材料得到混合溶液,磁性复合材料与六价铬废水的质量体积比为0.1~10:1000g/ml;步骤三)、混合溶液加入转速为100rpm~300rpm的恒温振荡器,并处于光催化反应器的光照下反应0.5~24h,并控制反应温度为10℃~50℃;然后将磁性复合材料利用磁铁从混合溶液中分离,完成对六价铬废水中六价铬的去除。本发明首针对目前植物修复后废弃红麻生物质的资源化利用及六价铬污染公开了一种安全、经济、高效的含铬废水处理方法。
Description
技术领域
本发明属于功能材料领域,涉及土壤重金属镉污染修复后的红麻废弃生物质在废水处理领域中的资源化应用,尤其涉及一种磁性生物炭复合材料在处理重金属废水中的应用。
背景技术
重金属污染是当今较为严重的污染问题。近年来,植物修复技术每年产生的废弃生物质,传统的焚烧、填埋等技术,可能会使得重金属重新进入环境,造成二次污染的发生。因此,开发废弃生物质的资源化利用途径具有重要的现实意义。
生物炭是一种很有前途的吸收各种化学污染物的吸附剂,生物炭在某些情况下可以像活性炭一样有效,但成本要低得多。首先,生物炭的高有机碳(OC)含量和大表面积(SA)通过疏水分区和孔隙填充为农药提供了丰富的吸附位点。此外,它们的芳香性、表面官能团和负表面电荷可能通过特定的相互作用增强对农药的吸附。
目前,TiO2因具有氧化能力强、催化活性高、性质稳定、价廉无毒等特点,被广泛应用于废水处理、空气净化、杀菌自洁等方面。但是,由于TiO2的禁带宽度为3.2eV,对可见光的利用效率低。铁酸铋(BiFeO3)是一种新型的窄带隙半导体,在受到波长小于等于610nm的可见光照射时,价带电子将被激发,产生具有高活性的光生空穴和光生电子,因此具有较强的反应活性,其本身具有磁性,还易于回收和多次重复使用,因此在可见光催化方面具有广泛的应用前景。而生物炭作为生物质热解后的产物,其自身是一种良好的吸附剂被广泛的应用于废水处理。因此,利用植物修复后的废弃生物质制备生物炭与铁酸铋的复合材料,可为废弃生物质的资源化利用提供新的思路。
发明内容
为解决上述问题,本发明公开了一种含铬废水的处理方法。本发明首针对目前植物修复后废弃富镉红麻生物质的资源化利用及六价铬污染公开了一种安全、经济、高效的含铬废水处理方法。
为解决上述技术问题,本发明的技术方如下:
一种含铬废水的处理方法,包括如下步骤:
步骤一)、取六价铬废水并调节pH值为1.0~7.0;
步骤二)、向六价铬废水中加入磁性复合材料得到混合溶液,磁性复合材料与六价铬废水的质量体积比为0.1~10:1000g/ml;
步骤三)、混合溶液加入转速为100rpm~300rpm的恒温振荡器,并处于光催化反应器的光照下反应0.5~24h,并控制反应温度为10℃~50℃;然后将磁性复合材料利用磁铁从混合溶液中分离,完成对六价铬废水中六价铬的去除。
进一步的改进,所述步骤一)中pH值为2.0~6.0;步骤三)中,恒温振荡器内的反应时间为1h~8h,反应温度为30~40℃。
进一步的改进,所述pH值为2.0。
进一步的改进,所述光催化反应器为氙灯,光电流设置为15A。
进一步的改进,所述磁性复合材料为BiFeO3/生物炭磁性复合材料,BiFeO3/生物炭磁性复合材料的制作方法如下:
步骤一、采集富镉红麻生物质,取富镉红麻生物质去皮后的茎,清洗、干燥,然后粉碎得到粉末产物;
步骤二、将粉末产物浸泡在0.05-0.2mol/L的NaOH溶液中,70-90℃水浴加热搅拌5-30min,然后加入浓度为0.15-0.2mol/L的Bi(NO3)3溶液和浓度为0.15-0.2mol/L的Fe(NO3)3溶液,80-90℃下水浴加热并搅拌1-60分钟,然后调节pH到7.0-7.5后得到混合液,混合液烘干得到BiFeO3/红麻生物质耦合材料;其中粉末产物与NaOH溶液的质量体积比为10-50:500-1000g/ml;NaOH溶液、Bi(NO3)3溶液和Fe(NO3)3溶液的体积比为500-1000:100-250:100-250;
步骤三、取BiFeO3/红麻生物质耦合材料,在真空管式炉内以50-200mL/min的流速通入氮气,以5-10℃/min的速度升高温度至300-500℃后保持温度热解1-5h,然后继续保持氮气流通条件下冷却至室温得到热解后产物,热解后的产物过50-200目筛子,制得BiFeO3/生物炭磁性复合材料。
进一步的改进,所富镉红麻生物质通过吸附土壤中的镉得到。
进一步的改进,所述步骤一中,所述红麻生物质去皮后的茎,清洗、干燥,然后粉碎过直径为0.1-3.0mm的筛子到粉末产物。
进一步的改进,所述步骤二中,搅拌速度为200-350rpm。
进一步的改进,所述步骤二中,混合液在70-110℃下烘干得到BiFeO3/红麻生物质耦合材料。
与现有技术相比,本发明的优点在于:
1.采用磁性复合材料处于含铬废水,吸附性好,且容易将处理后废水与吸附铬的复合材料快速分离回收;
2.本发明使用的BiFeO3/生物炭磁性复合材料,其原料成本低,经济性好,主要原料为土壤重金属镉污染植物修复后的红麻生物质,而氢氧化钠和硝酸铋、硝酸铁为常用的化工材料。
3.富镉红麻生物质中的镉在材料制备过程中,通过反应条件的控制,镉转化为具备光催化性能的CdS与CdO形态。
4.将BiFeO3/生物炭磁性复合材料直接加入反应器中进行吸附反应,整个工艺过程简单而容易操作,因为经过铁酸铋改性的生物炭具有磁性,因此要将耦合材料分离出来再利用也是便利的。
5.本发明的方法能对含有六价铬的废水实施有效处理,为重金属废水的处理提供的新的途径。
附图说明
图1为本发明实施例1的BiFeO3生物炭磁性复合材料对不同初始浓度六价铬的去除变化曲线图;
图2是本发明实施例2的BiFeO3生物炭磁性复合材料在不同pH值条件下对废水中六价铬的吸附变化曲线图。
具体实施方式
以下将结合具体实施例对本发明做进一步详细说明
实施例1:
本发明具体包括如下步骤:
1.BiFeO3/生物炭磁性复合材料的制备
在温度为25℃的光照培养室中开展土壤镉污染修复盆栽实验,取已钝化一年的富镉土壤分装到实底花盆中,其中土壤中的镉浓度为20mg/L,红麻通过种子播种,第一次播种后浇湿表层土壤,待出苗后,打开光源,控制光强为4000LX,待含水量低于12%,浇透土壤,培养3个月后,采集富镉红麻生物质,取去皮后的茎,清洗,在烘箱内以85℃干燥,剪碎后用粉碎机粉碎,过1.5mm筛子,取20g过筛的红麻生物质粉末并浸泡于500ml的浓度为0.1mol/L的NaOH溶液中,在90℃水浴加热搅拌5分钟。取0.15mol/L的Bi(NO3)3和Fe(NO3)3各取250ml并在三口烧瓶内混合,加入先前的NaOH和红麻粉末的混合液。在90℃下水浴加热,以350rpm搅拌30分钟。完成后将混合液从三颈烧瓶中倒出,调节pH到7.5。将混合液置于烘箱内以85℃烘干,制得BiFeO3/红麻生物质耦合材料。
将制得的BiFeO3/红麻生物质耦合材料置于真空管式炉内以100ml/min的流速通入氮气,以5℃/min的速度升高温度至350℃,温度升到指定温度后保持温度,热解3h后得到的产物在继续保持氮气流通条件下冷却至室温。热解后的产物过200目筛子,制得BiFeO3/生物炭磁性复合材料。
2.对六价铬废水的处理
配置浓度5、10、20,40mg/L的六价铬废水,用硝酸或者氢氧化钠调节pH值为2。将上述方法制得的BiFeO3/生物炭磁性复合材料添加到六价铬废水中。每升废水添加的BiFeO3/生物炭磁性复合材料为1.0g。将以上反应系统置于氙灯下,光电流设置为15A,150rpm/min磁力搅拌废水。光催化5小时候利用磁铁将BiFeO3/生物炭磁性复合材料从溶液中分离,完成对六价铬废水的处理。溶液中剩余的六价铬离子的浓度使用紫外分光光度法进行测定。计算的六价铬去除率结果见图1。由图1可知,BiFeO3/生物炭磁性复合材料对六价铬的去除率随着初始浓度的升高而降低,主要原因可能是BiFeO3/生物炭磁性复合材料的吸附位点及产生的光催化活性物质有限。
利用BiFeO3/生物炭磁性复合材料去除废水中六价铬的方法,包括以下步骤:
1.BiFeO3/生物炭磁性复合材料的制备
本步骤与实施例1的步骤1相同。
2.对六价铬废水进行处理
取上述方法制得的复合材料0.01g、0.02g、0.03g、0.04g、005g分别添加到pH值为2的200mL六价铬废水中,六价铬离子的初始浓度为10mg/L。将以上反应系统置于光催化氙灯下,搅拌并启动氙灯,氙灯光源电流设置为15A,光催化5小时后利用磁铁将BiFeO3/生物炭磁性复合材料从溶液中分离,完成对六价铬废水的去除。溶液中剩余的六价铬离子的浓度使用紫外分光光度法进行测定,实验结果如图2所示。实验数据显示,当BiFeO3/生物炭磁性复合材料的投加量越大时,对溶液中六价铬的去除能力越强。
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 (9)
1.一种含铬废水的处理方法,其特征在于,包括如下步骤:
步骤一)、取六价铬废水并调节pH值为1.0~7.0;
步骤二)、向六价铬废水中加入磁性复合材料得到混合溶液,磁性复合材料与六价铬废水的质量体积比为0.1~10:1000g/ml;
步骤三)、混合溶液加入转速为100rpm~300rpm的恒温振荡器,并处于光催化反应器的光照下反应0.5~24h,并控制反应温度为10℃~50℃;然后将磁性复合材料利用磁铁从混合溶液中分离,完成对六价铬废水中六价铬的去除。
2.如权利要求1所述的含铬废水的处理方法,其特征在于,所述步骤一)中pH值为2.0~6.0;步骤三)中,恒温振荡器内的反应时间为1h~8h,反应温度为30~40℃。
3.如权利要求2所述的含铬废水的处理方法,其特征在于,所述pH值为2.0。
4.如权利要求1所述的含铬废水的处理方法,其特征在于,所述光催化反应器为氙灯,光电流设置为15A。
5.如权利要求1所述的含铬废水的处理方法,其特征在于,所述磁性复合材料为BiFeO3/生物炭磁性复合材料,BiFeO3/生物炭磁性复合材料的制作方法如下:
步骤一、采集富镉红麻生物质,取富镉红麻生物质去皮后的茎,清洗、干燥,然后粉碎得到粉末产物;
步骤二、将粉末产物浸泡在0.05-0.2mol/L的NaOH溶液中,70-90℃水浴加热搅拌5-30min,然后加入浓度为0.15-0.2mol/L的Bi(NO3)3溶液和浓度为0.15-0.2mol/L的Fe(NO3)3溶液,80-90℃下水浴加热并搅拌1-60分钟,然后调节pH到7.0-7.5后得到混合液,混合液烘干得到BiFeO3/红麻生物质耦合材料;其中粉末产物与NaOH溶液的质量体积比为10-50:500-1000g/ml;NaOH溶液、Bi(NO3)3溶液和Fe(NO3)3溶液的体积比为500-1000:100-250:100-250;
步骤三、取BiFeO3/红麻生物质耦合材料,在真空管式炉内以50-200mL/min的流速通入氮气,以5-10℃/min的速度升高温度至300-500℃后保持温度热解1-5h,然后继续保持氮气流通条件下冷却至室温得到热解后产物,热解后的产物过50-200目筛子,制得BiFeO3/生物炭磁性复合材料。
6.如权利要求5所述的含铬废水的处理方法,其特征在于,所富镉红麻生物质通过吸附土壤中的镉得到。
7.如权利要求5所述的含铬废水的处理方法,其特征在于,所述步骤一中,所述红麻生物质去皮后的茎,清洗、干燥,然后粉碎过直径为0.1-3.0mm的筛子到粉末产物。
8.如权利要求5所述的含铬废水的处理方法,其特征在于,所述步骤二中,搅拌速度为200-350rpm。
9.如权利要求5所述的含铬废水的处理方法,其特征在于,所述步骤二中,混合液在70-110℃下烘干得到BiFeO3/红麻生物质耦合材料。
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