CN112355041B - 一种用于治理砷污染的超稳矿化剂的制备方法及应用 - Google Patents
一种用于治理砷污染的超稳矿化剂的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种用于治理砷污染的超稳矿化剂的制备方法及应用。所述的超稳矿化剂是通过旋转液膜反应器将钙盐、铁盐及碱进行共沉淀反应制得,然后将其用于去除废水中砷及重金属砷污染土壤的治理修复。本发明所制备的超稳矿化剂具有非常高的活性,通过缺陷位锚定的方式能够快速的将土壤中的砷矿化形成具有更为稳定结构的矿物形式,稳定性远超氢氧化物和碳酸盐,表现出超稳矿化态,解决了砷再次游离的难题。本发明的用于治理砷污染的超稳矿化剂及修复方法具有较高的经济和环保价值,能够在取得优异修复效果的同时有效降低成本。
Description
技术领域:
本发明属于水/土污染处理技术领域,特别涉及一种用于治理砷污染的超稳矿化剂的制备方法及应用。
背景技术:
据世界卫生组织公布,全球至少有5000多万人口正面临着地方性砷中毒的威胁,其中,大多数为亚洲国家,而中国正是受砷中毒危害最为严重的国家之一。近年来,砷污染越来越严重,其数量和危害程度呈日益上升的趋势。
砷污染主要的来源是工业来源和农业来源。工业来源主要是一些冶金企业废水废料的违规排放和化工企业废水废渣的排放。而农业砷排放来源则主要在农药和化肥的滥用。砷作为一种非金属的重金属元素,和汞、磷等具有一定的毒性,一般用来作为农业生产的农药和化肥。但是在大量使用这些农药和化肥的时候,农药和化肥中本来安全含量的砷则短时间在同个地区浓度迅速升高就造成一定的毒性,造成土壤和水体的污染。
随着冶金、化工等产业的日益发展,以及含砷制品市场的日益拓大,含砷废水的排放和污染问题,必将影响到人们的生活水平的提高,影响到人类生存环境的改善,所以解决砷污染问题已迫在眉睫。
在含砷废水处理方面,主要有中和沉淀法、絮凝沉淀法、铁氧体法、硫化物沉淀法等,这些方法适用于高浓度含砷废水,产生大量的固废,且难以达到国家对含砷废水的排放要求。膜过滤、反渗透、电化学等方法能够达标排放但成本高昂,难以实现大规模应用。
在砷污染土壤方面,2014年我国环境保护部和国土资源部首次联合发布的《全国土壤污染状况调查公报》显示:我国土壤污染总超标率高达16.1%,其中砷超标率达到2.7%。在现有技术中,主要有淋洗法,电动修复法,植物修复法,原位钝化法等,其中原位钝化策略是通过原位添加钝化剂,使土壤中重金属的赋存形态发生变化,由生物有效性高的活性态转化为生物有效性低的稳定态,从而降低其在土壤中的迁移性和生物可利用性,达到修复的目的。该技术在修复效果、操作灵活性、经济性、大规模应用方面更具竞争力,也得到了国家主管部门的重点推荐和行业的青睐。目前市场上常见的钝化剂主要依靠材料的静电引力和表面吸附作用实现对砷离子的钝化,这种钝化方式作用力较弱,易受外界条件的影响,导致污染物脱附再次形成污染。
因此,基于以上分析,具有高效、易操作、成本低、绿色化特点的砷处理材料的制备极为必要。
发明内容:
本发明提供了一种用于治理砷污染的超稳矿化剂的制备方法,并将其用于去除废水中砷及重金属砷污染土壤的治理修复。所述的超稳矿化剂是通过旋转液膜反应器将钙盐、铁盐及碱进行共沉淀反应制得。该制备方法过程便捷,原料广泛,所制备的超稳矿化剂具有非常高的活性,通过缺陷位锚定的方式能够快速的将土壤中的砷矿化形成具有更为稳定结构的矿物形式,其溶度积比相应氢氧化物或碳酸盐的溶度积常数小数十个数量级,稳定性远超氢氧化物和碳酸盐,表现出超稳矿化态。因此,解决了砷再次游离的难题。本发明的砷污染超稳矿化剂及修复方法具有较高的经济和环保价值,能够在取得优异修复效果的同时有效降低成本。
本发明所述的用于治理砷污染的超稳矿化剂的制备方法如下:
a)将钙盐和铁盐溶于去离子水中得到混合盐溶液;另外配制碱溶液;混合盐溶液中钙离子的浓度为0.05-0.5mol/L,钙离子与铁离子的物质的量之比为1.5-4.0,碱溶液中碱的物质的量为混合盐溶液中总金属离子物质的量的1.2-2倍;
b)将混合盐溶液和碱溶液同时加入旋转液膜反应器中,共混反应后将所得浆液离心,去离子洗涤、干燥即得超稳矿化剂。
上述步骤b)得到的浆液增加晶化过程,然后离心、去离子水洗涤、干燥得到超稳矿化剂。
所述的钙盐选自氯化钙、硝酸钙中的一种或两种。
所述的铁盐选自硫酸铁、硝酸铁、氯化铁中的一种或几种。
所述的碱选自氢氧化钠、氢氧化钾、氨水中的一种或几种。
将上述制备的超稳矿化剂用于处理含砷废水的应用。所述的处理含砷废水的具体操作为:将超稳矿化剂加入含砷废水中,超稳矿化剂的加入量为含砷废水中As的质量的1.1-50倍,含砷废水的pH≥3.5,在4-60℃温度下搅拌处理4-24小时达到去除平衡,将超稳矿化剂分离。
将上述制备的超稳矿化剂用于处理砷污染土壤的应用。所述的处理砷污染土壤的具体操作为:将超稳矿化剂加入到砷污染土壤中,超稳矿化剂的加入量与砷污染土壤的质量比为1:10-1:400,混合均匀,加水,保持土壤含水量在20-80%之间。
在上述含砷污染物处理过程中,超稳矿化剂中丰富的金属缺陷位与砷间形成多种类化合键,实现对砷的高效去除。使用该超稳矿化剂可快速将初始浓度为20mg/L的含砷废水中的砷的浓度降至0.007mg/L,达到饮用水的要求;在含砷土壤处理过程中,加入该超稳矿化剂,土壤中砷的固定率达到90%以上。
本发明的有益效果:
(1)材料制备过程简单,高效。反应物在微液膜反应器中形成微米尺度厚的微液膜促使反应物快速、充分反应,晶核迅速形成,同时在高切向力的作用下产物快速脱离反应器,可实现材料的稳定、连续合成,为材料的快速批量化制备奠定基础。
(2)所制备的超稳矿化剂中的钙在使用过程中会有部分游离至介质中,形成丰富的缺陷位,为砷的矿化提供了更多的反应活性位点,提高了效率。
(3)由于超稳矿化剂与砷之间强的化学键作用,可快速将废水中As的含量降至国家要求以下,通过条件优化可以达到饮用水对砷含量的要求(<0.01mg/L)。
附图说明:
图1为实施例1制备的超稳矿化剂的XRD图。
图2为实施例2制备的超稳矿化剂去除砷过程中的时间-去除率曲线图。
具体实施方式:
为了使相关人员更好的理解本发明的操作方式,下面通过具体实施例对本发明作进一步说明,但本发明的保护范围并不局限于此。
实施例1:
超稳矿化剂的制备:称取23.6g Ca(NO3)2·4H2O和20.2g Fe(NO3)3·9H2O溶于500ml去离子中得到溶液A;称取9.6g NaOH溶于500ml的去离子水中得到溶液B;将溶液A,溶液B同时快速加入转速为3000r/min旋转液膜反应器中,出料口收集浆料,去离子水离心洗涤后40℃干燥12小时即可。图1为所制备材料的XRD图,由图可以看出所制备的钙铁超稳矿化剂呈现出层状材料的结构特征,且无碳酸钙、氢氧化钙等物质的衍射峰。
超稳矿化剂对水中砷的去除:称取0.05g超稳矿化剂于100mL的烧杯中,加入50ml含***的水溶液,其中砷的浓度为20mg/L,室温下磁力搅拌4小时后,取上层溶液后用0.22μm的过滤膜过滤后通过ICP-MS测其中砷的浓度。结果表明,溶液中砷的浓度为0.04mg/L,超稳矿化剂对砷的去除达到99.8%,展示出极高的效率。
实施例2:
超稳矿化剂的制备:称取23.6g Ca(NO3)2·4H2O和12.2g Fe(NO3)3·9H2O溶于500ml去离子中得到溶液A,称取9.6g NaOH溶于500ml的去离子水中得到溶液B,将溶液A,溶液B同时快速加入转速为3000r/min旋转液膜反应器中,出料口收集浆料,去离子水离心洗涤后40℃干燥12小时即可。
超稳矿化剂对水中砷的去除:称取0.05g超稳矿化剂于100mL的烧杯中,加入50ml含***的水溶液,其中砷的浓度为20mg/L,40℃下磁力搅拌4小时后,取上层溶液后用0.22μm的过滤膜过滤后通过ICP-MS测其中砷的浓度。结果表明,溶液中砷的浓度为0.01mg/L,超稳矿化剂对砷的去除达到99.95%(图2)。
实施例3:
超稳矿化剂的制备:称取23.6g Ca(NO3)2·4H2O和12.2g Fe(NO3)3·9H2O溶于500ml去离子中得到溶液A,称取9.6g NaOH溶于500ml的去离子水中得到溶液B,将溶液A,溶液B同时快速加入转速为3000r/min旋转液膜反应器中,出料口收集浆料,去离子水离心洗涤后40℃干燥12小时即可。
超稳矿化剂对土壤中砷的固定:取1000g预处理的土样与20g超稳矿化剂在1L的烧杯中充分混合后加入500ml去离子水后自然放置,每间隔一定时间取样后采用CaCl2法测其生物有效态。修复7天后砷的有效态含量由0.282mg/kg降至0.013mg/kg,下降幅度达95.4%,表现出优异的钝化性能。
Claims (2)
1.一种用于治理砷污染的超稳矿化剂的制备方法,其特征在于,所述制备方法的具体步骤为:
a)将钙盐和铁盐溶于去离子水中得到混合盐溶液;另外配制碱溶液;混合盐溶液中钙离子的浓度为0.05-0.5mol/L,钙离子与铁离子的物质的量之比为1.5-4.0,碱溶液中碱的物质的量为混合盐溶液中总金属离子物质的量的1.2-2倍;
b) 将混合盐溶液和碱溶液同时加入反应器中,共混反应后将所得浆液晶化,然后离心、去离子水洗涤、干燥得到超稳矿化剂;
所述的钙盐选自氯化钙、硝酸钙中的一种或两种;
所述的铁盐选自硫酸铁、硝酸铁、氯化铁中的一种或几种;
所述的碱溶液选自氢氧化钠溶液、氢氧化钾溶液、氨水中的一种或几种。
2.根据权利要求1所述的方法制备得到的超稳矿化剂用于处理含砷废水及砷污染土壤中的应用。
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