CN114192110A - 一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂及其制备方法 - Google Patents
一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂及其制备方法 Download PDFInfo
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- CDJXAEDCBYDKBW-UHFFFAOYSA-M aluminum iron(2+) oxygen(2-) hydroxide Chemical compound [OH-].[O-2].[Al+3].[Fe+2] CDJXAEDCBYDKBW-UHFFFAOYSA-M 0.000 claims 1
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- 238000004519 manufacturing process Methods 0.000 abstract description 4
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- 231100000331 toxic Toxicity 0.000 abstract 1
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- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
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- 239000003643 water by type Substances 0.000 description 1
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Abstract
本发明公开了一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂的制备方法，步骤如下：称取氧化石墨烯加入去离子水中超声处理；分别加入九水合硝酸铝、七水硫酸亚铁至溶液中进一步超声处理；逐滴加入氨水溶液和氢氧化钠溶液，调节溶液pH值至5.5‑6.0，同时不断搅拌至形成沉淀；将获得的沉淀物转移至高压釜中，在180℃下放置10小时；收集高压釜中残留物，去离子水清洗后，在60℃条件下干燥以得到羟基氧化铝氧化铁复合吸附剂。本发明制备的羟基氧化铝氧化铁复合吸附剂用于去除水中有毒砷离子，具有稳定性好、吸附效率高、制造成本低、环保、可回收再利用等优点。
Description
技术领域
本发明属于水中除砷复合吸附剂制备技术领域，具体涉及一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂及其制备方法。
背景技术
砷是一种普遍存在的类金属元素，它可通过自然风化、生物作用、球化学反应等自然活动及人类工农业生产活动进入水流，长期饮用砷含量超标的水会导致高血压、心血管疾病肾癌、肝癌等多种人类健康疾病，砷污染作为全球性的环境问题已日益突出。在自然水域中，无机砷化物主要以+3和+5两种价态形式存在，而在氧化条件和酸性pH值下，砷则以+5价态形式存在。金属氧化物材料对水中重金属砷有较好的吸附效果，但此类材料易团聚，故而限制其投入实际应用，因此对金属氧化物吸附剂进行改性研制新型修复材料成为国内外砷去除领域的研究热点。
中国专利CN108435133A公布了一种可磁性分离的氧化石墨烯负载铁锰复合氧化物除砷材料及其制备方法，上述材料以氧化石墨烯为载体，在三价铁盐和二价铁盐混合体系中，采用原位沉淀法获得还原氧化石墨烯负载四氧化三铁产物，再加入硫酸锰、聚乙二醇400和三阶铁盐，采用共沉淀法制得。
上述专利使用原料种类较多，制备过程较为复杂，且根据相关学术研究表明还原氧化石墨烯负载铁锰复合氧化物吸附剂砷的最大吸附量仅为12mg/g，吸附容量较小。因此，寻求一种即能解决金属氧化物复合吸附剂易团聚问题，同时具有较大砷吸附容量高效复合吸附剂具有重大现实意义。
发明内容
本发明为了克服现有技术中存在的上述不足，提供一种生产陈本低廉、吸附效率高，且可回收再利用的用于水中除砷的羟基氧化铝氧化铁复合吸附剂及其制备方法。
为解决上述技术问题，本发明的技术方案为：一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂的制备方法，其特征是，包括以下步骤：
S1. 称取0.5g氧化石墨烯加入50ml去离子水中超声处理1小时；
S2. 分别将0.25g九水合硝酸铝、0.25g七水硫酸亚铁加入至溶液中进一步超声处理30分钟；
S3. 逐滴加入2mol/L的氨水溶液和2mol/L的氢氧化钠溶液至溶液中，调节溶液pH值至5.5-6.0，同时不断搅拌至形成沉淀；
S4. 将获得的沉淀物转移至高压釜中，在180℃下放置10小时；
S5. 收集高压釜中残留物，去离子水清洗后，在60℃条件下干燥3小时，得到羟基氧化铝氧化铁复合吸附剂。
一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂，由上述制备方法制得。
本发明与现有技术相比，具有以下优点和效果：
1、本发明以氧化石墨烯为载体，制作出了用于水中除砷的高效羟基氧化铝氧化铁复合吸附剂，且吸附剂中羟基氧化铝、羟基氧化铁均匀分布于载体中，有效地解决了金属氧化物复合颗粒在水中的团聚问题；
2、本发明所得高效羟基氧化铝氧化铁复合吸附剂具有丰富的孔径结构，且比表面积可达140m2/g以上，砷（+5价）的吸附容量可达24mg/g以上，吸附能力强；
3、本发明所得高效羟基氧化铝氧化铁复合吸附剂，在酸性pH值下，其所负载羟基氧化铝、羟基氧化铁的表面羟基会发生质子化，该质子化效应会促进吸附剂与水中含砷阴离子的静电吸附作用，从而使本发明所得吸附剂较其它金属氧化物复合吸附剂具有更强的吸附能力；
4、本发明使用材料较少，且采用简单的一步水热法进行制备，过程简单；
5、生产成本低廉，且吸附剂可回收再利用。
具体实施方式
一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂的制备方法，其特征是，包括以下步骤：
S1. 称取0.5g氧化石墨烯加入50ml去离子水中超声处理1小时；
S2. 分别将0.25g九水合硝酸铝、0.25g七水硫酸亚铁加入至溶液中进一步超声处理30分钟；
S3. 逐滴加入2mol/L的氨水溶液和2mol/L的氢氧化钠溶液至溶液中，调节溶液pH值至5.5-6.0，同时不断搅拌至形成沉淀；
S4. 将获得的沉淀物转移至高压釜中，在180℃下放置10小时；
S5. 收集高压釜中残留物，去离子水清洗后，在60℃条件下干燥3小时，得到羟基氧化铝氧化铁复合吸附剂。
所制得的石墨烯铜铁氧化物复合吸附剂的吸附效果如下：
实验例1：以浓度为0.1mg/L的砷（+5价）溶液为例进行效果说明。
用电子天平称取10mg所制备的羟基氧化铝氧化铁复合吸附剂于100ml锥形瓶中，加入50ml浓度为0.1mg/L的砷（+5价）溶液，在转速180rpm、温度25℃的条件下，将水样置于恒温水浴振荡器中振荡24小时后，用注射器取样，并立即用0.45μm的微孔滤膜过滤，采用原子荧光分光光度计进行测测定滤液中砷（+5价）的浓度，经测定、计算得出每克吸附剂砷（+5价）的吸附容量为24.5mg。
实验例2：以浓度为0.1mg/L的砷（+3价）溶液为例进行效果说明。
用电子天平称取10mg所制备的羟基氧化铝氧化铁复合吸附剂于100ml锥形瓶中，加入50ml浓度为0.1mg/L的砷（+3价）溶液，在转速180rpm、温度25℃的条件下，将水样置于恒温水浴振荡器中振荡24小时后，用注射器取样，并立即用0.45μm的微孔滤膜过滤，采用原子荧光分光光度计进行测测定滤液中砷（+3价）的浓度，经计算得出每克吸附剂砷（+3价）的吸附容量为31.6mg。
本发明以氧化石墨烯为载体，制作出了用于水中除砷的高效羟基氧化铝氧化铁复合吸附剂，且吸附剂中羟基氧化铝、羟基氧化铁均匀分布于载体中，有效地解决了金属氧化物复合颗粒在水中的团聚问题；高效羟基氧化铝氧化铁复合吸附剂具有丰富的孔径结构，且比表面积可达140m2/g以上，砷（+5价）的吸附容量可达24mg/g以上，吸附能力强；在酸性pH值下，其所负载羟基氧化铝、羟基氧化铁的表面羟基会发生质子化，该质子化效应会促进吸附剂与水中含砷阴离子的静电吸附作用，从而使本发明所得吸附剂较其它金属氧化物复合吸附剂具有更强的吸附能力；本发明使用材料较少，且采用简单的一步水热法进行制备，过程简单；生产成本低廉，且吸附剂可回收再利用。
本发明制备的石墨烯铜铁氧化物复合吸附剂可以重复回收再利用，具体操作方法如下：利用抽滤装置将吸附砷后吸附剂进行分离、洗涂、收集，并在烘干后将其浸泡于0.1mol/L的氢氧化钠与0.1mol/L次氯酸钠混合溶液中，解吸24小时后，抽滤、用去离子水洗至中性，放入干燥箱内烘干即可。
本说明书中未作详细描述的内容均属于本领域专业技术人员公知的现有技术。
Claims (2)
1.一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂的制备方法，其特征是，包括以下步骤：
S1. 称取0.5g氧化石墨烯加入50ml去离子水中超声处理1小时；
S2. 分别将0.25g九水合硝酸铝、0.25g七水硫酸亚铁加入至溶液中进一步超声处理30分钟；
S3. 逐滴加入2mol/L的氨水溶液和2mol/L的氢氧化钠溶液至溶液中，调节溶液pH值至5.5-6.0，同时不断搅拌至形成沉淀；
S4. 将获得的沉淀物转移至高压釜中，在180℃下放置10小时；
S5. 收集高压釜中残留物，去离子水清洗后，在60℃条件下干燥3小时，得到高效铝基和铁基复合吸附剂。
2.一种用于水中除砷的羟基氧化铝氧化铁复合吸附剂，其特征是，由权利要求1所述制备方法制得。
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