摘要
有害重金属是比较常见的污染物，对人体有强烈的致癌、致畸和致突变等毒害作用。随着工业化进程的加快，环境中的有害重金属含量日益增加，严重威胁人类的健康。因此，寻找一种能有效地吸附水体和液态食品中有害重金属的材料就成为亟待解决的问题。
壳聚糖是自然界存在的唯一碱性多糖，是地球上第二大可再生资源。壳聚糖在废水处理、食品医药、造纸、纺织和水净化等方面具有广泛的应用。壳聚糖分子中含有大量的氨基和羟基，利于对其进行改性，以增强壳聚糖的吸附能力、吸附选择性及对环境的适应能力。
本文以壳聚糖为功能单体，考察了无机材料、氨基化和硫代羰基化等改性壳聚糖树脂对有害重金属离子的吸附特性，对其结构作了初步表征，并从饱和吸附量、吸附选择性和在低pH下的吸附方面做了深入的研究，为壳聚糖树脂在重金属吸附领域的研究和应用提供有力的科学支持和理论依据。
1）首次建立了利用氢化物发生器-原子吸收分光光度计测定海带汁中总砷的方法。通过考察了消解温度，预还原剂的种类和浓度以及还原剂NaBH4浓度等条件的影响，最终确定消解温度为180℃，酸性介质为浓硝酸，预还原剂Vc的浓度为1%，还原剂NaBH4的浓度为1.8%，总砷检出量稳定。
2）制备了壳聚糖As(III)印迹树脂As-ICR，研究其对As(III)的吸附特性。通过利用分子印迹技术，以As(III)为印迹分子，制备As-ICR用于吸附水溶液和海带汁中的As(III)，考察不同pH、温度条件下As-ICR对As(III)的吸附。吸附反应主要是As-ICR上的氨基吸附As(III)，壳聚糖形成树脂后热稳定性和结晶性均有所下降。As-ICR对水溶液中的As(III)表现出选择性吸附。As-ICR对海带汁中的As(III)有选择性吸附。
3）对As-ICR进行改性，提高其对As(III)的吸附量。利用α-Fe2O3对壳聚糖进行改性制备α-Fe2O3改性壳聚糖As(III)印迹树脂As-IFICR用于提高对As(III)的吸附量。As-IFICR在pH5，30℃，As(III)浓度50mg/L下对As(III)的饱和吸附量为6.20mg/g，吸附过程符合Langmuir等温吸附模型和拟二级动力学方程。As-IFICR对As(III)的吸附量显著提高。As-IFICR对海带汁中As(III)的吸附能力显著高于As-ICR，且对有益金属元素的吸附量较小。
4）制备壳聚糖Pb2+印迹树脂Pb-ICR，研究其对Pb2+的吸附特性。Pb-ICR的氨基和羟基是吸附Pb2+的主要功能基团。Pb-ICR在40℃，pH6.0，吸附时间4h下对Pb2+的吸附量最大，且对Pb2+表现出选择性吸附。
5）对Pb-ICR进行改性，提高其对Pb2+的吸附选择性。利用四乙烯五胺对壳聚糖树脂进行改性制备四乙烯五胺改性壳聚糖Pb2+印迹树脂Pb-ITMCR用于提高壳聚糖树脂对金属离子的吸附选择性。Pb-ITMCR上的氨基参与吸附反应。Pb-ITMCR在pH6.0，40℃，8h下对Pb2+的吸附达到饱和状态，且Pb-ITMCR对Pb2+的吸附选择性较Pb-ICR有明显提高。
6）对Pb-ICR进行改性，提高其对pH的适应能力。利用二硫代氨基甲酸钠对壳聚糖树脂进行改性制备二硫代氨基甲酸钠改性壳聚糖Pb2+印迹树脂Pb-IDMCR用于拓宽壳聚糖树脂对pH的适用范围。Pb-IDMCR上的氨基、巯基和硫代羰基参与吸附过程，且壳聚糖的热稳定性降低。Pb-IDMCR在较低pH (pH1.0)下对Pb2+有较高的吸附量，拓宽了壳聚糖树脂对pH的适用范围。
我国是重金属污染较严重的国家之一，目前还没有很成熟的方法用于解决液态食品中重金属超标问题。本文以壳聚糖为功能单体，以戊二醛交联成壳聚糖树脂，根据不同的目的对壳聚糖树脂进行改性，用于液态食品和水体中有害重金属离子的选择性吸附，为改性壳聚糖树脂应用于有害重金属的脱除提供理论支持。
Harmful heavy metals are more common pollutants, causing cancer, teratogenicand mutation of adverse effects to the human body. With the development ofindustrialization, the harmful heavy metals content in the enviroment is increasing,which influencing the human being seriously. Therefore, seeking a kind of materialsfor adsorbing heavy metals from aqueous solution becomes a urgently problem to besolved.
Chitosan is the only alkaline polysaccharide in nature, which is the secondlargest renewable resources. Chitosan has been widely applied in waste watertreatment, food and medicine, paper and textile, water purification. Chitosan has a lotof free amino and hydroxyl groups, it is easily to be modified to enhance theadsorption properties, adsorption selectivity and adapting ability to the environment.
In this topic, chitosan was used as functional monomer, inorganic material,amination and sulfur based modification were investigated to the adsorptionproperties for harmful heavy metals, their structures were preliminary characterized,the adsorption properties of modified chitosan resin for heavy metals was discussedfrom aspects of adsorption capacity, adsorption selectivity and adsorption at low pH,which provide powerful scientific support and theoretical basis for researching andapplying of chitosan resin in the heavy metals adsorption areas.
1) The detection methods of total arsenic was established with HVG-FAAS forthe first time. Digestion temperature, the selection of pre-reduction agents andreduction agents NaBH4concentration were investigated to determine the the optimalconditions: digestion temperature was180℃, acid medium was nitric acid, the pre-reduction agent Vc concentration was1%, reduction agent NaBH4concentrationwas1.8%, detection limit was0.95μg/L, RSD was1.3%～7.6%, recovery rate was83.1%～105.3%, total arsenic detection was stable.
2) Chitosan resin was prepared with As(III) as imprinted ion As-ICR wasprepared to investgated the adsorption property. As-ICR was prepared throughmolecular imprinted technology with As(III) as imprinted ion to adsorb As(III) fromaqueous solution and Laminaria japonica juice. The adsorption of As-ICR for As(III)was investagted at different pH and temperature. The adsorption process was that theamino groups of As-ICR adsorb As(III), and the thermal stability and crystalline bothreduce after formed into chitosan resin. As-ICR selectively adsorbed As(III) fromaqueous solution. It also could adsorbed As(III) from Laminaria japonica juice.
3) As-ICR was modified to enhance the adsorption capacity. α-Fe2O3modifiedchitosan resin with As(III) as imprinted ions As-IFICR was prepared to improve theadsorption capacity of chitosan resin for As(III). The adsorption capacity of As-IFICRfor As(III) was6.20mg/g at pH5,30℃, As(III) concentration50mg/L, theadsorption process fit Langmuir isothermal adsorption model and pseudo secondkinetic equation. The adsorption capacity of As-IFICR for As(III) was improvedsignificantly. The adsorption capacity of As-IFICR for As(III) from Laminariajaponica juice was more than that of As-ICR, the adsorption for beneficial metalelements was less.
4) Chitosan resin was prepared with Pb2+as imprinted ion was prepared toinvestgated the adsorption property. Amino and hydroxyl groups were mainlyfunctional groups of Pb-ICR for Pb2+. The adsorption capacity of Pb-ICR for Pb2+wassaturated at40℃, pH6.0, contact time4h, and it could selectively adsorb Pb2+fromaqueous solution.
5) The Pb-ICR was modified to enhance the adsorption selectivity. The tetraethylene pentamine (TEPA) modified chitosan resin with Pb2+as imprinted ionsPb-ITMCR was prepared to enhance the adsorption selectivity of chitosan resin formetal ions. The amino groups of Pb-ITMCR participate in the adsorption. Theadsorption capacity of Pb-ITMCR for Pb2+was saturated at pH6.0,40℃, contacttime8h, the adsorption could fit the pseudo second kinetic equation and Langmuirisothermal adsorption model. The adsorption selectivity of Pb-ITMCR for Pb2+washigher than that of Pb-ICR.
6) The Pb-ICR was modified to enhance the pH adaptability. The sodiumdithiocarbamate modified chitosan resin with Pb2+as imprinted ions Pb-IDMCR wasprepared to widen the application scope of chitosan resin to pH. Amino, sulfydryl andthiocarbonyl groups of Pb-IDMCR involved in the adsorption process, and the thermalstability of chitosan decrease. The adsorption capacity of Pb-IDMCR for Pb2+washigher than that of chitosan resin at low pH (pH1.0), and the adaptability ofPb-IDMCR to pH improved greatly.
Nowdays, our country is one of the serious countries in heavy metal pollution,but no mature methods were applied to solve heavy metal pollution up to now. In thisresearch, chitosan was used as functional monomer to prepare crosslinked chitosanresin, chitosan resin was modified to selectively adsorb heavy metals from liquid foodand aqueous solution, which providing theory support for heavy metals removal.
引文
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