CN112007619B - 一种用于吸附的壳聚糖碳酸钙复合吸附剂及其制备方法 - Google Patents
一种用于吸附的壳聚糖碳酸钙复合吸附剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于吸附的壳聚糖碳酸钙复合吸附剂及其制备方法,属于有机材料改性领域。其壳聚糖碳酸钙复合吸附剂含有壳聚糖和纳米碳酸钙。其制备方法步骤包括:将壳聚糖溶解在乙酸溶液中;加入纳米碳酸钙;加入氯化钙;取一容器,在容器的内壁中涂上壳聚糖;将前述混合物转移到容器中;加入含有OH‑和CO3 ‑的溶液;密封静置,沉淀物清洗干燥、研磨,得到成品。本发明实验条件温和,操作简单,反应后处理简便,无任何副产物生成;本发明制成的成品,能够快速、针对性的吸收废水中Cu2+离子进行吸附,特异性好,吸附效率高。
Description
技术领域
本发明涉及有机材料改性技术领域,具体涉及一种用于吸附的壳聚糖碳酸钙复合吸附剂及其制备方法。
背景技术
壳聚糖,化学名为β-(1-4)-2-氨基-2-脱氧-D-葡萄糖;是一种直链天然高分子化合物,不溶于水,易于生物降解,可溶于盐酸和部分弱酸性水溶液,分子中存在大量的功能性基团,氨基和羟基等,具有孤对电子的基团可通过配位作用与重金属离子形成配合物而去将其去除,从而能很好地吸附废水中的重金属离子。但是壳聚糖存在分子量小、架桥能力和溶解性能差、对碱金属和碱土金属离子的吸附效果欠佳等不足,使其应用在废水处理方面的应用受到限制。
纳米碳酸钙是一种粒径处于纳米水平的粉体材料,因而结构发生了改变,呈现出其他普通碳酸钙所不具有的效应,由于尺寸小,使其有效面积增加,表面能升高,吸附性比块体的碳酸钙增强。但是由于纳米碳酸钙存在“亲水性及易团聚”两个缺陷使得纳米碳酸钙的应用受到制约。
因此,对具有吸附性能的壳聚糖和纳米碳酸钙进行复合改性以改善其吸附性能,以期待复合改性得到吸附性能稳定的壳聚糖/纳米碳酸钙复合材料,能够快速有效的吸附水中的铜离子。
发明内容
本发明针对上述现有技术存在的问题,提供一种用于吸附的壳聚糖碳酸钙复合吸附剂及其制备方法,能够有针对水中的Cu2+进行吸附。
为实现本发明的目的,通过以下技术方案予以实现:
一种用于吸附的壳聚糖碳酸钙复合吸附剂,包括壳聚糖和纳米碳酸钙;壳聚糖和纳米碳酸钙的质量比为1-10:1-2;
所述纳米碳酸钙的粒径≤70nm。
优选地,包括壳聚糖和纳米碳酸钙;壳聚糖和纳米碳酸钙的质量比为2:1。
一种用于吸附的壳聚糖碳酸钙复合吸附剂的制备方法,包括以下步骤:
(1)将壳聚糖溶解在乙酸溶液中;
(2)将纳米碳酸钙加入至步骤(1)的体系中;
(3)在步骤(2)的体系中加入氯化钙;
(4)取一容器,在容器的内壁中涂上壳聚糖;
(5)将步骤(3)的体系转移到步骤(4)的容器中;
(6)在步骤(5)的体系中,依次加入含有OH-的溶液和含有CO3-的溶液;
(7)将步骤(6)的体系密封静置,取沉淀物清洗至中性后干燥;然后研磨成粉末,得到成品。
优选地,所述步骤(1)和步骤(2)中,壳聚糖和纳米碳酸钙的质量比为1-10:1-2。
优选地,所述步骤(3)中,所述氯化钙的加入量与步骤(2)中纳米碳酸钙的加入量相同。
优选地,所述步骤(6)中,含有OH-的溶液和含有CO3-的溶液的质质量分数比为1:2。
优选地,所述步骤(7)中,所述干燥的条件为温度≥60℃,时间≥2h;所述研磨成粉末的粉末直径≤200目。
优选地,所述步骤(7)中,所述静置时间≥48h。
本发明选择用壳聚糖与纳米碳酸钙作为反应原料,运用凝胶改性的方法,在常温条件下经过复合,制备快速吸附水中Cu2+离子的壳聚糖/纳米碳酸钙复合吸附剂。本发明实验条件温和,操作简单,反应后处理简便,无任何副产物生成;本发明制成的成品,能够快速、针对性的吸收废水中Cu2+离子进行吸附,特异性好,吸附效率高。
附图说明
图1为本发明吸附材料的XRD图;
图2为本发明吸附材料的红外光谱图;
图3为本发明壳聚糖与纳米碳酸钙不同比例吸附材料与吸附时间关系图;
图4为本发明不同吸附材料与pH值关系图;
图5为本发明不同吸附与Cu2+离子初始浓度关系图;
图6为壳聚糖的结构式。
图1、2、4、5中的a是指纯纳米碳酸钙,b是指纯壳聚糖,c是指壳聚糖与纳米碳酸钙质量比为2:1的复合吸附剂。
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楚、完整地描述。其中,附图仅用于示例性说明,表示的仅是示意图,而非实物图,不能理解为对本专利的限制。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本发明的保护范围。
本发明中,如无特别指明,溶液中的百分比均指质量百分比;HAc是指醋酸;Qe是指平衡吸附量。
实施例一
所述复合吸附剂制备方法包括如下步骤:
步骤1:将2mL的HAc溶于98mL的蒸馏水中形成质量分数为2%的HAc溶液;将1.0000g的壳聚糖溶解于19mL2%的HAc溶液中;
步骤2:向步骤1体系中壳聚糖与纳米碳酸钙按质量比2:1的比例,加入0.5000g粒径为70nm的纳米碳酸钙;
步骤3:向步骤2体系中加入0.5000g的CaCl2;CaCl2是作为本絮凝剂使用,当体系中不加入絮凝剂则体系会变成乳浊液而非需要的凝胶状;当氯化钙换成溴化钙、碘化钙或者其他的金属卤化物均不能达到需要的效果。
步骤4:称取0.5000g的壳聚糖加蒸馏水润湿成糊状,均匀涂抹在烧杯内壁;此步骤的壳聚糖仅起模具作用,并不计入壳聚糖和纳米碳酸钙的质量比中。
步骤5:将步骤3中的壳聚糖/Ca2+粘稠物转移至步骤4的烧杯中;
步骤6:取5.0000g的NaOH和10.0000g的NaCO3分别配制成质量分数为5%的NaOH溶液和质量分数为10%的NaCO3溶液;NaOH溶液和NaCO3溶液作为胶凝剂使用。
步骤7:将步骤6中5%的NaOH溶液和10%的NaCO3溶液依次滴加到步骤5体系中;
步骤8:步骤7反应体系密封静置48h,将静置沉淀后得到的白色固体过滤,并用蒸馏水清洗至中性;
步骤9:步骤8中过滤得到的白色固体,置于烘箱中60℃干燥2h,得到干燥后的白色固体,常温常压下,用搪瓷研钵手动研磨成约200目的粉末,得到复合吸附剂。
实施例二至实施例七
与实施例一的区别在于,步骤1和步骤2中的壳聚糖与纳米碳酸钙加入的量不同,如下表所示,其余步骤均相同。
序号 | 壳聚糖加入量 | 纳米碳酸钙加入量 | 比例 |
实施例二 | 10.0000g | 1.0000g | 10:1 |
实施例三 | 5.0000g | 1.0000g | 5:1 |
实施例四 | 1.0000g | 1.0000g | 1:1 |
实施例五 | 1.0000g | 2.0000g | 1:2 |
实施例六 | 1.0000g | 不添加 | 1:0 |
实施例七 | 不添加 | 1.0000g | 0:1 |
对实施例一至七制成的复合吸附剂进行吸附能力的测试,具体步骤为:
步骤1:以微量NaNO3为模拟水中Cu2+离子的稳定剂,配制成质量浓度为100mg/L的Cu2+溶液,其中含有0.08mmol/L的NaNO3。
步骤2:将实施例制成的复合吸附剂取0.0200g,投入到150ml的Cu2+离子溶液中,搅拌4h后,过滤,得到澄清溶液。
步骤3:运用原子吸收分光光度技术,观测步骤2中澄清溶液中Cu2+离子的变化。
反应结果如图3所示,实验后发现,壳聚糖与纳米碳酸钙的质量比2:1时,并在吸附4h时,其Qe最高。
确定壳聚糖与纳米碳酸钙的最佳效果比例后,测试其Qe与pH值、Cu2+离子初始浓度的关系,结果如图4、图5所示。按照上述方法,复合吸附剂吸附水溶液中的Cu2+离子后,过滤得到Cu2+离子澄清溶液中,其原子吸收数据变化明显,随着复合吸附剂吸附时间的增加,溶液中剩余Cu2+离子浓度显著下降,对应的吸附容量升高。同时,模拟废水的pH值以及Cu2+离子的初始浓度都有一个最佳值。
验证例
按照实施例中的制备方法方法,制备的复合吸附剂典型产物如下:
(1)实施例一合成的复合吸附剂其XRD检测结果如图1所示,其衍射峰与纳米碳酸钙以及标准卡为PDF#05-0586的六方晶系的碳酸钙衍射峰基本吻合,并且在2Theta(°)=20.30°可以看到壳聚糖的非定形物相衍射峰,说明纳米碳酸钙与壳聚糖的晶型结构没有发生太大变化,两种材料的很好地复合在一起。但复合后的材料衍射峰没有纳米碳酸钙的衍射峰尖锐,说明两种材料之间发生了相互作用,结晶度降低,吸附活性升高。
(2)实施例一合成的复合吸附剂其FT-IR测试结果如图2所示,-OH振动:3600cm-1;-NH2振动:3400cm-1;-CH3、-CH2-的碳氢伸缩振动:2877.38cm-1;C-N伸缩振动:1448.16cm-1;N-H的弯曲振动:1662.55cm-1;ν(C-O):1153.97-1079.04cm-1;纳米碳酸钙:-OH振动:3600cm-1;CO3 2-上的C=O伸缩振动:1797.76cm-1处有吸收。复合材料:-OH和-NH2的振动:3364.75cm-1;曲线c中,875.35cm-1,712.99cm-1的尖峰为纳米碳酸钙的特征吸收峰。
Claims (6)
1.一种用于吸附的壳聚糖碳酸钙复合吸附剂,其特征在于,包括壳聚糖和纳米碳酸钙;壳聚糖和纳米碳酸钙的质量比为2:1;所述纳米碳酸钙的粒径≤70nm;
其由以下制备方法制备而成:
(1)将壳聚糖溶解在乙酸溶液中;
(2)将纳米碳酸钙加入至所述步骤(1)的体系中;
(3)在所述步骤(2)的体系中加入氯化钙;
(4)取一容器,在容器的内壁中涂上壳聚糖;
(5)将所述步骤(3)的体系转移到步骤(4)的容器中;
(6)在所述步骤(5)的体系中,依次加入含有OH-的溶液和含有CO3 -的溶液;
(7)将所述步骤(6)的体系密封静置,取沉淀物清洗至中性后干燥;然后研磨成粉末,得到成品。
2.一种根据权利要求1所述用于吸附的壳聚糖碳酸钙复合吸附剂的制备方法,其特征在于,包括以下步骤:
(1)将壳聚糖溶解在乙酸溶液中;
(2)将纳米碳酸钙加入至所述步骤(1)的体系中;
(3)在所述步骤(2)的体系中加入氯化钙;
(4)取一容器,在容器的内壁中涂上壳聚糖;
(5)将所述步骤(3)的体系转移到步骤(4)的容器中;
(6)在所述步骤(5)的体系中,依次加入含有OH-的溶液和含有CO3 -的溶液;
(7)将所述步骤(6)的体系密封静置,取沉淀物清洗至中性后干燥;然后研磨成粉末,得到成品。
3.根据权利要求2所述的用于吸附的壳聚糖碳酸钙复合吸附剂的制备方法,其特征在于:所述步骤(3)中,所述氯化钙的加入量与步骤(2)中纳米碳酸钙的加入量相同。
4.根据权利要求2所述的用于吸附的壳聚糖碳酸钙复合吸附剂的制备方法,其特征在于:所述步骤(6)中,含有OH-的溶液和含有CO3 -的溶液的质量分数比为1:2。
5.根据权利要求2所述的用于吸附的壳聚糖碳酸钙复合吸附剂的制备方法,其特征在于:所述步骤(7)中,所述干燥的条件为温度≥60℃,时间≥2h;所述研磨成粉末的粉末直径≤200目。
6.根据权利要求2所述的用于吸附的壳聚糖碳酸钙复合吸附剂的制备方法,其特征在于:所述步骤(7)中,所述静置时间≥48h。
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