CN107141495A - 一种交联羧甲基壳聚糖‑有机蒙脱土高效重金属吸附剂的制备方法 - Google Patents

一种交联羧甲基壳聚糖‑有机蒙脱土高效重金属吸附剂的制备方法 Download PDF

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CN107141495A
CN107141495A CN201710297913.8A CN201710297913A CN107141495A CN 107141495 A CN107141495 A CN 107141495A CN 201710297913 A CN201710297913 A CN 201710297913A CN 107141495 A CN107141495 A CN 107141495A
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organo montmorillonite
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邱鸿浩
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Chengdu Bomei Real Run Technology Co
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Abstract

本发明公开了一种交联羧甲基壳聚糖‑有机蒙脱土重金属吸附剂的制备方法，步骤包括：将有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时得A；羧甲基壳聚糖溶解于水中，溶解完全后在搅拌条件下滴加三聚磷酸钠得B；将A和B混合，70～80℃下充分搅拌2～3小时后进行湿热处理。本发明制得的重金属吸附剂具有pH适用范围宽、热稳定性好的特点，相比壳聚糖‑有机蒙脱土重金属吸附剂有更好的吸附性能。

Description

一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制 备方法
技术领域
本发明属于功能材料技术领域，具体地说，是一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法。
背景技术
空气、土壤、水中的有毒重金属的威胁正逐渐成为全球性问题，因此有效地除去有毒重金属技术成为一项富有挑战性的工作。高分子重金属离子吸附剂已经成为一种比较常用的重金属废水处理药剂，常温下在较宽的pH范围内能与废水中Hg、Cd 、Cu 、Pb 、Mn 、Ni、Zn 、Cr等多种重金属离子迅速反应，生成不溶于水的絮状沉淀物，沉淀快、易过滤，稳定性高，灵敏性高，从而达到吸附去除重金属离子的目，在电镀、电子、线路板等行业得到了广泛的应用。与此同时，有机吸附剂存在效率和热稳定性较差、抗污染能力低、使用寿命不长的问题，而且通常需要与其它方法配合使用才能达到最佳的分离效果。与有机吸附剂相比，无机吸附剂具有吸附效率高、化学稳定性好、耐酸碱和有机溶剂、使用寿命长等优点。因此将有机与无机吸附剂结合形成的复合材料是是重金属吸附领域的一个研究热点。
羧甲基壳聚糖是壳聚糖在碱性条件下与氯乙酸反应制得的一种水溶性壳聚糖衍生物，由于羧甲基的引入破换了其晶体的规整性，使得结晶度大大降低，加上亲水基团的引入，水溶性较壳聚糖明显提高，可在较宽pH范围内溶解，应用范围因此扩大。羧甲基壳聚糖分子中含有-OH，-NH2，-COOH等集团，与壳聚糖相比，能更有效地络合金属离子。
中国专利CN101524635B公开了一种壳聚糖-有机蒙脱土纳米复合材料的制备方法，它通过插层的方法将壳聚糖负载在具有层状结构的有机蒙脱土片层间，所制得的纳米复合材料结合了有机和无机吸附剂各自的优势。然而，壳聚糖不能直接溶于水溶液中，只能溶于酸性溶液中，而且在酸性溶液下，壳聚糖容易降解且其表面上的氨基主要以-NH3 +形式存在，不易于金属离子络合，很大程度上限制了其在废水处理净化领域中的应用，并且复合材料的吸附性能还有待进一步提高。
发明内容
本发明的目的在于提供一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，通过该方法制得的吸附剂不仅结合了有机和无机吸附剂各自的特点，而且进一步提高了吸附剂的吸附能力。
本发明通过下述技术方案实现：
一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，包括以下步骤：
（1）将有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
（2）将羧甲基壳聚糖溶解于水中，溶解完全后在搅拌条件下滴加三聚磷酸钠，羧甲基壳聚糖与三聚磷酸钠的质量比为1:1～1:10；
（3）将步骤（1）和步骤（2）的产物混合，70～80℃下充分搅拌2～3小时；
（4）将步骤（3）所得产物进行湿热处理；
其中羧甲基壳聚糖与有机蒙脱土的质量比为1:1～1:5。
优选的，步骤（1）有机蒙脱土是经过十六烷基三甲基溴化铵、十八烷基三甲基氯化铵或双十烷基二甲基氯化铵改性所得的有机化蒙脱土。
优选的，步骤（2）羧甲基壳聚糖为粘度范围在170～250mpa﹒s的水溶性羧甲基壳聚糖。
优选的，步骤（2）搅拌条件是150r/min，30min。
优选的，步骤（4）湿热处理的条件是121℃，20min。
优选的，羧甲基壳聚糖与三聚磷酸钠的质量比为1:5，羧甲基壳聚糖与有机蒙脱土的质量比1:3。
与现有技术相比，本发明的有益效果是：
（1）羧甲基壳聚糖是两性聚电解质，因为羧基的引入，改善了其在水中的溶解性，扩大了材料使用的pH范围。
（2）因为羧基可以与溶液中的金属离子配位，所以羧基的引入增加了材料的吸附位点密度，提高了吸附能力。
（3）表面活性剂三聚磷酸钠充当交联剂，在湿热条件下与羧甲基壳聚糖反应形成交联壳聚糖，所得产物具有良好的热稳定性，在酸性介质中不溶解，扩大了吸附剂的使用范围。
具体实施方式
下面通过实施例对本发明作进一步的详细说明。
实施例1：
本实施例提供一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，包括以下步骤：
（1）将3.6g经十六烷基三甲基溴化铵改性所得有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
（2）将1.2g羧甲基壳聚糖溶解于水中，溶解完全后在150r/min搅拌条件下滴加6g三聚磷酸钠，搅拌30min。
（3）将步骤（1）和步骤（2）的产物混合，70～80℃下充分搅拌2～3小时；
（4）将步骤（3）所得产物121℃，20min下进行湿热处理；
实施例2：
本实施例提供一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，包括以下步骤：
（1）将3.6g经十八烷基三甲基氯化铵改性所得有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
（2）将3.6g羧甲基壳聚糖溶解于水中，溶解完全后在150r/min搅拌条件下滴加3.6g三聚磷酸钠，搅拌30min。
（3）将步骤（1）和步骤（2）的产物混合，70～80℃下充分搅拌2～3小时；
（4）将步骤（3）所得产物121℃，20min下进行湿热处理；
实施例3：
本实施例提供一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，包括以下步骤：
（1）将4.5g经双十烷基二甲基氯化铵改性所得有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
（2）将0.9g羧甲基壳聚糖溶解于水中，溶解完全后在150r/min搅拌条件下滴加9g三聚磷酸钠，搅拌30min。
（3）将步骤（1）和步骤（2）的产物混合，70～80℃下充分搅拌2～3小时；
（4）将步骤（3）所得产物121℃，20min下进行湿热处理；
对比例1：
本实施例提供一种壳聚糖-有机蒙脱土重金属吸附剂的制备方法，包括以下步骤：
（1）将3.6g经十六烷基三甲基溴化铵改性所得有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
（2）将1.2g壳聚糖溶解于水中，在150r/min搅拌条件下搅拌30min。
（3）将步骤（1）和步骤（2）的产物混合，70～80℃下充分搅拌2～3小时；
（4）将步骤（3）所得产物121℃，20min下进行湿热处理；
对比例2：
本实施例提供一种壳聚糖-有机蒙脱土重金属吸附剂的制备方法，包括以下步骤：
（1）将3.6g经双十烷基二甲基氯化铵改性所得有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
（2）将1.2g壳聚糖溶解于水中，在150r/min搅拌条件下搅拌30min。
（3）将步骤（1）和步骤（2）的产物混合，70～80℃下充分搅拌2～3小时；
（4）将步骤（3）所得产物121℃，20min下进行湿热处理；
应用测试：
分别对实施例1～3制备的交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂和对比例1～2的壳聚糖-有机蒙脱土重金属吸附剂处理电镀工业废水的性能进行检测，具体测试步骤如下：
分别取上述制备好的重金属吸附剂1.0g，加入到100ml含有重金属离子的电镀工业废水，调节溶液的pH=5.7，室温下振荡处理8小时。处理完后，将吸附剂过滤出，借助原子放射光谱法测定吸附前后电镀工业废水中重金属离子（Pb2+、Ni2+、Cd2+）浓度的变化。测试结果如表1所示。
表1
从表1的实验结果可以看出，本发明制备的交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂吸附重金属离子的效果比壳聚糖-有机蒙脱土重金属吸附剂好的多。
以上所述，仅是本发明的较佳实施例，并非对本发明做任何形式上的限制，凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化，均落入本发明的保护范围之内。

Claims (6)

1.一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，其特征在于，包括以下步骤：
(1)将有机蒙脱土配置成悬浮液，70～80℃下加热搅拌，保温0.5～1小时；
(2)将羧甲基壳聚糖溶解于水中，溶解完全后在搅拌条件下滴加三聚磷酸钠，羧甲基壳聚糖与三聚磷酸钠的质量比为1:1～1:10；
(3)将步骤(1)和步骤(2)的产物混合，70～80℃下充分搅拌2～3小时；
(4)将步骤(3)所得产物进行湿热处理；
其中羧甲基壳聚糖与有机蒙脱土的质量比1:1～1:5。
2.根据权利要求1所述的一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，其特征在于：所述步骤(1)有机蒙脱土是经过十六烷基三甲基溴化铵、十八烷基三甲基氯化铵或双十烷基二甲基氯化铵改性所得的有机化蒙脱土。
3.根据权利要求1或2所述的一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，其特征在于：所述步骤(2)羧甲基壳聚糖为粘度范围在170～250mpa﹒s的水溶性羧甲基壳聚糖。
4.根据权利要求3所述的一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，其特征在于：所述步骤(2)搅拌条件是150r/min，30min。
5.根据权利要求4所述的一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，其特征在于：所述步骤(4)湿热处理的条件是121℃，20min。
6.根据权利要求5所述的一种交联羧甲基壳聚糖-有机蒙脱土高效重金属吸附剂的制备方法，其特征在于：所述羧甲基壳聚糖与三聚磷酸钠的质量比为1:5，羧甲基壳聚糖与有机蒙脱土的质量比1:3。
CN201710297913.8A 2017-04-29 2017-04-29 一种交联羧甲基壳聚糖‑有机蒙脱土高效重金属吸附剂的制备方法 Withdrawn CN107141495A (zh)

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CN108328746A (zh) * 2018-01-29 2018-07-27 华中科技大学 一种羧甲基改性的壳聚糖/酵母吸附剂、其制备和应用
CN108579693A (zh) * 2018-05-23 2018-09-28 东华理工大学 一种三聚磷酸钠交联壳聚糖/钠基膨润土气凝胶的制备方法
CN108579693B (zh) * 2018-05-23 2021-01-05 东华理工大学 一种三聚磷酸钠交联壳聚糖/钠基膨润土气凝胶的制备方法
CN110527143A (zh) * 2019-09-12 2019-12-03 四川轻化工大学 一种硫酸钙晶须的改性方法及其在水性聚氨酯涂料中的应用
CN110527142A (zh) * 2019-09-12 2019-12-03 四川轻化工大学 一种硫酸钙晶须的改性方法及其在水性丙烯酸涂料中的应用
CN110527142B (zh) * 2019-09-12 2021-09-03 四川轻化工大学 一种硫酸钙晶须的改性方法及其在水性丙烯酸涂料中的应用
CN111533286A (zh) * 2020-05-19 2020-08-14 胡锦香 一种复合缓释环保型阻垢剂及其制备方法
CN112779019A (zh) * 2021-01-07 2021-05-11 何雨昕 一种增强作物抗逆性的土壤调理剂及其制备方法
CN114890601A (zh) * 2022-05-19 2022-08-12 杭州特种纸业有限公司 一种钢纸生产用水的平衡利用方法

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