CN111545176A - 一种多孔磁性复合生物吸附剂的制备方法 - Google Patents

一种多孔磁性复合生物吸附剂的制备方法 Download PDF

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CN111545176A
CN111545176A CN202010293457.1A CN202010293457A CN111545176A CN 111545176 A CN111545176 A CN 111545176A CN 202010293457 A CN202010293457 A CN 202010293457A CN 111545176 A CN111545176 A CN 111545176A
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许崇娟
李慧芝
李志英
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University of Jinan
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Abstract

本发明公开了一种多孔磁性复合生物吸附剂的制备方法，其特征在于，（1）采用β‑环糊精与蛋白粉混合物，羧基化三氧化二铁磁性纳米颗粒，γ‑二氧化锰，衣康酸，过硫酸铵，制备得到多孔磁性复合微球；（2）在反应器中，按如下组成质量百分浓度加入，去离子水：84~88%，2，6‑二甲氧基‑β‑环糊精：5~8%，搅拌溶解，多孔磁性复合微球：6~10%，各组分之和为百分之百，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。该吸附剂对多溴联苯醚具有很高的吸附容量，具有专一性和特异，成本低，机械强度高，可反复使用10次以上，吸附剂容易分离。

Description

一种多孔磁性复合生物吸附剂的制备方法
技术领域
本发明涉及一种改性磁性生物吸附剂的制备方法，特别涉及一种多孔磁性复合生物吸附剂的制备方法及对多溴联苯醚吸附分离的应用，属于环保技术领域。
背景技术
多溴联苯醚(PBDEs) 作为一种溴系阻燃剂的一大类阻燃物质，由于其优异的阻燃性能，已经越来越广泛的应用于各种消费产品当中。但是随着在环境样品中不断报道PBDEs的检出，该类化合物所造成的环境问题也越来越受到大家特别是环境科学的关注是一类环境中广泛存在的全球性有机污染物。由于其具有环境持久性，远距离传输，生物可累积性及对生物和人体具有毒害效应等特性，对其环境问题的研究已成为当前环境科学的一大热点。2009年5月，联合国环境规划署正式将四溴联苯醚和五溴联苯醚、六溴联苯醚和七溴联苯醚列入《斯德哥尔摩公约》。已有的研究资料主要集中在PBDEs的环境行为研究方面，而关于这类化合物在淡水生态系统中水生生物体内生物积累的研究资料有限。作为一种潜在的干扰内分泌功能，发育毒性、生殖毒性、致癌，对生态环境和人体健康产生严重的危害。由于PBDEs分布广泛，在环境中含量极低，如何对其进行有效的去除是一项亟待解决的问题。
环糊精是环糊精转葡萄糖基酶作用于淀粉的产物，是由六个以上葡萄糖以α—1,4—糖苷键连结的环状寡聚糖，其中最常见、研究最多的是α-环糊精、β-环糊精、γ-环糊精，分别由六个、七个和八个葡萄糖分子构成，是相对大和相对柔性的分子。环糊精分子成锥柱状或圆锥状花环，有许多可旋转的键和羟基，内有一个空腔，表观外型类似于接导管的橡胶塞。空腔内部排列着配糖氧桥原子，氧原子的非键电子对指向中心，使空腔内部具有很高的电子密度，表现出部分路易斯碱的性质。分子构型为葡萄糖的C-1椅式构型，在它的圆筒内部有-CH-葡萄糖苷结合的O原子，故呈疏水性。葡萄糖的2位和3位的-OH基在圆筒的一端开口处，6位的-OH基在圆筒的另一端开口处，所以圆筒的二端开口处都呈亲水性，这样，环糊精的筒形体的内部上层、中层、下层由不同的基团组成。在强碱性溶液中也可稳定存在，在酸性溶液中则部分水解成葡萄糖和非环麦芽糖。本申请将β-环糊精与蛋白粉混匀溶解于水中后，加入羧基化四氧化三铁纳米颗粒与γ-二氧化锰、衣康酸在过硫酸铵引发聚合反应，制得到多孔磁性复合微球，再采用2，6-二甲氧基-β-环糊精浸泡多孔磁性复合微球，然后对多溴联苯醚进行吸附分离，该吸附剂即具有磁性吸附剂的特性，又具有天然高分子特性，同时还具有对多溴联苯醚具有专一的选择性。
多孔材料是一种由相互贯通或封闭的孔洞构成网络结构的材料，孔洞的边界或表面由支柱或平板构成，多孔材料一般具有相对密度低、比强度高、比表面积大、重量轻、渗透性好等优点，通常比表面积越大、孔隙越多、表面链接官能团的位点越丰富，链接上的活性基团越多，活性基团越多吸附剂的吸附容量就越大，其吸附能力越强。
发明内容
本发明的目的之一是提供一种多孔磁性复合生物吸附剂的制备方法，获取的一种多孔磁性复合生物吸附剂对多溴联苯醚的进行吸附分离。
本发明的目的通过以下技术方案实现。
一种多孔磁性复合生物吸附剂的制备方法，其特征在于，该方法具有以下工艺步骤：
（1） 多孔磁性复合微球的制备：在反应器中，按如下组成质量百分浓度加入，去离子水：62~66%，β-环糊精与蛋白粉混合物：12~16%，微热混匀，加入羧基化三氧化二铁磁性纳米颗粒：3~5%，γ-二氧化锰：6~10%，衣康酸：6~8%，超声波分散20min，再加入过硫酸铵：2~4%，各组分之和为百分之百，温度升至50±2℃恒温，反应5 h将所得粘稠状悬浮液喷撒在质量百分浓度为5%的氯化镁+3%硫酸钠混合溶液中，通过喷头的直径控制复合微球的粒径，清洗，固液分离，冷冻干燥，得到多孔磁性复合微球；
（2）多孔磁性复合生物吸附剂制备：在反应器中，按如下组成质量百分浓度加入，去离子水：84~88%，2，6-二甲氧基-β-环糊精：5~8%，搅拌溶解，多孔磁性复合微球：6~10%，各组分之和为百分之百，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。
在步骤（1）中所述的β-环糊精与蛋白粉的质量比1：6，在玛瑙研钵中研磨为一体。
在步骤（1）中所述的喷头的直径控制在0.6~1.0mm之间。
在步骤（1）中所述的磁性多孔复合微球粒径在0.6~1.0mm之间。
在步骤（1）中所述的羧基化三氧化二铁磁性纳米颗粒与γ-二氧化锰质量比为：1:2。
在步骤（1）中所述的γ-二氧化锰粒径在200~400目之间。
备方法对分离富集，特点为：将制备的一种多孔磁性复合生物吸附剂用去离子水浸泡0.5~1h，按静态法吸附。
将制备的一种多孔磁性复合生物吸附剂用去离子水浸泡0.5~1h，按动态法吸附。
本发明与现有技术比较，具有如下优点及有益效果：
（1）本发明获得的一种多孔磁性复合生物吸附剂具有良好的物理化学稳定性和优异的机械强度，具有大的比表面积，吸附容量大，对多溴联苯醚最大吸附容量达131.21mg/g，耐磨可反复使用次数可达10次以上，吸附的速度快，吸附选择好，解吸性能好，能够在较宽的酸碱范围内使用。
（2）本发明获得的一种多孔磁性复合生物吸附剂的制备方法既具有固相载体材料的优点，也解决了活性基团应用到水环境中的流失问题，吸附剂可通过外加磁场回收，对多溴联苯醚具有具有很强的专一性和特异。
（3）合成的过程要求的条件容易控制，能耗低，操作简单，属于清洁生产工艺，易于工业化生产，是天然绿色产品，可生物降解。
具体实施方式
实施例1
（1） 多孔磁性复合微球的制备：在反应器中，分别加入，去离子水：64mL，β-环糊精与蛋白粉混合物：14g，微热混匀，加入羧基化三氧化二铁磁性纳米颗粒：4g，γ-二氧化锰：8g，衣康酸：7g，超声波分散20min，再加入过硫酸铵：3g，温度升至50±2℃恒温，反应5 h将所得粘稠状悬浮液喷撒在质量百分浓度为5%的氯化镁+3%硫酸钠混合溶液中，通过喷头的直径控制复合微球的粒径，清洗，固液分离，冷冻干燥，得到多孔磁性复合微球；
（2）多孔磁性复合生物吸附剂制备：在反应器中，分别加入，去离子水：86 mL，2，6-二甲氧基-β-环糊精：6g，搅拌溶解，多孔磁性复合微球：8g，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。
实施例2
（1） 多孔磁性复合微球的制备：在反应器中，分别加入，去离子水：630mL，β-环糊精与蛋白粉混合物：160g，微热混匀，加入羧基化三氧化二铁磁性纳米颗粒：30g，γ-二氧化锰：60g，衣康酸：80g，超声波分散20min，再加入过硫酸铵：40g，温度升至50±2℃恒温，反应5 h将所得粘稠状悬浮液喷撒在质量百分浓度为5%的氯化镁+3%硫酸钠混合溶液中，通过喷头的直径控制复合微球的粒径，清洗，固液分离，冷冻干燥，得到多孔磁性复合微球；
（2）多孔磁性复合生物吸附剂制备：在反应器中，分别加入，去离子水：880mL，2，6-二甲氧基-β-环糊精：50g，搅拌溶解，多孔磁性复合微球：70g，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。
实施例3
（1） 多孔磁性复合微球的制备：在反应器中，分别加入，去离子水：650mL，β-环糊精与蛋白粉混合物：120g，微热混匀，加入羧基化三氧化二铁磁性纳米颗粒：50g，γ-二氧化锰：100g，衣康酸：60g，超声波分散20min，再加入过硫酸铵：20g，温度升至50±2℃恒温，反应5h将所得粘稠状悬浮液喷撒在质量百分浓度为5%的氯化镁+3%硫酸钠混合溶液中，通过喷头的直径控制复合微球的粒径，清洗，固液分离，冷冻干燥，得到多孔磁性复合微球；
（2）多孔磁性复合生物吸附剂制备：在反应器中，分别加入，去离子水：840 mL，2，6-二甲氧基-β-环糊精：80g，搅拌溶解，多孔磁性复合微球：80g，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。
实施例4
（1） 多孔磁性复合微球的制备：在反应器中，分别加入，去离子水：660mL，β-环糊精与蛋白粉混合物：130g，微热混匀，加入羧基化三氧化二铁磁性纳米颗粒：40g，γ-二氧化锰：80g，衣康酸：70g，超声波分散20min，再加入过硫酸铵：20g，温度升至50±2℃恒温，反应5 h将所得粘稠状悬浮液喷撒在质量百分浓度为5%的氯化镁+3%硫酸钠混合溶液中，通过喷头的直径控制复合微球的粒径，清洗，固液分离，冷冻干燥，得到多孔磁性复合微球；
（2）多孔磁性复合生物吸附剂制备：在反应器中，分别加入，去离子水：850 mL，2，6-二甲氧基-β-环糊精：50g，搅拌溶解，多孔磁性复合微球：100g，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。
实施例5
称取1.0g 多孔磁性复合生物吸附剂置于250mL具塞锥形瓶中浸泡0.5~1.0h，过滤洗涤后，加入100mL浓度为100mg/L多溴联苯醚标准溶液中，以稀酸或碱调节体系的pH值为6.0~9.0，在室温下震荡吸附30 min，取上清液，用色谱测定多溴联苯醚的浓度，根据吸附前后溶液中多溴联苯醚的浓度差，计算出多孔磁性复合生物吸附剂对多溴联苯醚的去除率，本发明所制得的多孔磁性复合生物吸附剂对多溴联苯醚的去除率都在95.2%以上，最高可达97.6%。按相同步骤将多溴联苯醚标准溶液的浓度增加到500mg/L，吸附剂称取0.1g，测定多孔磁性复合生物吸附剂对多溴联苯醚吸附容量为131.21mg/g。

Claims (6)

1.一种多孔磁性复合生物吸附剂的制备方法，其特征在于，该方法具有以下工艺步骤：
（1） 多孔磁性复合微球的制备：在反应器中，按如下组成质量百分浓度加入，去离子水：62~66%，β-环糊精与蛋白粉混合物：12~16%，微热混匀，加入羧基化三氧化二铁磁性纳米颗粒：3~5%，γ-二氧化锰：6~10%，衣康酸：6~8%，超声波分散20min，再加入过硫酸铵：2~4%，各组分之和为百分之百，温度升至50±2℃恒温，反应5 h将所得粘稠状悬浮液喷撒在质量百分浓度为5%的氯化镁+3%硫酸钠混合溶液中，通过喷头的直径控制复合微球的粒径，清洗，固液分离，冷冻干燥，得到多孔磁性复合微球；
（2）多孔磁性复合生物吸附剂制备：在反应器中，按如下组成质量百分浓度加入，去离子水：84~88%，2，6-二甲氧基-β-环糊精：5~8%，搅拌溶解，多孔磁性复合微球：6~10%，各组分之和为百分之百，室温搅拌反应2h，冷却后，用去离子水洗涤、固液分离，干燥，得到多孔磁性复合生物吸附剂。
2.根据权利要求1中所述的一种多孔磁性复合生物吸附剂的制备方法，其特征在于，步骤（1）中所述的β-环糊精与蛋白粉的质量比1：6，在玛瑙研钵中研磨为一体。
3.根据权利要求1中所述的一种多孔磁性复合生物吸附剂的制备方法，其特征在于，步骤（1）中所述的喷头的直径控制在0.6~1.0mm之间。
4.根据权利要求1中所述的一种多孔磁性复合生物吸附剂的制备方法，其特征在于，步骤（1）中所述的磁性多孔复合微球粒径在0.6~1.0mm之间。
5.根据权利要求1中所述的一种多孔磁性复合生物吸附剂的制备方法，其特征在于，步骤（1）中所述的羧基化三氧化二铁磁性纳米颗粒与γ-二氧化锰质量比为：1:2。
6.根据权利要求1中所述的一种多孔磁性复合生物吸附剂的制备方法，其特征在于，步骤（1）中所述的γ-二氧化锰粒径在200~400目之间。
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