CN114797787A - 载铁椰壳活性炭壳聚糖复合微球的制备及其应用 - Google Patents
载铁椰壳活性炭壳聚糖复合微球的制备及其应用 Download PDFInfo
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Abstract
本发明公布一种载铁椰壳活性炭壳聚糖复合微球的制备方法及其应用。该方法包括以下步骤:将洗净后的颗粒状椰壳活性炭洗净研磨成粉末状,过150目筛。将预处理后的椰壳活性炭粉末和乙酸溶液超声搅拌混合均匀,得到椰壳活性炭悬浮液;加入壳聚糖粉末,超声搅拌至完全溶解,得椰壳活性炭壳聚糖混合液;再加入FeCl3·6H2O混合均匀,将混合液滴入到NaOH溶液中,室温下静置24h,过滤,去离子水洗涤至pH接近中性,加入戊二醛‑甲醇混合液,振荡交联反应,过滤,乙醇溶液洗涤,烘干得载铁椰壳活性炭壳聚糖复合微球。本发明所得载铁椰壳活性炭壳聚糖复合微球制备方法简便、低成本、易得、环保,对水体中不同酸碱度条件下的As(Ⅲ)具有良好的吸附效果。
Description
技术领域
本发明涉及无机材料领域。更具体地说,本发明涉及一种载铁椰壳活性炭壳聚糖复合微球的制备方法及用途。
背景技术
水体中含有超标的重金属对人体会造成伤害。其中,重金属砷(As)因其存在的广泛性、高毒性和致癌性而受到人们关注。世界卫生组织(WHO)和美国环境保护署(USEPA)也将砷(As)定义为一种“已知的人类致癌物”。自然界中,砷的主要形态有无机砷酸盐和亚砷酸盐两种。通常,在氧化性水体中主要以五价砷为主,在还原性水体中主要以三价砷为主。三价砷比五价砷毒性大,约为60倍,且具有水溶性大、不易降解等特性,易于生物体累积。人体长期暴露于砷环境,可引起皮肤癌、肺癌、膀胱癌和肝癌等癌症。长期摄入砷含量超标的饮用水会引起机体慢性中毒,即砷中毒。砷中毒可引起皮肤、周围神经损伤、肝坏死或心血管疾病,严重的可导致皮肤癌和多种内脏癌。因此,去除水体中的砷是非常有必要的,也是水处理领域的必经一步。
当前,水体中应用较为成熟的除砷技术主要有化学沉淀法、吸附法、离子交换法、生物法等。与其他方法相比,吸附法因操作简便、低成本、高效率、环保不易造成二次污染而备受推崇。椰壳活性炭作为吸附法中高效材料之一,因其具有吸附能力强、化学稳定性好、力学强度高,且可方便再生等特点,被广泛研究和使用。但椰壳活性炭多为用高温煅烧制备后再加以改性,操作繁琐且具有一定的危险性,且单独使用椰壳活性炭用于吸附不易回收。壳聚糖本身就是具有大量羟基和高活性氨基的天然可降解高分子材料,能通过螯合反应与重金属离子进行配位,加上其含丰富的羟基、氨基等含氧官能团,是另一种具有吸引力的新型吸附剂。但是壳聚糖自身多为粉末状,不易固液分离,且稳定性不佳,在酸性环境易流失,极大限制壳聚糖的适用范围。
发明内容
针对椰壳活性炭、壳聚糖存在的优缺点,本发明提供一种耐酸性较强且易实现固液分离的载铁椰壳活性炭壳聚糖复合微球复合微球的制备方法。同时提供一种载铁椰壳活性炭壳聚糖复合微球的用途,对水中As(III)的去除具有较好的效果。
为了实现本发明的这些目的和其它优点,提供一种载铁椰壳活性炭壳聚糖复合微球的制备方法,包括以下步骤:
(1)用去离子水将颗粒状椰壳活性炭反复浸泡并冲洗,将洗净的椰壳活性炭置于45℃烘箱中烘干备用;
(2)将干燥后的椰壳活性炭研磨成粉末状,并过150目筛;
(3)配制1.5%的醋酸溶液,加入粉末状椰壳活性炭,超声搅拌使其溶解均匀;
(4)往溶液中加入同质量的壳聚糖粉末,超声搅拌使其混合均匀,得椰壳活性炭壳聚糖混合溶液;
(5)称取0.1M FeCl3·6H2O加入至椰壳活性炭壳聚糖混合溶液中,超声搅拌至FeCl3·6H2O完全溶解,得到含铁椰壳活性炭壳聚糖混合溶液;
(6)将该混合溶液滴加至NaOH溶液中,静置24h。用去离子水将静置后的载铁椰壳活性炭壳聚糖微球洗至pH接近中性,使其成球状,得载铁椰壳活性炭壳聚糖复合微球;
(7)将配制好的5wt%戊二醛-甲醇混合液倒入装有湿性载铁椰壳活性炭壳聚糖微球的烧杯中,匀速振荡3h,使其固结交联。将振荡后的微球过滤,用乙醇溶液洗涤至无醛味,放置烘箱中,45℃烘干,即得载铁椰壳活性炭壳聚糖复合微球。
本发明优选的是,步骤(1)中清洗椰壳活性炭,是去除活性炭表面的杂质及灰分。
本发明优选的是,步骤(3)中称取粉末状椰壳活性炭的质量为5g。
本发明优选的是,步骤(4)中称取壳聚糖的质量为5g,椰壳活性炭同壳聚糖质量比为1:1。
本发明优选的是,步骤(6)中滴加采用内径为1.5mm的滴管进行。
本发明优选的是,步骤(6)中NaOH溶液的体积分数为20%
本发明还提供了一种载铁椰壳活性炭壳聚糖复合微球作为吸附剂的用途。
本发明采用共沉淀法,以椰壳活性炭和壳聚糖为前体物,FeCl3·6H2O为改性剂,戊二醛为交联剂制备了载铁椰壳活性炭壳聚糖复合微球。其中Fe3+湿法改性提高了吸附剂的吸附容量,交联提高了吸附剂的耐酸性及稳定性。利用该方法合成的载铁椰壳活性炭壳聚糖复合微球成本低、操作简单、绿色环保,且对水体中As(Ⅲ)具有良好的去除效果。
本发明的其它优点、目标和特征将部分通过下面的说明体现,部分还将通过对本发明的研究和实践而为本领域的技术人员所理解。
附图说明
图1为颗粒状椰壳活性炭的有关参数;
图2为椰壳活性炭壳聚糖复合微球的SEM图像;
图3为载铁椰壳活性炭壳聚糖复合微球的SEM图像;
图4为载铁椰壳活性炭壳聚糖复合微球相关材料的XRD图像;
图5为载铁椰壳活性炭壳聚糖复合微球在不同pH条件下对As(Ⅲ)的吸附情况;
具体实施方式
下面结合附图和实施例对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。
需要说明的是,下述实施方案中所述实验方法,如无特殊说明,均为常规方法,所述试剂和材料,如无特殊说明,均可从商业途径获得。
实施例1
(1)配制200ml 1.5%的醋酸溶液,加入5g粉末状椰壳活性炭,超声搅拌使其溶解均匀;加入5g壳聚糖粉末,再次超声搅拌,得椰壳活性炭壳聚糖混合液;
(2)称取0.1M的FeCl3·6H2O加入至椰壳活性炭壳聚糖混合液,搅拌至FeCl3·6H2O完全溶解,得含铁椰壳活性炭壳聚糖混合液;
(3)将含铁椰壳活性炭壳聚糖混合液滴加到20%NaOH溶液中,室温下静置固结24h,将NaOH溶液过滤,用去离子水洗涤至pH近中性,得湿态载铁椰壳活性炭壳聚糖复合微球;
(4)将湿态载铁椰壳活性炭复合微球置于5wt%的戊二醛-甲醇混合液,匀速振荡交联2.5h,过滤,并用乙醇溶液洗涤至无醛味,放置烘箱中,45℃烘干,即得载铁椰壳活性炭壳聚糖复合微球。
吸附实验显示,对于50mL初始浓度为25mg/L、pH为3的As(Ⅲ)溶液,50mg载铁椰壳活性炭壳聚糖复合微球的吸附量为11.870mg/g,未改性的椰壳活性炭壳聚糖复合微球吸附量为1.737mg/g。
实施例2
(1)配制200ml 1.5%的醋酸溶液,加入5g粉末状椰壳活性炭,超声搅拌使其溶解均匀;加入5g壳聚糖粉末,再次超声搅拌,得椰壳活性炭壳聚糖混合液;
(2)称取0.1M的FeCl3·6H2O加入至椰壳活性炭壳聚糖混合液,搅拌至FeCl3·6H2O完全溶解,得含铁椰壳活性炭壳聚糖混合液;
(3)将含铁椰壳活性炭壳聚糖混合液滴加到20%NaOH溶液中,室温下静置固结24h,将NaOH溶液过滤,用去离子水洗涤至pH近中性,得湿态载铁椰壳活性炭壳聚糖复合微球;
(4)将湿态载铁椰壳活性炭复合微球置于5wt%的戊二醛-甲醇混合液,匀速振荡交联2.5h,过滤,并用乙醇溶液洗涤至无醛味,放置烘箱中,45℃烘干,即得载铁椰壳活性炭壳聚糖复合微球。
吸附实验显示,对于50mL初始浓度为25mg/L、pH为7的As(Ⅲ)溶液,50mg载铁椰壳活性炭壳聚糖复合微球的吸附量为12.015mg/g,未改性的椰壳活性炭壳聚糖复合微球吸附量为0.975mg/g。
实施例3
(1)配制200ml 1.5%的醋酸溶液,加入5g粉末状椰壳活性炭,超声搅拌使其溶解均匀;加入5g壳聚糖粉末,再次超声搅拌,得椰壳活性炭壳聚糖混合液;
(2)称取0.1M的FeCl3·6H2O加入至椰壳活性炭壳聚糖混合液,搅拌至FeCl3·6H2O完全溶解,得含铁椰壳活性炭壳聚糖混合液;
(3)将含铁椰壳活性炭壳聚糖混合液滴加到20%NaOH溶液中,室温下静置固结24h,将NaOH溶液过滤,用去离子水洗涤至pH近中性,得湿态载铁椰壳活性炭壳聚糖复合微球;
(4)将湿态载铁椰壳活性炭复合微球置于5wt%的戊二醛-甲醇混合液,匀速振荡交联2.5h,过滤,并用乙醇溶液洗涤至无醛味,放置烘箱中,45℃烘干,即得载铁椰壳活性炭壳聚糖复合微球。
吸附实验显示,对于50mL初始浓度为25mg/L、pH为11的As(Ⅲ)溶液,50mg载铁椰壳活性炭壳聚糖复合微球的吸附量为6.517mg/g,未改性的椰壳活性炭壳聚糖复合微球吸附量为0mg/g。
Claims (7)
1.载铁椰壳活性炭壳聚糖复合微球的制备方法,其特征在于,包括步骤如下:
(1)用去离子水将颗粒状椰壳活性炭反复浸泡并冲洗,以去除灰分及表面杂质,将洗净的椰壳活性炭置于45℃烘箱中烘干备用;
(2)将干燥后的椰壳活性炭研磨成粉末状,并过150目筛;
(3)配制1.5%的醋酸溶液,加入粉末状椰壳活性炭,超声搅拌使其溶解均匀;
(4)往溶液中加入同质量的壳聚糖粉末,超声搅拌使其混合均匀,得椰壳活性炭壳聚糖混合溶液;
(5)称取0.1mol FeCl3·6H2O加入至椰壳活性炭壳聚糖混合溶液中,超声搅拌至FeCl3·6H2O完全溶解,得到含铁椰壳活性炭壳聚糖混合溶液;
(6)将该混合溶液滴加至NaOH溶液中,静置24h;用去离子水将静置后的载铁椰壳活性炭壳聚糖微球洗至pH接近中性,使其成球状,得载铁椰壳活性炭壳聚糖微球;
(7)将配制好的5wt%戊二醛-甲醇混合液倒入装有湿性载铁椰壳活性炭壳聚糖微球的烧杯中,匀速振荡3h,使其固结交联;将振荡后的微球过滤,用乙醇溶液洗涤至无醛味,放置烘箱中,45℃烘干,即得载铁椰壳活性炭壳聚糖复合微球。
2.如权利要求1所述的载铁椰壳活性炭壳聚糖复合微球的制备方法,其特征在于,步骤(1)中椰壳活性炭需要用去离子水多次清洗。
3.如权利要求1所述的载铁椰壳活性炭壳聚糖复合微球的制备方法,其特征在于,步骤(3)中称取粉末状椰壳活性炭的质量为5g。
4.如权利要求1所述的载铁椰壳活性炭壳聚糖复合微球的制备方法,其特征在于,步骤(4)中称取壳聚糖的质量为5g,椰壳活性炭同壳聚糖质量比为1:1。
5.如权利要求1所述的载铁椰壳活性炭壳聚糖复合微球的制备方法,其特征在于,步骤(6)中滴加采用内径为1.5mm的滴管进行。
6.如权利要求1所述的载铁椰壳活性炭壳聚糖复合微球的制备方法,其特征在于,步骤(6)中NaOH溶液的体积分数为20%。
7.如权利要求1~5任一项所述的载铁椰壳活性炭壳聚糖复合微球作为吸附剂的用途。
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