CN105582903B - 一种片状污水处理复合凝胶材料及其制备方法 - Google Patents
一种片状污水处理复合凝胶材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种片状污水处理复合凝胶材料及其制备方法。该片状污水处理复合凝胶材料其各组分的重量份组成为：聚乙烯醇20~30份，三乙烯四胺80~120份，交联剂1~3份，接枝剂0.1~0.5份，表面处理剂0.05~0.2份，相容剂0.04~0.2份，无机粉体10~15份。通过聚乙烯醇与三乙烯四胺接枝共聚，加入无机粉体交联制备成复合凝胶，再经过挤出、热压得到一种片状污水处理复合凝胶材料，可有效应用于污水处理对重金属离子的吸附作用，其片状污水处理凝胶材料使用方便，制备工艺简单，成本低，具有市场应用前景。
Description
技术领域
本发明属于污水处理领域，具体涉及一种片状污水处理复合凝胶材料及其制备方法。
背景技术
随着社会经济的发展，人们生活质量的提高，附带的生产污水的排放也逐年增加，目前我国污水量已经达到820亿吨，年增长为20亿吨，每天污水的排放量近2亿吨。污水的大量排放，从而造成了江、河、湖、海以及环境的严重污染，对人们的身体健康将造成非常大的伤害。如无机盐汞污水将抑制人体中各种酶的活性，使细胞的正常功能发生障碍，同时在人体中将被全部吸收掉，无法进行代谢排出体外。又如日本的水俣病、痛痛病，这些污水造成人体疾病，所带来的身体以及心理上的伤害将无法估量。为了改善污水排放对环境造成恶劣影响，污水处理技术应运而生，对于污水处理需要达到某一排放标准或可进行再生时才能排放到环境中，污水处理广泛应用于建筑、农业、交通、能源、石化、环保、医疗、餐饮等各个领域。工业污水所含的污染物因工厂种类不同而千差万别，工业所排出的污水将直接注入水体中引起污染，同时在农业中由于耕作或开荒使土地表面疏松，在土壤和地形还未稳定时降雨，大量泥沙流入水中，增加水中悬浮物，其中还包括农药、化肥造成水体的污染。对于污水处理必须严格负责，才能很好的保护环境，节约水资源，防止水体污染。对于污水处理已经成为全球性问题，因此需要开发一种高效、低成本、无二次污染的污水处理剂。
公开号为104722272A的专利公开了一种新型废水污水处理吸附材料及其制备工艺方法，该发明包括膨润土有机改性、膨润土固定化和连续化处理含酚工业废水三个部分，此发明如果污水中离子浓度过高会压缩膨润土颗粒双电层，抑制膨润土的分散和扩散，甚至使膨润土产生凝聚和聚结，因此不能有效的应用于污水处理，效果不佳、成本较高。公开号为103601433A的专利公开了一种制备污水处理用高效除磷材料的方法，该发明材料制备包括以下步骤（1）将粘土、普通水泥、熟石灰和油页岩渣在105℃下干燥12~24小时；（2）将步骤（1）干燥后的粘土120~180克、普通水泥40~60克、熟石灰80~120克和油页岩80~120克，加水190~280ml，利用曝气装置通入0.2L/min空气，充分搅拌10~25分钟，即获得混合物；（3）放入造粒机制成粒径为3.5~4.5mm颗粒；（4）在105℃干燥12~24小时，即获得污水处理用高效除磷材料，此发明对重金属离子吸附性较差对污水处理效果不佳，制备工艺复杂。
发明内容
目前污水处理材料对重金属离子以及动植物油吸附性差、成本高的缺陷，本发明的目的在于提供一种片状污水处理复合凝胶材料及其制备方法，该片状污水处理复合凝胶材料是通过聚乙烯醇与三乙烯四胺接枝共聚，加入无机粉体交联制备成复合凝胶，再经过挤出、热压得到一种片状污水处理复合凝胶材料，可有效应用于污水处理对重金属离子的吸附作用，其片状材料具有使用方便的特点。
本发明通过以下技术方案达到发明目的：
一种片状污水处理复合凝胶材料的制备方法，包括如下步骤：
(1) 以重量份计，将10~15份无机粉体在球磨机中研磨至1~2μm，再置于高速混合机中，加入0.05~0.2份表面处理剂，控制温度在80~120℃，转速为900~1200r/min条件下，搅拌10~15min，最后冷却至室温，所述的表面处理剂为硬脂酸盐、磷酸乙二胺、磷酸丙二胺、氯化铵中的一种；
(2) 将20~30份聚乙烯醇，80~90份水加入到氮气保护条件下的反应釜中，在80~95℃水浴中搅拌5~10min使其完全溶解，加入0.1~0.5份接枝剂，在搅拌过程中缓慢加入80~120份三乙烯四胺，进行链引发聚合反应，控制聚合温度在60~70℃，聚合时间为2~3h，得到聚乙烯醇/三乙烯四胺接枝共聚物，所述的接枝剂为硝酸铈铵、丁二酸酐中的一种；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及1~3份交联剂、0.04~0.2份相容剂加入到反应釜中，在温度为50~60℃、pH值为6~7搅拌条件下反应1~ 2h，得到复合凝胶，所述的交联剂为二羟甲基二羟乙基脲、戊二醛、Ｎ,Ｎ’－亚甲基丙烯酰胺中的一种；
(4) 将步骤(3)所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为160~180℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料的制备方法。
步骤(1)所述的无机粉体为蒙脱土、膨润土、硅藻土、沸石、水滑石、海泡石、蛇纹石中的一种。
步骤(2)所述的聚乙烯醇分子式为[C2H4O]n，其n为435~4347，分子量为88000~180000，醇解度为80%~99%。
步骤(3)所述的相容剂为马来酸酐接枝苯乙烯、马来酸酐接枝丙烯腈-丁二烯苯乙烯共聚物中的一种。
步骤(4)中所述的双螺杆挤出机，螺杆转速为90~120r/min，各区温度控制在：一区150~160℃；二区165~170℃；三区170~165℃；四区165~160℃；五区160~145℃。
上述的一种片状污水处理复合凝胶材料及其制备方法所制得的一种片状污水处理复合凝胶材料及其制备方法。
本发明在接枝剂作用下聚乙烯醇/三乙烯四胺接枝共聚，使其对重金属离子的强吸附性以及螯合作用，三乙烯四胺存在较活泼的氨基对重金属离子具有强螯合作用，在交联剂的作用下制备成三维网络结构的复合凝胶，增强对污水的处理能力以及吸附作用，添加无机粉体使得材料具有耐水性、耐热性、增强增韧的作用，同时还提高吸附性，接枝共聚物保留接枝物各自性质，增强聚合物其特性，如吸附性、螯合作用，制备成片状其使用方便，工艺简单。
本发明具有以下的突出特点和有益效果：
1、本发明一种片状污水处理复合凝胶材料，利用接枝共聚的特性，使聚乙烯醇与三乙烯四胺接枝共聚，可有效对重金属离子的吸附作用。
2、本发明一种片状污水处理复合凝胶材料，制备成片状其使用、运输方便。
3、本发明一种片状污水处理复合凝胶材料制备工艺简单，成本低，具有广阔市场应用前景。
具体实施方式
实施例1
(1) 将10份蒙脱土在球磨机中研磨至1μm，再置于高速混合机中，加入0.05份硬质酸盐，控制温度在80℃，转速为900r/min条件下，搅拌10min，最后冷却至室温；
(2) 将20份聚乙烯醇，80份水加入到氮气保护条件下的反应釜中，在80℃水浴中搅拌5min使其完全溶解，加入0.1份硝酸铈铵，在搅拌过程中缓慢加入80份三乙烯四胺，进行链引发聚合反应，控制聚合温度在60℃，聚合时间为2h，经过洗涤、干燥得到聚乙烯醇/三乙烯四胺接枝共聚物；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及1份二羟甲基二羟乙基脲、0.04份马来酸酐接枝苯乙烯加入到反应釜中，在温度为50℃、pH值为6搅拌条件下反应1h，得到复合凝胶；
(4) 将步骤(3)所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为160℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料。
实施例2
(1) 将11份膨润土在球磨机中研磨至1.2μm，再置于高速混合机中，加入0.08份磷酸乙二胺，控制温度在90℃，转速为1000r/min条件下，搅拌11min，最后冷却至室温；
(2) 将22份聚乙烯醇，82份水加入到氮气保护条件下的反应釜中，在82℃水浴中搅拌6min使其完全溶解，加入0.2份丁二酸酐，在搅拌过程中缓慢加入90份三乙烯四胺，进行链引发聚合反应，控制聚合温度在62℃，聚合时间为2.2h，经过洗涤、干燥得到聚乙烯醇/三乙烯四胺接枝共聚物；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及1.2份戊二醛、0.08份马来酸酐接枝丙烯腈-丁二烯苯乙烯共聚物加入到反应釜中，在温度为52℃、pH值为6.2搅拌条件下反应1.2h，得到复合凝胶；
(4) 将上述所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为165℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料。
实施例3
(1) 将12份硅藻土在球磨机中研磨至1.4μm，再置于高速混合机中，加入0.1份磷酸丙二胺，控制温度在100℃，转速为1100r/min条件下，搅拌12min，最后冷却至室温；
(2) 将24份聚乙烯醇，84份水加入到氮气保护条件下的反应釜中，在86℃水浴中搅拌7min使其完全溶解，加入0.3份硝酸铈铵，在搅拌过程中缓慢加入100份三乙烯四胺，进行链引发聚合反应，控制聚合温度在64℃，聚合时间为2.4h，经过洗涤、干燥得到聚乙烯醇/三乙烯四胺接枝共聚物；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及1.4份Ｎ,Ｎ’－亚甲基丙烯酰胺、0.1份马来酸酐接枝苯乙烯加入到反应釜中，在温度为54℃、pH值为6.4搅拌条件下反应1.4h，得到复合凝胶；
(4) 将上述所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为170℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料。
实施例4
(1) 将13份沸石在球磨机中研磨至1.6μm，再置于高速混合机中，加入0.15份氯化铵，控制温度在110℃，转速为1200r/min条件下，搅拌13min，最后冷却至室温；
(2) 将26份聚乙烯醇，86份水加入到氮气保护条件下的反应釜中，在88℃水浴中搅拌8min使其完全溶解，加入0.4份丁二酸酐，在搅拌过程中缓慢加入110份三乙烯四胺，进行链引发聚合反应，控制聚合温度在66℃，聚合时间为2.6h，经过洗涤、干燥得到聚乙烯醇/三乙烯四胺接枝共聚物；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及2份戊二醛、0.14份马来酸酐接枝苯乙烯加入到反应釜中，在温度为56℃、pH值为6.8搅拌条件下反应1.8h，得到复合凝胶；
(4) 将上述所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为175℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料。
实施例5
(1) 将15份水滑石在球磨机中研磨至1.8μm，再置于高速混合机中，加入0.2份磷酸乙二胺，控制温度在120℃，转速为1200r/min条件下，搅拌14min，最后冷却至室温；
(2) 将28份聚乙烯醇，88份水加入到氮气保护条件下的反应釜中，在92℃水浴中搅拌9min使其完全溶解，加入0.5份丁二酸酐，在搅拌过程中缓慢加入120份三乙烯四胺，进行链引发聚合反应，控制聚合温度在68℃，聚合时间为3h，经过洗涤、干燥得到聚乙烯醇/三乙烯四胺接枝共聚物；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及2.4份二羟甲基二羟乙基脲、0.18份马来酸酐接枝丙烯腈-丁二烯苯乙烯共聚物加入到反应釜中，在温度为58℃、pH值为7搅拌条件下反应2h，得到复合凝胶；
(4) 将上述所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为180℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料。
下表为各实施例污水处理性能：
| 检测项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
| Cd2+去除率(%) | 94.5 | 93.5 | 92.4 | 96.2 | 97.7 |
| Pb2+去除率(%) | 96.4 | 95.4 | 96.8 | 96.9 | 99.5 |
| Ni2+去除率(%) | 94.2 | 97.6 | 94.7 | 95.8 | 98.3 |
| Hg2+去除率(%) | 98.7 | 95.8 | 97.6 | 97.6 | 96.8 |
| Cu2+去除率(%) | 95.7 | 96.6 | 95.3 | 99.4 | 94.8 |
Claims (6)
1.一种片状污水处理复合凝胶材料的制备方法，其特征在于包括如下步骤：
(1) 以重量份计，将10~15份无机粉体在球磨机中研磨至1~2μm，再置于高速混合机中，加入0.05~0.2份表面处理剂，控制温度在80~120℃，转速为900~1200r/min条件下，搅拌10~15min，最后冷却至室温，所述的表面处理剂为硬脂酸盐、磷酸乙二胺、磷酸丙二胺、氯化铵中的一种；
(2) 将20~30份聚乙烯醇，80~90份水加入到氮气保护条件下的反应釜中，在80~95℃水浴中搅拌5~10min使其完全溶解，加入0.1~0.5份接枝剂，在搅拌过程中缓慢加入80~120份三乙烯四胺，进行链引发聚合反应，控制聚合温度在60~70℃，聚合时间为2~3h，经过洗涤、干燥得到聚乙烯醇/三乙烯四胺接枝共聚物，所述的接枝剂为硝酸铈铵、丁二酸酐中的一种；
(3) 将步骤(2)所得的接枝共聚物与步骤(1)的产物以及1~3份交联剂、0.04~0.2份相容剂加入到反应釜中，在温度为50~60℃、pH值为6~7搅拌条件下反应1~2h，得到复合凝胶，所述的交联剂为二羟甲基二羟乙基脲、戊二醛、Ｎ,Ｎ’－亚甲基丙烯酰胺中的一种；
(4) 将步骤(3)所得到的复合凝胶经过双螺杆挤出机，通过熔融、混炼、切粒，再经过温度为160~180℃平板硫化机热压成片，得到一种片状污水处理复合凝胶材料。
2.根据权利要求1所述的一种片状污水处理复合凝胶材料的制备方法，其特征在于步骤(1)所述的无机粉体为蒙脱土、膨润土、硅藻土、沸石、水滑石、海泡石、蛇纹石中的一种。
3.根据权利要求1所述的一种片状污水处理复合凝胶材料的制备方法，其特征在于步骤(2)所述的聚乙烯醇分子式为[C2H4O]n，其n为435~4347，分子量为88000~180000，醇解度为80%~99%。
4.根据权利要求1所述的一种片状污水处理复合凝胶材料的制备方法，其特征在于步骤(3)所述的相容剂为马来酸酐接枝苯乙烯、马来酸酐接枝丙烯腈-丁二烯苯乙烯共聚物中的一种。
5.根据权利要求1所述的一种片状污水处理复合凝胶材料的制备方法，其特征在于步骤(4)中所述的双螺杆挤出机，螺杆转速为90~120r/min，各区温度控制在：一区150~160℃；二区165~170℃；三区170~165℃；四区165~160℃；五区160~145℃。
6.权利要求1~5中任一项所述的一种片状污水处理复合凝胶材料的制备方法所制得的一种片状污水处理复合凝胶材料。
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