CN105597428A - 一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法 - Google Patents

一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法 Download PDF

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CN105597428A
CN105597428A CN201610098213.1A CN201610098213A CN105597428A CN 105597428 A CN105597428 A CN 105597428A CN 201610098213 A CN201610098213 A CN 201610098213A CN 105597428 A CN105597428 A CN 105597428A
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余煜玺
谭晓林
郭银清
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Lvna Technology Co Ltd
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Abstract

本发明公开了一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法，包括如下步骤：(1)将高分子聚合物溶于溶剂中，搅拌均匀，得到均一纺丝体系；(2)将上述均一纺丝体系采用金属圆柱电极在尼龙无纺布上进行静电纺丝以得到一复合纳米纤维膜；(3)将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解，水洗至中性后，置于聚乙烯胺水溶液中，再进行干燥；(4)将步骤(3)加工后的复合纳米纤维膜置于戊二醛水溶液中浸泡，水洗后进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料。本发明制备条件温和，工艺简单，制备的纳米纤维过滤材料的纤维直径小、孔隙率高、孔径小、比表面积大，能有效吸附废水中的Cr(Ⅵ)，且在弱碱液中解吸后可循环使用。

Description

一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法
技术领域
本发明属于污水处理装置技术领域，具体涉及一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法。
背景技术
铬是一种对环境和人体伤害非常大的重金属元素。铬在水中通常以三价和六价两种形态存在，六价铬的毒性远大于三价铬。化工、轻工、冶金、纺织、机械等行业都会产生大量的铬废水、废渣，而这些铬废水、废渣都由于当前经济、技术等原因不能进行有效处理，直接排放进江河湖海中，对水环境造成巨大的污染。据了解，水体中Cr(Ⅵ)浓度超过100mg/L就可以对水生物致死。人体如摄入超大剂量的铬会导致肾脏和肝脏的损伤、恶心、胃肠道刺激、胃溃疡、痉挛甚至死亡。故如何降低水中的Cr(Ⅵ)浓度成为当前环境保护领域中非常紧迫的问题。
发明内容
本发明的目的在于提供一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法。
本发明的原理如下：
本发明的具体技术方案如下：
一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法，包括如下步骤：
(1)将高分子聚合物溶于溶剂中，搅拌均匀，得到6～20wt％的均一纺丝体系；该高分子聚合物为聚酰胺、聚氨酯、聚丙烯腈或聚醚酰亚胺；
(2)将上述均一纺丝体系采用金属圆柱电极在尼龙无纺布上进行静电纺丝以得到一复合纳米纤维膜，静电纺丝的工艺参数为：输出电压为35～85Kv，接收距离为8～50cm，纺丝温度为室温，湿度为30～80％；
(3)将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解15～70min，水洗至中性后，置于1～3wt％的聚乙烯胺水溶液中10～30min，再于55～65℃进行干燥，该碱性水解液中含有20～85wt％的乙醇；
(4)将步骤(3)加工后的复合纳米纤维膜置于浓度为10～220mmol/L的戊二醛水溶液中浸泡1～13min，水洗后于55～65℃进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料。
在本发明的一个优选实施方案中，所述溶剂为水、乙醇、氯仿、N，N-二甲基甲酰胺、乙酸、N-甲基吡咯烷酮、四氢呋喃、六氟异丙醇和甲酸中的至少一种。
在本发明的一个优选实施方案中，所述碱性水解液为含有20～85wt％乙醇的氢氧化钠溶液或碳酸钠溶液。
在本发明的一个优选实施方案中，所述步骤(1)为：将高分子聚合物溶于溶剂中，搅拌均匀，得到6～20wt％的均一纺丝体系。
在本发明的一个优选实施方案中，所述步骤(2)中静电纺丝的工艺参数为：输出电压为35～85Kv，接收距离为8～50cm，纺丝温度为室温，湿度为30～80％。
在本发明的一个优选实施方案中，所述步骤(3)为：将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解15～70min，水洗至中性后，置于1～3wt％的聚乙烯胺水溶液中10～30min，再于55～65℃进行干燥。
在本发明的一个优选实施方案中，所述步骤(4)为：将步骤(3)加工后的复合纳米纤维膜置于浓度为10～200mmol/L的戊二醛水溶液中浸泡1～13min，水洗后于55～65℃进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料。
本发明的有益效果是：本发明的制备方法通过静电纺丝技术制备复合纳米纤维膜，再经化学改性后得到的具有吸附Cr(Ⅵ)功能的纳米纤维过滤材料，其制备条件温和，工艺简单，制备的纳米纤维过滤材料的纤维直径小、孔隙率高、孔径小、比表面积大，能有效吸附废水中的Cr(Ⅵ)，且在弱碱液中解吸后可循环使用，是化工污水净化领域的优良选材。
附图说明
图1为本发明实施例1制备的纳米纤维过滤材料的SEM图。
图2为本发明实施例1制备的纳米纤维过滤材料的FT-IR图。
图3为本发明实施例2制备的纳米纤维过滤材料的SEM图。
图4为本发明实施例2制备的纳米纤维过滤材料的FT-IR图。。
具体实施方式
以下通过具体实施方式结合附图对本发明的技术方案进行进一步的说明和描述。
实施例1
(1)将8g聚丙烯腈(PAN)加入到92g二甲基甲酰胺(DMF)中，并在50℃条件下充分搅拌2h得到质量分数为8wt％的PAN/DMF纺丝溶液(即均一纺丝体系)。
(2)将上述纺丝体系倒入装有金属圆柱电极的槽内，以尼龙无纺布作为基底，在输出电压为70Kv、接收距离为14cm、温度为30℃、湿度为45％的条件下进行静电纺丝，纺丝5分钟后得到一层均匀的白色纳米纤维膜(即所述复合纳米纤维膜)。
(3)取10g复合纳米纤维膜置于由85mL无水乙醇、15mL去离子水和3gNaOH所组成的碱性水解液中水解30min，得到水解PAN纳米纤维膜，然后用去离子水清洗至中性后，置于质量分数为3wt％的聚乙烯胺水溶液中15min，放入60℃的烘箱内干燥若干分钟。
(4)将上述干燥后的纳米纤维膜置于浓度为80mmol/L的戊二醛水溶液中1min，水洗后2次后放入60℃的烘箱内干燥，最终得到具有吸附Cr(Ⅵ)功能的纳米纤维过滤材料。
图1、2分别为所制备的纳米纤维过滤材料的扫描电镜图和红外谱图。
实施例2
(1)将10g聚醚酰亚胺(PEI)加入到90gN-甲基吡咯烷酮(NMP)中，并在50℃条件下充分搅拌12h得到质量分数为10wt％的PEI/NMP纺丝溶液(即均一纺丝体系)。
(2)将上述纺丝体系倒入装有金属圆柱电极的槽内，以尼龙无纺布作为基底，在输出电压为75Kv、接收距离为18cm、温度为25℃、湿度为30％的条件下进行静电纺丝，纺丝5分钟后得到一层均匀的白色纳米纤维膜(即所述复合纳米纤维膜)。
(3)取10g复合纳米纤维膜置于由80mL无水乙醇、20mL去离子水和5gNaOH所组成的碱性水解液中水解45min，得到水解PEI纳米纤维膜，然后用去离子水清洗至中性后，置于质量分数为3wt％的聚乙烯胺水溶液中20min，放入60℃的烘箱内干燥若干分钟。
(4)将上述干燥后的纳米纤维膜置于浓度为150mmol/L的戊二醛水溶液中2min，水洗后2次后放入60℃的烘箱内干燥，最终得到具有吸附Cr(Ⅵ)功能的纳米纤维过滤材料。
图3、4分别为所制备的纳米纤维过滤材料的扫描电镜图和红外谱图。
实施例3
(1)将9g聚酰胺6(PA6)加入到91g甲酸(FA)和乙酸(HAc)的混合液(甲酸与乙酸的质量比为3:1)中，并在室温条件下充分搅拌10h得到质量分数为9wt％的PA6/FA-HAc纺丝溶液(即均一纺丝体系)。
(2)将上述纺丝体系倒入装有金属圆柱电极的槽内，以尼龙无纺布作为基底，在输出电压为80Kv、接收距离为17cm、温度为20℃、湿度为65％的条件下进行静电纺丝，纺丝5分钟后得到一层均匀的白色纳米纤维膜(即所述复合纳米纤维膜)。
(3)取10g复合纳米纤维膜置于由90mL无水乙醇、10mL去离子水和5gNaOH所组成的碱性水解液中水解60min，得到水解PA6纳米纤维膜，然后用去离子水清洗至中性后，置于质量分数为3wt％的聚乙烯胺水溶液中15min，放入60℃的烘箱内干燥若干分钟。
(4)将上述干燥后的纳米纤维膜置于浓度为100mmol/L的戊二醛水溶液中3min，水洗后2次后放入60℃的烘箱内干燥，最终得到具有吸附Cr(Ⅵ)功能的纳米纤维过滤材料。
实施例4
(1)将10g聚氨酯(PU)加入到90g二甲基甲酰胺(DMF)和四氢呋喃(THF)的混合液(二甲基甲酰胺和四氢呋喃质量比为2:1)中，并在20℃条件下充分搅拌2h得到质量分数为10wt％的PAN/DMF-THF纺丝溶液(即均一纺丝体系)。
(2)将上述纺丝体系倒入装有金属圆柱电极的槽内，以尼龙无纺布作为基底，在输出电压为70Kv、接收距离为14cm、温度为30℃、湿度为45％的条件下进行静电纺丝，纺丝5分钟后得到一层均匀的白色纳米纤维膜(即所述复合纳米纤维膜)。
(3)取10g复合纳米纤维膜置于由40mL无水乙醇、60mL去离子水和4gNaOH所组成的碱性水解液中水解30min，得到水解PU纳米纤维膜，然后用去离子水清洗至中性后，置于质量分数为3wt％的聚乙烯胺水溶液中15min，放入60℃的烘箱内干燥若干分钟。
(4)将上述干燥后的纳米纤维膜置于浓度为200mmol/L的戊二醛水溶液中1min，水洗后2次后放入60℃的烘箱内干燥，最终得到具有吸附Cr(Ⅵ)功能的纳米纤维过滤材料。
复合纳米过滤材料吸附Cr(Ⅵ)试验
准确称取一定质量的上述实施例制备的纳米纤维过滤材料，置于Cr(Ⅵ)浓度为50mg/L、pH值为5(本发明制得的纳米纤维过滤材料对污水中Cr(Ⅵ)吸附的最佳pH值是3～6)的2000mL溶液中，控制温度在30℃并恒温振荡10h后取出，室温下置于0.1.mol/L的氢氧化钠水溶液中1h解吸附，干燥后循环使用。参照二苯碳酰二肼分光光度法，使用USB2000型紫外-可见分光光度计(美国海洋光学公司)测定溶液中吸附前后六价铬离子的浓度，计算得出复合纳米过滤材料的Cr(Ⅵ)吸附量。结果如下表：
本领域普通技术人员可知，本发明的技术方案在下述范围内变化时，仍然能够得到与上述实施例相同或相近的技术效果。
一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法，包括如下步骤：
(1)将高分子聚合物溶于溶剂中，搅拌均匀，得到6～20wt％的均一纺丝体系；该高分子聚合物为聚酰胺、聚氨酯、聚丙烯腈或聚醚酰亚胺；
(2)将上述均一纺丝体系采用金属圆柱电极在尼龙无纺布上进行静电纺丝以得到一复合纳米纤维膜，静电纺丝的工艺参数为：输出电压为35～85Kv，接收距离为8～50cm，纺丝温度为室温，湿度为30～80％，优选的工艺参数为：输出电压为40～80Kv，接收距离为10～50cm，纺丝温度为室温，湿度为30～70％；
(3)将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解15～70min，水洗至中性后，置于1～3wt％的聚乙烯胺水溶液中10～30min，再于55～65℃进行干燥，该碱性水解液中含有20～85wt％的乙醇，优选的，将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解20～30min，水洗至中性后，置于1～3wt％的聚乙烯胺水溶液中10～30min，再于55～65℃进行干燥；
(4)将步骤(3)加工后的复合纳米纤维膜置于浓度为10～220mmol/L的戊二醛水溶液中浸泡1～13min，水洗后于53～67℃进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料，优选的，将步骤(3)加工后的复合纳米纤维膜置于浓度为10～200mmol/L的戊二醛水溶液中浸泡1～10min，水洗后于55～65℃进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料。
所述溶剂为水、乙醇、氯仿、N，N-二甲基甲酰胺、乙酸、N-甲基吡咯烷酮、四氢呋喃、六氟异丙醇和甲酸中的至少一种。
所述碱性水解液为含有20～85wt％乙醇的氢氧化钠溶液或碳酸钠溶液。
以上所述，仅为本发明的较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。

Claims (7)

1.一种用于去除污水中Cr(VI)的纳米纤维过滤材料的制备方法，其特征在于：包括如下步骤：
(1)将高分子聚合物溶于溶剂中，搅拌均匀，得到6～20wt％的均一纺丝体系；该高分子聚合物为聚酰胺、聚氨酯、聚丙烯腈或聚醚酰亚胺；
(2)将上述均一纺丝体系采用金属圆柱电极在尼龙无纺布上进行静电纺丝以得到一复合纳米纤维膜，静电纺丝的工艺参数为：输出电压为35～85Kv，接收距离为8～50cm，纺丝温度为室温，湿度为30～80％；
(3)将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解15～70min，水洗至中性后，置于1～3wt％的聚乙烯胺水溶液中10～30min，再于55～65℃下进行干燥，该碱性水解液中含有20～85wt％的乙醇；
(4)将步骤(3)加工后的复合纳米纤维膜置于浓度为10～220mmol/L的戊二醛水溶液中浸泡1～13min，水洗后于53～67℃进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料。
2.如权利要求1所述的制备方法，其特征在于：所述溶剂为水、乙醇、氯仿、N，N-二甲基甲酰胺、乙酸、N-甲基吡咯烷酮、四氢呋喃、六氟异丙醇和甲酸中的至少一种。
3.如权利要求1所述的制备方法，其特征在于：所述碱性水解液为含有20～85wt％乙醇的氢氧化钠溶液或碳酸钠溶液。
4.如权利要求1至3中任一权利要求所述的制备方法，其特征在于：所述步骤(1)为：将高分子聚合物溶于溶剂中，搅拌均匀，得到6～20wt％的均一纺丝体系。
5.如权利要求1至3中任一权利要求所述的制备方法，其特征在于：所述步骤(2)中静电纺丝的工艺参数为：输出电压为35～85Kv，接收距离为8～50cm，纺丝温度为室温，湿度为30～80％。
6.如权利要求1至3中任一权利要求所述的制备方法，其特征在于：所述步骤(3)为：将上述复合纳米纤维膜在浓度为1～5％的碱性水解液中水解15～70min，水洗至中性后，置于1～3wt％的聚乙烯胺水溶液中10～30min，再于55～65℃进行干燥。
7.如权利要求1至3中任一权利要求所述的制备方法，其特征在于：所述步骤(4)为：将步骤(3)加工后的复合纳米纤维膜置于浓度为10～200mmol/L的戊二醛水溶液中浸泡1～10min，水洗后于55～65℃进行干燥，得到用于去除污水中Cr(VI)的纳米纤维过滤材料。
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