CN113398894A - 吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法 - Google Patents

吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法 Download PDF

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CN113398894A
CN113398894A CN202110624297.9A CN202110624297A CN113398894A CN 113398894 A CN113398894 A CN 113398894A CN 202110624297 A CN202110624297 A CN 202110624297A CN 113398894 A CN113398894 A CN 113398894A
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polyacrylonitrile
mixed solution
nanofiber membrane
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曹新旺
杨银芝
严元
黄芷嫣
方凯炀
谢锦鹏
陈益人
邓中民
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Wuhan Textile University
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    • B01J20/28038—Membranes or mats made from fibers or filaments
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
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Abstract

本发明涉及一种吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法，制备方法包括以下步骤：1、利用竹笋壳提取竹笋壳纤维，并制备纳米晶须；2、将竹笋壳纳米晶须分散在N,N‑二甲基甲酰胺中，得到混合溶液，混合溶液中竹笋壳纳米晶须的质量浓度为0.2‑1.4％，并对混合溶液进行超声波处理；3、向上一步处理后的混合溶液中加入聚丙烯腈得到纺丝液，纺丝液中聚丙烯腈的质量分数为10‑20％，在50‑70℃条件下对纺丝液磁力搅拌3‑4h；4、对纺丝液采用静电纺丝技术制备得到纳米纤维膜。本发明以农业废弃物竹笋壳作为原料，改善聚丙烯腈薄膜的疏水性能，成本低，实现了资源的合理利用，反应条件温和，操作简单。

Description

吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法
技术领域
本发明涉及印染废水制备方法领域，具体涉及一种吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法。
背景技术
近年来，随着印染工业的发展，越来越多的废水未被完全处理就排放出去，严重污染环境对人体的健康也造成了危害，传统水处理系统对其去除效果差。本研究以竹笋壳纤维为原料制备竹笋壳纳米晶须，然后采用静电纺丝技术制备聚丙烯腈纳米纤维膜，使其用于废水中染料的吸附。聚丙烯腈(PAN)因其成膜性好、不易水解及化学稳定性好而被广泛应用于静电纺丝中作为基底的存在。静电纺丝技术制备的纳米纤维具有直径小、孔隙率高、比表面积小等特点而广泛用于制膜工艺。纳米纤维素是一种储量丰富的可再生资源，具有良好的可降解性和生物相容性，其良好的亲水性，可改善聚丙烯腈薄膜的疏水性能。
发明内容
本发明要解决的技术问题是针对以上不足，提供一种吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法。
为解决以上技术问题，本发明采用以下技术方案：
吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法，包括以下步骤：
步骤1、利用竹笋壳提取竹笋壳纤维，并利用竹笋壳纤维制备纳米晶须；
步骤2、将竹笋壳纳米晶须分散在N,N-二甲基甲酰胺中，得到混合溶液，混合溶液中竹笋壳纳米晶须的质量浓度为0.2-1.4％，并对混合溶液进行超声波处理；
步骤3、向上一步处理后的混合溶液中加入聚丙烯腈，得到纺丝液，纺丝液中聚丙烯腈的质量分数为10-20％，在50-70℃条件下对纺丝液磁力搅拌 3-4h；
步骤4、利用上一步处理后得到的纺丝液，采用静电纺丝技术制备得到纳米纤维膜。
进一步的，所述步骤2的混合溶液中竹笋壳纳米晶须的质量浓度为1.4％。
进一步的，所述步骤3的纺丝液中聚丙烯腈的质量分数为15％。
吸附印染废水的聚丙烯腈纳米纤维膜，由上述方法制备得到。
有益效果：1.纳米纤维素具有良好的亲水性和生物相容性，本发明可改善聚丙烯腈薄膜的疏水性能。2.以农业废弃物竹笋壳作为原料成本低，实现了资源的合理利用。3.反应条件温和，操作简单。
下面结合实施例对本发明进行详细说明。
具体实施方式
以下对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
吸附印染废水的聚丙烯腈纳米纤维膜的制备方法，包括以下步骤：
(1)竹笋壳纤维的提取
竹笋壳于50℃温水中清洗去除表面的绒毛及杂质，在烘箱中烘干备用，将烘干的竹笋壳剪切成小块(纵向30mm，横截面2×2mm)，以浴比1:40，加入2mL/LH2SO4在60℃水浴锅中加热1h，常温下用清水将竹笋壳洗涤至中性，并将其放入烘箱中70℃烘干备用，取5g处理过的竹笋壳以浴比1:40，煮练温度为95℃、氢氧化钠用量为18g/L、过氧化氢用量为40mL/L的水浴锅中碱煮150min，用2mL/LH2SO4以浴比1:20进行酸洗中和纤维表面的碱性溶液，最后常温下用清水洗涤至中性烘干即得到竹笋壳纤维。
(2)竹笋壳纳米晶须的制备
将提取的竹笋壳纤维粉碎过60目筛得到0.03mm的纤维粉末，在浴比为 1：30的二甲基亚砜中处理6h温度为50℃，然后用离心机洗涤至中性，将得到的样品放入70℃烘箱中烘干。采用浴比为1：100，并加入0.042gTEMPO， 0.6gNaBr，并逐滴加入一定量浓度为12％的NaClO溶液，并调节PH值为10-11，匀速搅拌3h，等PH值保持稳定然后加入5mL无水乙醇结束反应，将得到的溶液于离心机中以5000rpm转速离心5分钟反复洗涤5-6次至中性，去除离心管中的上清液取沉淀，以固液比为1：150，放入高速均质仪中以10000rpm 转速分散10分钟，得到纳米纤维素晶须悬浮液液。将其放入-20℃中冷冻处理1天，取出后置于冷冻干燥机中，干燥2天后取出得到白色竹笋壳纳米纤维素晶须。
(3)聚丙烯腈纳米纤维膜的制备
将浓度为0％、0.2％、0.6％、1％、1.4％、1.6％的竹笋壳纳米晶须分散在 N,N-二甲基甲酰胺中，并在40℃条件下超声30分钟。再加入聚丙烯腈配置质量分数为15％的聚丙烯腈纺丝液，在60℃条件下磁力搅拌3h待溶液呈透明浅黄色，采用静电纺丝技术制备得到纳米纤维膜。静电纺丝条件为：电压 12KV，接收距离20cm，注射器流速1mL/h。
(4)聚丙烯腈纳米纤维膜对染料的吸附
配置浓度为0mg/L、0.2mg/L、0.4mg/L、0.6mg/L、0.8mg/L、1mg/L的亚甲基蓝(MB)溶液，测试该浓度在可见光下的吸光度，绘制浓度范围在 0-1mg/L的标准浓度-吸光度曲线，测试不同含量纳米晶须制备得到纳米纤维膜对MB的吸附能力，结果表明随着竹笋壳纳米晶须含量增加对MB的吸附能力越强，添加量为1.4％时纳米纤维膜对MB的吸附能力较好大约为98％，当纤维素纳米晶须达到一定浓度后，吸附基团的数量远远大于染料的数量，因此添加量大于1.4％后吸附效果并没有明显变化。
以上所述为本发明最佳实施方式的举例，其中未详细述及的部分均为本领域普通技术人员的公知常识。本发明的保护范围以权利要求的内容为准，任何基于本发明的技术启示而进行的等效变换，也在本发明的保护范围之内。

Claims (4)

1.吸附印染废水的聚丙烯腈纳米纤维膜的制备方法，其特征在于，包括以下步骤：
步骤1、利用竹笋壳提取竹笋壳纤维，并利用竹笋壳纤维制备纳米晶须；
步骤2、将竹笋壳纳米晶须分散在N,N-二甲基甲酰胺中，得到混合溶液，混合溶液中竹笋壳纳米晶须的质量浓度为0.2-1.4％，并对混合溶液进行超声波处理；
步骤3、向上一步处理后的混合溶液中加入聚丙烯腈，得到纺丝液，纺丝液中聚丙烯腈的质量分数为10-20％，在50-70℃条件下对纺丝液磁力搅拌3-4h；
步骤4、利用上一步处理后得到的纺丝液，采用静电纺丝技术制备得到纳米纤维膜。
2.根据权利要求1所述的吸附印染废水的聚丙烯腈纳米纤维膜的制备方法，其特征在于，所述步骤2的混合溶液中竹笋壳纳米晶须的质量浓度为1.4％。
3.根据权利要求1所述的吸附印染废水的聚丙烯腈纳米纤维膜的制备方法，其特征在于，所述步骤3的纺丝液中聚丙烯腈的质量分数为15％。
4.吸附印染废水的聚丙烯腈纳米纤维膜，其特征在于，由上述权利要求1-3中任一种方法制备得到。
CN202110624297.9A 2021-06-04 2021-06-04 吸附印染废水的聚丙烯腈纳米纤维膜及其制备方法 Pending CN113398894A (zh)

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