CN111057267A - 磁性三聚氰胺疏水亲油海绵的制备方法 - Google Patents

磁性三聚氰胺疏水亲油海绵的制备方法 Download PDF

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CN111057267A
CN111057267A CN201911201894.XA CN201911201894A CN111057267A CN 111057267 A CN111057267 A CN 111057267A CN 201911201894 A CN201911201894 A CN 201911201894A CN 111057267 A CN111057267 A CN 111057267A
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sponge
melamine
magnetic
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姜炜
宋欣
郝嘎子
胡玉冰
肖磊
张光普
郭虎
柯香
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Nanjing University of Science and Technology
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Abstract

本发明公开了一种磁性三聚氰胺疏水亲油海绵的制备方法。所述方法将三聚氰胺海绵浸没在质量分数为0.5～1％的硅烷偶联剂的甲苯溶液中，浸没完全后，使溶剂挥发并干燥，在纳米Fe3O4的乙醇分散液中超声，干燥，得到磁性三聚氰胺疏水亲油海绵。本发明采用浸渍法制备硅烷偶联剂改性的三聚氰胺海绵，再通过超声法制备磁性三聚氰胺疏水亲油海绵，充分利用三聚氰胺海绵的多孔结构保证了吸附材料的良好性能，并结合超声技术，将磁性材料包覆在海绵体上，减弱纳米颗粒间的作用，增强颗粒与海绵体间的作用。本发明的磁性三聚氰胺疏水亲油海绵可通过磁力回收循环使用，多次循环后的海绵油吸附性能几乎保持不变。

Description

磁性三聚氰胺疏水亲油海绵的制备方法
技术领域
本发明属于疏水亲油的吸附材料的制备技术领域，涉及一种磁性三聚氰胺疏水亲油海绵的制备方法。
背景技术
海上石油资源的开发与探索，必然会带来石油泄漏的风险，直接性地造成对海洋的污染。因此，海洋石油污染治理成为必须重视的课题。目前，吸油材料在石油污染治理方面表现出了潜在的优势。
三聚氰胺海绵又称密胺海绵，是一种具有较高开孔率的新型泡沫塑料，它具有三维网络结构，具有很强的物理吸附能力，同时还具有较优异的吸声性、阻燃性、隔热性、热稳定性等良好性能。三聚氰胺海绵具有较高吸附性能，但并不具备疏水亲油性能，因此在用作油污吸附处理材料时，要对其进行疏水改性。Song等人(Song S,Yang H,Su C, etal.Ultrasonic-microwave assisted synthesis of stable reduced graphene oxidemodified melamine foam with superhydrophobicity and high oil adsorptioncapacities[J].Chemical Engineering Journal,2016,306:504-511.)，用超声波和微波协同辅助的方法制备了疏水的改性三聚氰胺海绵；Feng等人(Feng Y,Wang Y,Wang Y,etal.Furfuryl alcohol modified melamine sponge for high-efficient oil spillclean-up and recovery[J].J.Mater.Chem.A, 2017,5(41):21893-21897.)，在酸性条件下，用糖醇为改性剂在三聚氰胺海绵的表面进行聚合反应，制备了改性的疏水性三聚氰胺海绵。然而，处理油污需要综合考虑经济成本、制备效率等，在制备改性三聚氰胺海绵的过程中，应避免使用较为昂贵的药品、试剂和较为复杂的实验装置和实验设备，更应尽量缩短制备的步骤。
浸渍法是一种将固体浸泡在某种混合组分的化合物溶液中以使得混合组份中的活性物质以离子等形式吸附到固体表面的方法。浸渍法主要是利用表面张力的作用，使得相应的液体进入到空隙中，同时利用活性组分对载体表面的吸附能力，实现组合。浸渍法能够负载在载体表面，利用率高、用量较少，能有效地减少活性组分的使用量，属于一种较为简单、经济的方法。
发明内容
本发明的目的在于提供一种工艺简单、安全可靠、成本较低、稳定性较好且油吸附性能显著提高的磁性三聚氰胺疏水亲油海绵的制备方法。该方法在保持改性海绵油吸附性能的基础上，加入磁性材料，增加其磁性能，便于海绵材料的回收再利用。
实现本发明目的的技术解决方案如下：
磁性三聚氰胺疏水亲油海绵的制备方法，具体步骤如下：
将三聚氰胺海绵浸没在质量分数为0.5～1％的硅烷偶联剂的甲苯溶液中，浸没完全后，使溶剂挥发并干燥，在纳米Fe3O4的乙醇分散液中超声，干燥，得到磁性三聚氰胺疏水亲油海绵。
优选地，所述的硅烷偶联剂选自甲基三氯硅烷、丙基三氯硅烷或戊基三氯硅烷等。
优选地，所述的浸泡时间为30min～2h。
优选地，所述的纳米Fe3O4的平均粒径为200nm，其在乙醇分散液中的浓度为 5～10mg/mL。
优选地，所述的超声时间为10～30min。
与现有技术相比，本发明具有如下优点：
(1)本发明采用浸渍法制备硅烷偶联剂改性的三聚氰胺海绵，再通过超声法制备磁性三聚氰胺疏水亲油海绵，充分利用了三聚氰胺海绵的多孔结构保证了吸附材料的良好性能。
(2)通过浸渍法制备的硅烷偶联剂改性的三聚氰胺海绵，制备方法简单，耗时较少，制备的海绵疏水亲油性能良好。
(3)结合超声技术，将磁性材料包覆在海绵体上。超声波能够产生空化作用，有效防止因纳米颗粒的粒径小、表面能大而产生的团聚现象，以减弱纳米颗粒间的作用，增强颗粒与海绵体间的作用，磁性三聚氰胺疏水亲油海绵可通过磁力回收循环使用，多次循环后的海绵油吸附性能几乎保持不变。
附图说明
图1为实施例1中制得的磁性三聚氰胺疏水亲油海绵改性前后的SEM对比图；
图2为实施例1中制得的磁性三聚氰胺疏水亲油海绵改性前后的VSM对比图；
图3为实施例1中制得的磁性三聚氰胺疏水亲油海绵的水接触角图。
具体实施方式
下面结合实施例和附图对本发明作进一步详述。
实施例1
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例2
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的丙基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例3
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的甲基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例4
选用体积为2×2×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例5
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为1％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min 后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例6
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡2h 后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例7
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取300mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为10mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
实施例8
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声30min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
对比例1
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.2％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性200nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
对比例2
选用体积为1×1×2cm的三聚氰胺海绵，放置在烧杯底部。配置质量分数为0.5％的戊基三氯硅烷的甲苯溶液，倒入放置海绵的烧杯中，溶液需完全浸没海绵。浸泡30min后，挤出海绵中的改性溶液，并用甲苯反复清洗三次。将海绵放入通风橱中，待溶剂挥发完全后，放入120℃的烘箱中干燥1h。称取150mg的磁性20nmFe3O4纳米颗粒，超声分散在30mL的无水乙醇中，配置成浓度为5mg/mL的Fe3O4乙醇分散液。将改性的海绵浸没在分散液中，超声10min，取出放入60℃的烘箱中干燥2h，获得磁性三聚氰胺疏水亲油海绵。
对各实施例和对比例制得的磁性三聚氰胺疏水亲油海绵油吸附性能进行表征。
磁性三聚氰胺疏水亲油海绵进行油吸附性能测试，测试的具体过程如下：
步骤一：对磁性三聚氰胺疏水亲油海绵进行称重，质量记为m0。
步骤二：将足够量的食用油倒入表面皿中，把预称重的磁性三聚氰胺疏水亲油海绵加入其中，当吸附达到平衡以后，对吸附后的海绵进行称重，质量记为mx。
步骤三：根据公式：Q＝(mx-m0)/m0，计算三种海绵的吸附倍率Q。
各实施例和对比例中磁性三聚氰胺疏水亲油海绵的油吸附性能如表1所示。
表1各实施例和对比例中磁性三聚氰胺疏水亲油海绵的吸油性能
Figure RE-GDA0002392266510000051
Figure RE-GDA0002392266510000061
为了充分了解制得的磁性三聚氰胺疏水亲油海绵的性能，分别对其进行了SEM、FTIR等测试，并测试了其磁性能、油吸附性能等。
图1是空白三聚氰胺海绵、经由戊基三氯硅烷改性后的三聚氰胺疏水亲油海绵、磁性三聚氰胺疏水亲油海绵的SEM图，其中a、b为空白三聚氰胺海绵在不同放大倍率下的扫描电镜图，c、d为经由戊基三氯硅烷改性后的三聚氰胺疏水亲油海绵在不同放大倍率下的扫描电镜图，e、f为磁性三聚氰胺疏水亲油海绵在不同放大倍率下的扫描电镜图。由图e、f可以看出，制得的磁性三聚氰胺疏水亲油海绵的骨架上明显覆盖上了大量的颗粒物，说明在戊基三氯硅烷改性的基础上，海绵上又成功涂覆上了一层涂层。
对磁性三聚氰胺疏水亲油海绵进行了磁性能测试，测试的结果如图2所示，其中a为空白三聚氰胺海绵磁性能测试曲线图，b为磁性三聚氰胺疏水亲油海绵磁性能测试曲线图。由图中可以看出，空白三聚氰胺海绵是不具有磁性的，但磁性三聚氰胺海绵是具有较强磁性能的。
对磁性三聚氰胺疏水亲油海绵进行了水接触角测试，测试结果如图3所示，其水接触角为140°，由此可知其具有好的疏水性。

Claims (6)

1.磁性三聚氰胺疏水亲油海绵的制备方法，其特征在于，具体步骤如下：
将三聚氰胺海绵浸没在质量分数为0.5～1％的硅烷偶联剂的甲苯溶液中，浸没完全后，使溶剂挥发并干燥，在纳米Fe3O4的乙醇分散液中超声，干燥，得到磁性三聚氰胺疏水亲油海绵。
2.根据权利要求1所述的制备方法，其特征在于，所述的硅烷偶联剂选自甲基三氯硅烷、丙基三氯硅烷或戊基三氯硅烷。
3.根据权利要求1所述的制备方法，其特征在于，所述的浸泡时间为30min～2h。
4.根据权利要求1所述的制备方法，其特征在于，所述的纳米Fe3O4的平均粒径为200nm。
5.根据权利要求1所述的制备方法，其特征在于，所述的纳米Fe3O4在乙醇分散液中的浓度为5～10mg/mL。
6.根据权利要求1所述的制备方法，其特征在于，所述的超声时间为10～30min。
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