CN114452960A - 一种光驱动吸油的MXene改性三聚氰胺海绵及其制备方法 - Google Patents
一种光驱动吸油的MXene改性三聚氰胺海绵及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种光驱动吸油的MXene改性三聚氰胺海绵及其制备方法，首先将三聚氰胺海绵浸泡在由MXene、聚二甲基硅氧烷与有机溶剂组成的混合溶液中，然后将海绵‑改性液混合物转移至水热反应釜中于140‑150℃下水热反应2‑3h，冷却至室温后取出海绵并将其置于60‑70℃保温固化2‑4h即可。本发明采用浸泡+水热处理+热固化的方式完成了海绵的改性，其中水热处理有利于MXene更好的分散并紧密负载在海绵上，后期的热固化确保了MXene在使用过程中不易从海绵上脱落，经此处理后的海绵重复使用性能大幅度提升，有助于降低油水分离成本。此外本发明还具有制备工艺简单、生产使用成本较低、产品性能优异、可反复使用等优点，在原油泄露应急处理方面有较好的应用前景。
Description
技术领域
本发明涉及三聚氰胺海绵材料及水处理技术领域，具体涉及一种光驱动吸油的MXene改性三聚氰胺海绵及其制备方法。
背景技术
环境污染特别是水污染，是当前人类社会急需解决的问题之一。在海上进行石油生产、储存与运输过程中，由于意外事故、不正常操作等原因，不可避免会出现原油溢出、排放与泄露等问题。例如海洋油田开发过程中的井喷事故、输油管线的泄漏事故、油轮的泄漏事故等，这些泄露的烃类原油将对海洋环境造成极大的危害。一旦出现溢油事故一方面要尽可能缩小污染区域，另一方面要迅速消除和回收海面上的浮油。原油的粘度较大且通常漂浮在海面上，目前常见的回收材料普遍存在生产成本较高、技术路线较为复杂、吸附时间较长等问题。
三聚氰胺海绵是一种超轻、多孔、具有良好压缩恢复性能的泡沫材料，可多次重复使用并且价格低廉，被广泛应用于隔热保温、交通运输、航天航空等领域。通过对三聚氰胺海绵进行表面改性或低表面能修饰使其疏水亲油，又能用作油水分离吸附材料。中国发明专利CN106698583A报道了一种超疏水三聚氰胺海绵吸附型油水分离材料的制备方法，该方案以三聚氰胺海绵为基底，在聚吡咯表面原位还原银纳米粒子，最后进行氟化处理使产物具有油水分离功能。中国发明专利CN107501601 A公开了一种超疏水的三聚氰胺复合海绵材料，首先将乙烯基三乙氧基硅烷微球负载在三聚氰胺海绵表面，再通过3-(异丁烯酰氧)丙基三甲氧基硅烷与二乙烯苯在其表面的聚合反应，得到超疏水的三聚氰胺海绵复合材料。分析可知，上述这些工艺过程均较为繁琐复杂。中国发明专利CN111057267A报道了一种磁性三聚氰胺疏水亲油海绵的制备方法，将三聚氰胺海绵浸没在硅烷偶联剂的甲苯溶液中，进而在纳米氧化铁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。然而负载在海绵上的纳米粒子容易脱落，减弱了海绵的重复利用性能。中国发明专利CN107159129A公开了一种PDMS构筑超疏水三聚氰胺海绵碳材料，将三聚氰胺海绵浸于PDMS溶液中，取出烘干后再置于管式炉中在惰性气体保护下高温碳化，得到PDMS构筑超疏水三聚氰胺海绵碳材料。该方案在惰性气体保护下对材料进行了高温处理，不仅能耗高而且碳化会使得海绵材料的体积收缩失去部分弹性，必然导致吸油能力和反复使用性能的降低。
发明内容
本发明的目的之一在于提供一种光驱动吸油的MXene改性三聚氰胺海绵的制备方法，该方法包括以下步骤：首先将MXene、硅烷、有机溶剂混合得到改性液，接着将三聚氰胺海绵浸泡在改性液中，然后将海绵-改性液混合物转移至水热反应釜中进行水热反应，最后取出干燥。
进一步的，所述MXene的层数不超过5层，且横向尺寸不超过5μm；所述硅烷具体为聚二甲基硅氧烷，所述有机溶剂选自乙酸乙酯、乙酸丁酯中的至少一种。
进一步的，改性液中MXene的浓度为0.5-4g/L，硅烷的浓度为0.5-10g/L。
进一步的，三聚氰胺海绵在改性液中的浸泡温度为常温，浸泡时间为2-4h。
进一步的，水热反应温度为140-150℃，水热反应时间为2-3h。高温高压条件下进行的水热反应有助于MXene片层更好、更紧密的分散在三聚氰胺海绵内，进而实现更好的改性效果。
进一步的，水热反应完将三聚氰胺海绵冷却至室温，取出后置于60-70℃的环境中充分热固化。
本发明的第二重目的在于提供一种光驱动吸油的MXene改性三聚氰胺海绵。
本发明的第三重目的在于利用上述MXene改性的三聚氰胺海绵吸附分离溶液中的原油。
三聚氰胺海绵的多孔网络结构有利于吸附液体，聚二甲基硅氧烷使海绵具有疏水吸油性能，MXene的光热转换能力使得三聚氰胺海绵具有光热转换性能。改性后的三聚氰胺海绵在太阳光照射下温度会升高，从而促进了液面上的原油流动，最终提升了海绵的吸油能力。与常规浸泡改性方式相比，本发明制备工艺中的水热处理有利于MXene更好的分散并紧密负载在海绵上，后期的热固化确保了MXene在使用过程中不易从海绵上脱落，经此处理后的海绵重复使用性能大幅度提升，有助于降低油水分离成本。总之本发明具有制备工艺简单、生产使用成本较低、产品性能优异且可反复再生使用等优点，在原油泄露应急处理方面有较好的应用前景。
具体实施方式
为使本领域普通技术人员充分理解本发明的技术方案和有益效果，以下结合具体实施例进行进一步说明。
本发明所使用的原料均为普通市售，各实施例中的MXene为同一批次产品，分析表明其具有5层结构，横向尺寸不超过5微米。
实施例1
1)将0.05g MXene、0.1g聚二甲基硅氧烷、60mL乙酸乙酯混合均匀得到溶液A，将三聚氰胺海绵置于溶液A中浸泡3h；
2)将步骤1)中的海绵-溶液A混合物转移至水热反应釜中，加热至150℃保温反应2h，冷却至室温后取出海绵；
3)将步骤2)得到的三聚氰胺海绵置于烘箱中，在60℃下保温固化3h，得到MXene改性的三聚氰胺海绵。
实施例2
1)先将0.1g MXene、0.2g聚二甲基硅氧烷、80mL乙酸丁酯混合均匀得到溶液A，再将三聚氰胺海绵置于溶液A中浸泡2h；
2)将步骤1)中的海绵-溶液A混合物转移至水热反应釜中，加热至140℃保温反应3h，冷却至室温后取出；
3)将步骤2)得到的三聚氰胺海绵置于烘箱中，在65℃下保温固化3h，得到MXene改性三聚氰胺海绵。
实施例3
1)先将0.05g MXene、0.3g聚二甲基硅氧烷、80mL乙酸乙酯混合均匀得到溶液A，再将三聚氰胺海绵置于溶液A中浸泡4h；
2)将步骤1)中的海绵-溶液A混合物转移至水热反应釜中，加热至150℃保温反应2h，冷却至室温后取出；
3)将步骤2)得到的三聚氰胺海绵置于烘箱中，在60℃下保温固化4h，得到MXene改性三聚氰胺海绵。
实施例4
1)先将0.2g MXene、0.5g聚二甲基硅氧烷、100mL乙酸乙酯混合均匀得到溶液A，再将三聚氰胺海绵置于溶液A中浸泡3h；
2)将步骤1)中的海绵-溶液A混合物转移至水热反应釜中，加热至145℃保温反应2h，冷却至室温后取出；
3)将步骤2)得到的三聚氰胺海绵置于烘箱中，在60℃下保温固化3h，得到MXene改性三聚氰胺海绵。
对比例1
1)先将0.05g MXene、0.1g聚二甲基硅氧烷、60mL乙酸乙酯混合均匀得到溶液A，再将三聚氰胺海绵置于溶液A中浸泡3h；
2)将步骤1)得到的三聚氰胺海绵置于烘箱中，在60℃下保温固化3h，得到MXene改性三聚氰胺海绵。
为充分了解本发明各实施例及对比例制得的MXene改性三聚氰胺海绵的吸附及再生性能，在常温下进行了以下实验：首先配制浓度为50g/L的原油/水混合液，接着将其分成重量相同的若干组；将预先称量好的MXene改性三聚氰胺海绵(干重)浸没在原油/水混合液中，待其吸附平衡后计算单位质量海绵吸附原油的能力。按照上述方法，在浸泡的同时对海绵施加太阳光灯辐射照射15分钟后，计算单位质量海绵吸附原油的能力。用镊子挤出吸附饱和海绵中的原油进行再生，再生后的海绵按照上述方法继续进行测试，记录再生10次后的吸附情况。
表1不同MXene改性三聚氰胺海绵的吸附及再生性能对比表
表1为各实施例及对比例制得的MXene改性三聚氰胺海绵的吸附及再生性能对比表。从表1可以看出，由于原油较为粘稠，在没有太阳光照射时，所有海绵的吸附能力都较差；但是有太阳光照射时，由于MXene良好的光热转换能力，大幅提高了海绵的吸附能力。经过水热处理后的改性海绵吸附能力更大，这说明水热处理提高了改性海绵的吸附能力。与此同时，MXene改性三聚氰胺海绵具有良好的再生吸附能力，更有利于其实际应用。
Claims (9)
1.一种光驱动吸油的MXene改性三聚氰胺海绵的制备方法，其特征在于该方法包括以下步骤：首先将MXene、硅烷、有机溶剂混合得到改性液，接着将三聚氰胺海绵浸泡在改性液中，然后将海绵-改性液混合物转移至水热反应釜中进行水热反应，最后取出干燥。
2.如权利要求1所述的方法，其特征在于：所述MXene的层数不超过5层，且横向尺寸不超过5μm。
3.如权利要求1所述的方法，其特征在于：所述硅烷具体为聚二甲基硅氧烷，所述有机溶剂选自乙酸乙酯、乙酸丁酯中的至少一种。
4.如权利要求1所述的方法，其特征在于：改性液中MXene的浓度为0.5-4g/L，硅烷的浓度为0.5-10g/L。
5.如权利要求1所述的方法，其特征在于：三聚氰胺海绵在改性液中的浸泡温度为常温，浸泡时间为2-4h。
6.如权利要求1所述的方法，其特征在于：水热反应温度为140-150℃，水热反应时间为2-3h。
7.如权利要求1所述的方法，其特征在于：水热反应完将三聚氰胺海绵冷却至室温，取出后置于60-70℃的环境中充分热固化。
8.一种光驱动吸油的MXene改性三聚氰胺海绵，其特征在于：该海绵按照权利要求1-7中的任意一种方法制备得到。
9.权利要求8所述MXene改性三聚氰胺海绵在油水分离方面的应用。
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