CN113663655A - 一种高弹性pdms/cbc海绵吸附材料的制备方法 - Google Patents
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Abstract
本发明涉及一种高弹性PDMS/CBC海绵吸附材料的制备方法，利用超声法将CBC附着在PDMS海绵的表面，制得PDMS/CBC海绵，并用于对油水混合物中油的吸附回收。本发明以CBC为改性配体，高弹性PDMS海绵为支撑材料，制备复合改性材料的方法，用于提高油水混合物的吸附分离性能。由于CBC具有较高的比表面积，测试结果表明所获得的高弹性PDMS/CBC海绵有优越的油水分离性能，且有较高的可重复使用性。
Description
技术领域
本发明涉及材料制备和分离技术领域，尤其是一种能吸附分离油水混合物的高弹性PDMS/CBC海绵吸附材料的制备方法。
背景技术
近几十年来，随着石油工业、制造业等工业化的不断发展，水污染造成了严重的生态环境问题。石油泄漏和有机物泄漏已成为世界上重要的水污染源。目前常用的离心、浮选、重选等处理工艺，由于操作复杂、能耗高、二次污染、油水分离不彻底等原因，难以在实际生活中大规模应用。因此，迫切需要开发一种简单高效的油水混合物处理方法。
随着海绵、泡沫、气凝胶等3D多孔材料的出现，使得油水分离的认知领域更加广泛。3D多孔材料比2D网格材料有更多的优势，无需提前收集含油废水，大大节省了处理时间，而且3D多孔材料易于回收，重复使用率高。
聚二甲基硅氧烷(Polydimethylsiloxane，简称PDMS)是一种含有硅氧键和长烷基链的疏水性材料，该材料能耐高温、化学稳定性好、具有良好的弹性。用PDMS海绵作为吸油剂的基体是不二选择。碳化细菌纤维素(CarbonizedBacterial Cellulose，简称CBC)是将细菌纤维素在氮气保护下进行高温煅烧，变成碳材料，碳化后的细菌纤维素保留了细菌纤维素的延展性和柔韧性，又具备了碳材料的疏水性和良好的机械性能。因此，将这两种材料结合将会大大提高吸附材料的吸附性能。
发明内容
本发明要解决的技术问题是：为了克服现有技术中之不足，本发明提供一种高弹性PDMS/CBC海绵吸附材料的制备方法，利用超声法将CBC附着在PDMS海绵的表面，制得PDMS/CBC海绵，并用于对油水混合物中油的吸附回收。
本发明解决其技术问题所采用的技术方案是：一种高弹性PDMS/CBC海绵吸附材料的制备方法，具有以下步骤：
S1、将道康宁PDMS预聚体和固化剂按照10:1的比例进行混合，室温下充分搅拌混合1～3h；
S2、将一块方糖放入步骤S1中的混合溶液，完全浸入后放入真空烘箱中室温真空脱气处理，脱气时间为2～5h；
S3、将步骤S2中的方糖取出放入聚四氟乙烯模具中，再放入烘箱中固定温度进行固化处理2～8h；
S4、将步骤S3中固化后的方糖取出，用小刀将周围多余的PDMS切掉，然后将含有方糖的PDMS海绵浸泡在温度为70℃～90℃热水中，间隔2h换一次水，维持24h，然后将除去方糖的PDMS海绵放入温度为60℃～80℃的烘箱中烘干；
S5、将0.01～0.1g的CBC分散在50mL四氢呋喃溶液中，制得CBC分散液；
S6、将步骤S4中的海绵加入步骤S5中的CBC分散液，然后进行超声处理0.5～2h，取出海绵用蒸馏水清洗海绵表面的CBC，放入温度为60℃～80℃烘箱烘干；
S7、重复步骤S6次数1～10次。
本发明的有益效果是：本发明制备过程简单绿色，利用PDMS本身具有的弹性，使用了牺牲模板法制备了高弹性可重复使用的海绵，并采用浸涂法将CBC涂覆在PDMS海绵的表面，由于CBC具有较高的比表面积，从而有效地增加了海绵对有机溶剂和油的吸附能力。
附图说明
下面结合附图和实施例对本发明进一步说明。
图1是本发明中PDMS和PDMS/CBC的扫描电镜形貌图。
图2是本发明中PDMS和PDMS/CBC的傅里叶红外光谱图。
图3是本发明中PDMS/CBC的应力-应变曲线图。
具体实施方式
现在结合附图对本发明作进一步详细的说明。这些附图均为简化的示意图，仅以示意方式说明本发明的基本结构，因此其仅显示与本发明有关的构成。
实施例1：
将道康宁PDMS预聚体15g和固化剂1.5g按10：1的比例置于规格为25mL的烧杯中，在室温下充分搅拌混合1h；将方糖加入上述混合均匀的溶液中，放入真空烘箱中室温下真空脱气2h，然后将充满PDMS溶液的方糖取出，放入聚四氟乙烯模具中烘箱中60℃固化8h；将固化后的方糖取出，切除多余的PDMS，将完整的充满方糖的PDMS海绵放入70℃的热水中，进行糖模板溶解，每隔2h换次水，维持24h，然后将溶解后的PDMS海绵放入60℃的烘箱中进行烘干。
将0.01gCBC粉末分散在50mL的四氢呋喃溶液中，再将烘干后的PDMS海绵加入上述分散液中，超声处理0.5h；取出海绵用蒸馏水冲洗掉表面残留的CBC,60℃烘箱烘干，再将烘干后的PDMS/CBC海绵重复浸涂上述的CBC分散液，重复次数为3次。
实施例2:
将道康宁PDMS预聚体15g和固化剂1.5g按10：1的比例置于规格为25mL的烧杯中，室温下充分搅拌混合2h；将方糖加入上述混合均匀的溶液中，放入真空烘箱中室温下真空脱气3h，然后将充满PDMS溶液的方糖取出，放入聚四氟乙烯模具中烘箱中80℃固化4h；将固化后的方糖取出，切除多余的PDMS，将完整的充满方糖的PDMS海绵放入80℃的热水中，进行糖模板溶解，每隔2h换次水，维持24h；然后将溶解后的PDMS海绵放入80℃的烘箱中进行烘干。
将0.05gCBC粉末分散在50mL的四氢呋喃溶液中，再将烘干后的PDMS海绵加入上述分散液中，超声处理1h；取出海绵用蒸馏水冲洗掉表面残留的CBC,80℃烘箱烘干，再将烘干后的PDMS/CBC海绵重复浸涂上述的CBC分散液，重复次数为5次。
实施例3：
将道康宁PDMS预聚体15g和固化剂1.5g按10：1的比例置于规格为25mL的烧杯中，室温下充分搅拌混合3h；将方糖加入上述混合均匀的溶液中，放入真空烘箱中室温下真空脱气5h，然后将充满PDMS溶液的方糖取出，放入聚四氟乙烯模具中烘箱中120℃固化2h；将固化后的方糖取出，切除多余的PDMS，将完整的充满方糖的PDMS海绵放入90℃的热水中，进行糖模板溶解，每隔2h换次水，维持24h，然后将溶解后的PDMS海绵放入80℃的烘箱中进行烘干。
将0.1gCBC粉末分散在50mL的四氢呋喃溶液中，再将烘干后的PDMS海绵加入上述分散液中，超声处理2h，取出海绵用蒸馏水冲洗掉表面残留的CBC,80℃烘箱烘干，再将烘干后的PDMS/CBC海绵重复浸涂上述的CBC分散液，重复次数为8次。
如图1所示为PDMS和PDMS/CBC的扫描电镜形貌图。其中图1(a)和图1(b)是PDMS的形貌图，从图中可以看出，材料的表面相对比较光滑，且呈现不均匀的多孔的结构，这是方糖溶解后留下的孔道。图1(c)和图1(d)是PDMS/CBC的形貌图，从图中清晰的看出材料内部是由直径不同的大孔组成的蜂窝状大孔结构。在每个孔的表面都附着了CBC，表面十分的粗糙，这有利于增加材料的比表面积，提高材料的吸附能力，也证明了CBC成功地被附着在PDMS上。
如图2所示为PDMS和PDMS/CBC的红外光谱图。从图中可以看出，在1258cm-1和1010cm-1处出现了Si-O-Si键的特征峰，而Si-C键则在790cm-1出显现，这都是属于PDMS的特征峰。当添加CBC之后，可以看到PDMS/CBC中关于PDMS的几个特征峰都有所减弱，可能是由于增加的CBC的量多，负载在PDMS的表面，导致PDMS的特征峰的透过率有所减弱，但还依然存在。
如图3所示为PDMS/CBC的应力-应变曲线图。从图中可以看出，PDMS/CBC海绵在形变80％的压力下重复压缩了50次。而它在被重复压缩五十次时前后的曲线基本重合，说明了PDMS/CBC海绵具有良好的弹性，且没有形变，这也证明了PDMS/CBC海绵的可重复使用性。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (6)
1.一种高弹性PDMS/CBC海绵吸附材料的制备方法，其特征是：具有以下步骤：
S1、将道康宁PDMS预聚体和固化剂按照10:1的比例进行混合，室温下充分搅拌混合；
S2、将一块方糖放入步骤S1中的混合溶液，完全浸入后放入真空烘箱中室温真空脱气处理；
S3、将步骤S2中的方糖取出放入聚四氟乙烯模具中，再放入烘箱中固定温度进行固化处理；
S4、将步骤S3中固化后的方糖取出，用小刀将周围多余的PDMS切掉，然后将含有方糖的PDMS海绵浸泡在热水中，间隔2h换一次水，维持24h，然后将除去方糖的PDMS海绵放入烘箱中烘干；
S5、将适量的CBC分散在50mL四氢呋喃溶液中，制得CBC分散液；
S6、将步骤S4中的海绵加入步骤S5中的CBC分散液，然后进行超声处理，取出海绵用蒸馏水清洗海绵表面的CBC，烘箱烘干；
S7、重复步骤S6。
2.如权利要求1所述的高弹性PDMS/CBC海绵吸附材料的制备方法，其特征是：所述的步骤S1中的搅拌时间为1～3h。
3.如权利要求1所述的高弹性PDMS/CBC海绵吸附材料的制备方法，其特征是：所述的步骤S2中的脱气时间为2～5h。
4.如权利要求1所述的高弹性PDMS/CBC海绵吸附材料的制备方法，其特征是：所述的步骤S5中CBC的投加量为0.01～0.1g。
5.如权利要求1所述的高弹性PDMS/CBC海绵吸附材料的制备方法，其特征是：所述的步骤S6中的超声处理时间为0.5～2h。
6.如权利要求1所述的高弹性PDMS/CBC海绵吸附材料的制备方法，其特征是：所述的步骤S7中重复步骤S6的次数为1～10次。
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