CN114749022B - 一种氮化硼/氧化石墨烯纳滤膜、制备方法及其应用 - Google Patents
一种氮化硼/氧化石墨烯纳滤膜、制备方法及其应用 Download PDFInfo
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Abstract
本发明涉及纳滤膜制备技术领域,具体涉及一种氮化硼/氧化石墨烯纳滤膜、制备方法及其应用,该方法将氨基功能化氮化硼纳米片负载于氧化石墨烯纳米片并组装成膜,协同利用氮化硼纳米片与氧化石墨烯纳米片的官能团相互作用增强复合膜的理化性质稳定,同时利用氮化硼纳米片的引入产生的丰富纳米孔道,从而实现高效的染料分离效果。该方法的特点是简单、易操作,无需对氧化石墨烯原材料进行复杂的化学处理,对于氧化石墨烯在膜领域的分离应用具有很好的指导意义。
Description
技术领域
本发明涉及纳滤膜制备技术领域,具体涉及一种氮化硼/氧化石墨烯纳滤膜、制备方法及其应用。
背景技术
化学试剂生产和生物制药过程中有机溶剂的回收成本占生产成本总额的40-70%。相较与传统的蒸馏、汽化、吸附、萃取和层析技术,膜分离技术在纯化和分离应用中更能满足企业对经济成本、环境保护和安全的需求。有机溶剂纳滤膜因其出色的稳定和分离性能是近年来最具有代表性的分离膜种类。然而,现有工作报道有机溶剂纳滤膜在膜分离应中很难兼具通量和截留性能,因此无法满足工业需求。
二维纳米片组装膜,如氧化石墨烯、硫属化合物、层状金属氧化物、金属有机框架化合物和金属碳氮化物已经被报道具有很好的分离应用研究价值。理论上,二维纳米材料的纳米片大小和厚度以及由纳米片组装形成的纳米孔道大小都会影响纳米膜的通量和选择性。氧化石墨烯纳米片组装膜因其较为成熟的制备技术和可控的成本优势,在分离应用中展现应用前景。但是,氧化石墨烯纳米片表面丰富的官能团极亲水,在水环境中很难维持其物理结构的完整性,因此严重限制其分离应用。另外,氧化石墨烯膜在有机体系中展现出的较低的通量特点很难满足工业应用。
鉴于上述缺陷,本发明创作者经过长时间的研究和实践终于获得了本发明。
发明内容
本发明的目的在于解决氧化石墨烯膜在分离应用中的稳定差,通量和选择性之间相互制约的问题,提供了一种氮化硼/氧化石墨烯纳滤膜、制备方法及其应用。
为了实现上述目的,本发明公开了一种氮化硼/氧化石墨烯纳滤膜的制备方法,包括以下步骤:
S1:制备氨基功能化氮化硼纳米片水分散液:将氮化硼与尿素混合,球磨,透析洗涤去除多余的尿素,得到氨基功能化氮化硼纳米片水分散液;
S2:制备氮化硼-氧化石墨烯复合膜:将步骤S1中得到的氨基功能化氮化硼纳米片与氧化石墨纳米片水溶液混合搅拌,将得到的混合液正压组装成氮化硼-氧化石墨烯复合膜;
S3:将步骤S2中正压制备得到的氮化硼-氧化石墨烯混合膜在氮气压力下静压。
所述步骤S1中氮化硼和尿素的质量比为1:10~1:50。
所述步骤S1中球磨的转速为200~600rpm。
所述步骤S1中透析洗涤时间为14天。
所述步骤S2中氨基功能化氮化硼纳米和氧化石墨纳米片的质量比为1:2或1:1或2:1。
所述氮化硼-氧化石墨复合膜为平面式。
所述步骤S3中氮气压力为0.1~1bar。
本发明还公开了一种采用上述制备方法制得的氮化硼/氧化石墨烯纳滤膜以及这种氮化硼/氧化石墨烯纳滤膜在水系或有机系染料分离中的应用,所述水洗体系中测试的染料为伊红Y、孟加拉玫瑰红、亚甲基蓝、罗丹明6G、灿烂黄或伊文思蓝,所述有机体系为甲醇、乙醇或异丙醇,所述有机体系中测试的染料为伊文思蓝、酸性品红、固绿、刚果红或亮蓝。
本发明中制备的氮化硼/氧化石墨烯纳滤膜利用纳米片组装过程中产生的大量丰富的纳米孔道,基于纳米孔道对溶质荷溶剂分子的筛选分离原理,有效过滤溶剂分子和截留染料分子,实现了对污水、废有机溶液的有效净化。
与现有技术比较本发明的有益效果在于:本发明提供了一种简单、易操作的提升氧化石墨烯膜稳定性和分离性能的方法。该方法利用氮化硼纳米片与氧化石墨烯纳米片丰富官能团相互作用特点,充分发挥氮化硼纳米片引入产生的丰富水通道优势,从而有效提升氧化石墨烯膜的稳定性和分离性能。对于氧化石墨烯膜在水系和有机体系中的分离应用具有很好的指导意义。
附图说明
图1为本发明的氮化硼纳米片负载于氧化石墨烯表面的透射电镜图;
图2为本发明的氮化硼纳米片与氧化石墨烯纳米片混合的扫描电子显微镜图;
图3为氮化硼/氧化石墨烯的X射线光电子能谱;
图4为本发明的氮化硼/氧化石墨烯的X射线衍射图;
图5为本发明的氮化硼和氧化石墨烯混合紫外可见、拉曼和红外图;
图6为本发明的氮化硼/氧化石墨烯纳滤膜与氧化石墨烯纳滤膜通量对比;
图7为本发明的氮化硼/氧化石墨烯纳滤膜对水、甲醇、乙醇和异丙醇溶液中染料分子的分离性能。
具体实施方式
以下结合附图,对本发明上述的和另外的技术特征和优点作更详细的说明。
实施例1
(1)制备氨基功能化氮化硼纳米片水分散液
将0.5g商业氮化硼与10g尿素混合,用行星式高能球磨机球磨在400rpm下研磨20h,透析14天洗涤去除多余的尿素,得到乳白色的氨基功能化氮化硼纳米片水分散液。
(2)制备氮化硼-氧化石墨烯复合膜
控制混合溶液纳米片总质量,本例中控制纳米膜的面密度为69mg/m2,将氨基功能化的氮化硼纳米片与氧化石墨纳米片水溶液按1:2质量比混合搅拌。将混合好的氮化硼-氧化石墨烯混合液在陶瓷或有机基底上用正压装置上组装成氮化硼-氧化石墨复合膜。
(3)将正压制备的氮化硼-氧化石墨烯混合膜在氮气1bar压力下静压。
(4)测试氮化硼-氧化石墨烯复合膜在水系或有机系中染料分离性能
选择伊红Y,孟加拉玫瑰红,亚甲基蓝,罗丹明6G,灿烂黄,伊文思蓝作为探针染料分子,配置100mL不同浓度染料水分散溶液,测试过程中分别收集40mL滤液,用紫外可见分光光度计分别测试原液浓度、滤液浓度和保留液的吸光度强度。附图1可说明本实施例的氮化硼均匀分散于氧化石墨烯表面,为纳米复合膜的稳定制备提供了源材料保障,也为稳定高效的分离应用提供了纳滤膜保障。
实施例2
(1)制备氨基功能化氮化硼纳米片水分散液
将0.5g商业氮化硼与20g尿素混合,用行星式高能球磨机球磨在500rpm下研磨50h,透析14天洗涤去除多余的尿素,得到乳白色的氨基功能化氮化硼纳米片水分散液。
(2)制备氮化硼-氧化石墨烯复合膜
控制混合溶液纳米片总质量,本例中控制纳米膜的面密度为83mg/m2,将氨基功能化的氮化硼纳米片与氧化石墨纳米片水溶液按1:1质量比混合搅拌。将混合好的氮化硼-氧化石墨烯混合液在陶瓷或有机基底上用正压装置上组装成氮化硼-氧化石墨复合膜。
(3)将正压制备的氮化硼-氧化石墨烯混合膜在氮气1bar压力下静压。
(4)测试氮化硼-氧化石墨烯复合膜在水系或有机系中染料分离性能
选择伊红Y,孟加拉玫瑰红,亚甲基蓝,罗丹明6G,灿烂黄,伊文思蓝作为探针染料分子,配置100mL不同浓度染料水分散溶液,测试过程中分别收集40mL滤液,用紫外可见分光光度计分别测试原液浓度、滤液浓度和保留液的吸光度强度。附图2、图3可说明本实施例的氮化硼与氧化石墨纳米片在纳滤膜内混合均匀,为纳米复合膜的稳定制备提供了源材料保障,也为稳定高效的分离应用提供了纳滤膜保障。
实施例3
(1)制备氨基功能化氮化硼纳米片水分散液
将0.5g商业氮化硼与10g尿素混合,用行星式高能球磨机球磨在600rpm下研磨20h,透析14天洗涤去除多余的尿素,得到乳白色的氨基功能化氮化硼纳米片水分散液。
(2)制备氮化硼-氧化石墨烯复合膜
控制混合溶液纳米片总质量,本例中控制纳米膜的面密度为69mg/m2,将氨基功能化的氮化硼纳米片与氧化石墨纳米片水溶液按2:1质量比混合搅拌。将混合好的氮化硼-氧化石墨烯混合液在陶瓷或有机基底上用正压装置上组装成氮化硼-氧化石墨复合膜。
(3)将正压制备的氮化硼-氧化石墨烯混合膜在氮气1bar压力下静压。
(4)测试氮化硼-氧化石墨烯复合膜在水系或有机系中染料分离性能
选择伊文思蓝和酸性品红作为探针染料分子,配置100mL不同浓度染料甲醇溶液,测试过程中分别收集40mL滤液,用紫外可见分光光度计分别测试原液浓度、滤液浓度和保留液的吸光度强度。附图4可说明本实施例的氮化硼均匀分散于氧化石墨烯表面产生的纳米孔道为稳定高效的分离应用提供了纳滤膜保障。
实施例4
(1)制备氨基功能化氮化硼纳米片水分散液
将0.5g商业氮化硼与20g尿素混合,用行星式高能球磨机球磨在400rpm下研磨20h,透析14天洗涤去除多余的尿素,得到乳白色的氨基功能化氮化硼纳米片水分散液。
(2)制备氮化硼-氧化石墨烯复合膜
控制混合溶液纳米片总质量,本例中控制纳米膜的面密度为69mg/m2,将氨基功能化的氮化硼纳米片与氧化石墨纳米片水溶液按1:2质量比混合搅拌。将混合好的氮化硼-氧化石墨烯混合液在陶瓷或有机基底上用正压装置上组装成氮化硼-氧化石墨复合膜。
(3)将正压制备的氮化硼-氧化石墨烯混合膜在氮气1bar压力下静压。
(4)测试氮化硼-氧化石墨烯复合膜在水系或有机系中染料分离性能
选择酸性品红和固绿作为探针染料分子,配置100mL不同浓度染料乙醇溶液,测试过程中分别收集40mL滤液,用紫外可见分光光度计分别测试原液浓度、滤液浓度和保留液的吸光度强度。附图5、图7可说明本实施例的氮化硼均匀分散于氧化石墨烯表面,为纳米复合膜的稳定制备提供了源材料保障,也为稳定高效的水系分离应用提供了纳滤膜保障。
实施例5
(1)制备氨基功能化氮化硼纳米片水分散液
将0.5g商业氮化硼与20g尿素混合,用行星式高能球磨机球磨在400rpm下研磨20h,透析14天洗涤去除多余的尿素,得到乳白色的氨基功能化氮化硼纳米片水分散液。
(2)制备氮化硼-氧化石墨烯复合膜
控制混合溶液纳米片总质量,本例中控制纳米膜的面密度为69mg/m2,将氨基功能化的氮化硼纳米片与氧化石墨纳米片水溶液按1:2质量比混合搅拌。将混合好的氮化硼-氧化石墨烯混合液在陶瓷或有机基底上用正压装置上组装成氮化硼-氧化石墨复合膜。
(3)将正压制备的氮化硼-氧化石墨烯混合膜在氮气1bar压力下静压。
(4)测试氮化硼-氧化石墨烯复合膜在水系或有机系中染料分离性能
选择亮蓝作为探针染料分子,配置100mL不同浓度染料异丙醇溶液,测试过程中分别收集40mL滤液,用紫外可见分光光度计分别测试原液浓度、滤液浓度和保留液的吸光度强度。附图6、图7可说明本实施例的氮化硼均匀分散于氧化石墨烯表面,为纳米复合膜的稳定制备提供了源材料保障,也为稳定高效的有机分离应用提供了纳滤膜保障。
以上所述仅为本发明的较佳实施例,对本发明而言仅仅是说明性的,而非限制性的。本专业技术人员理解,在本发明权利要求所限定的精神和范围内可对其进行许多改变,修改,甚至等效,但都将落入本发明的保护范围内。
Claims (7)
1.一种氮化硼/氧化石墨烯纳滤膜的制备方法,其特征在于,包括以下步骤:
S1:制备氨基功能化氮化硼纳米片水分散液:将氮化硼与尿素混合,球磨,透析洗涤去除多余的尿素,得到氨基功能化氮化硼纳米片水分散液;
S2:制备氮化硼-氧化石墨烯复合膜:将步骤S1中得到的氨基功能化氮化硼纳米片与氧化石墨纳米片水溶液混合搅拌,将得到的混合液正压组装成氮化硼-氧化石墨烯复合膜;
S3:将步骤S2中正压制备得到的氮化硼-氧化石墨烯混合膜在氮气压力下静压;
所述步骤S1中氮化硼和尿素的质量比为1:20或1:40;
所述步骤S1中球磨的转速为200~600rpm;
所述步骤S2中氨基功能化氮化硼纳米和氧化石墨纳米片的质量比为1:2或1:1或2:1。
2.如权利要求1所述的一种氮化硼/氧化石墨烯纳滤膜的制备方法,其特征在于,所述步骤S1中透析洗涤时间为14天。
3.如权利要求1所述的一种氮化硼/氧化石墨烯纳滤膜的制备方法,其特征在于,所述步骤S3中氮气压力为0.1~1bar。
4.一种采用如权利要求1~3任一项所述的制备方法制得的氮化硼/氧化石墨烯纳滤膜。
5.一种如权利要求4所述的氮化硼/氧化石墨烯纳滤膜在水系或有机系染料分离中的应用。
6.如权利要求5所述的一种氮化硼/氧化石墨烯纳滤膜在水系或有机系染料分离中的应用,所述水系中测试的染料为伊红Y、孟加拉玫瑰红、亚甲基蓝、罗丹明6G、灿烂黄或伊文思蓝。
7.如权利要求5所述的一种氮化硼/氧化石墨烯纳滤膜在水系或有机系染料分离中的应用,所述有机系为甲醇、乙醇或异丙醇,所述有机系中测试的染料为伊文思蓝、酸性品红、固绿、刚果红或亮蓝。
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