自支撑NH2-MIL-125/聚噁二唑复合正渗透膜的制备及性能

doi:10.7503/cjcu20190697

摘要/Abstract

摘要：

合成了高强度亲水性含羧基聚噁二唑材料(POD-COOH)和含氨基金属有机框架材料(NH₂-MIL-125), 以NH₂-MIL-125为填料, 与POD-COOH基体材料进行溶液共混, 并通过溶液浇铸法制备系列新型自支撑复合正渗透膜, 研究NH₂-MIL-125的引入对复合正渗透膜结构和性能的影响. 研究结果表明, 所制备的系列复合正渗透膜均呈致密结构, 且随着NH₂-MIL-125含量的增加, 复合膜的表面亲水性增加、电负性增强, 并保持良好的机械性能. 以去离子水为进料液, 1.5 mol/L硫酸钠溶液为汲取液, 对上述自支撑复合膜进行正渗透性能测试, 发现由于消除了传统正渗透膜支撑层的内浓差极化现象, 该新型复合正渗透膜在分离过程中具有优异的正渗透性能.

关键词: 自支撑正渗透膜, 聚噁二唑, 内浓差极化

Abstract:

A high-strength hydrophilic carboxyl-containing polyoxadiazole material(POD-COOH) and an amino-containing metal organic frame material(NH₂-MIL-125) were synthesized first, then a series of novel self-standing composite forward osmosis membranes were prepared using NH₂-MIL-125 as filler and POD-COOH as matrix by solution blending and casting method. Further the effects of NH₂-MIL-125 introduction on the structure and performance of composite forward osmosis membranes were investigated. The results demonstrated that the prepared self-standing composite forward osmosis membranes had a dense homogeneous structure. The hydrophilicity and electronegativity of the membranes were improved with increasing NH₂-MIL-125 content. And the composite membranes maintained good mechanical properties. When the testing feed and draw solutions were pure water and 1.5 mol/L Na₂SO₄ solution respectively, the prepared self-standing composite membranes exhibited excellent forward osmosis performance, which is attributed to the elimination of internal concentration polarization existing in support layer of traditional forward osmosis membranes.

Key words: Self-standing forward osmosis membrane, Polyoxadiazole, Internal concentration polarization

中图分类号:

O631

TrendMD:

何男, 刘威, 杨霞, 王宪泽, 崔晓春, 吴敬慧, 耿直. 自支撑NH₂-MIL-125/聚噁二唑复合正渗透膜的制备及性能. 高等学校化学学报, 2020, 41(6): 1370.

HE Nan, LIU Wei, YANG Xia, WANG Xianze, CUI Xiaochun, WU Jinghui, GENG Zhi. Preparation and Performance of Self-standing NH₂-MIL-125/polyoxadiazole Composite Forward Osmosis Membranes ^†. Chem. J. Chinese Universities, 2020, 41(6): 1370.

图/表 13

Scheme 1 Synthetic route of POD

Scheme 2 Synthetic route of POD-COOH

Fig.1 1H NMR spectrum of POD

Fig.2 1H NMR spectrum of POD-COOH

Fig.3 FTIR spectra of POD(a), POD-COOH(b), 1%NH2-MIL-125/POD-COOH(c), 3%NH2-MIL-125/POD-COOH(d) and 5%NH2-MIL-125/POD-COOH(e) forward osmosis membranes

Fig.4 SEM images of POD(A), POD-COOH(B), 1%NH2-MIL-125/POD-COOH(C), 3%NH2-MIL-125/POD-COOH(D) and 5%NH2-MIL-125/POD-COOH(E) forward osmosis membranes

Table 1 Thickness, water contact angle, Zeta potential and tensile strength of the forward osmosis membranes

Membrane sample	Thicknesses/μm	Water contact angle/(°)	Zeta potential/mV	Tensile strength/MPa
POD	5.0	78.7	-6.2	62.5
POD-COOH	5.0	75.0	-32.1	70.1
1%NH₂-MIL-125/POD-COOH	5.0	73.1	-37.3	56.2
3%NH₂-MIL-125/POD-COOH	5.0	72.0	-41.5	51.3
5%NH₂-MIL-125/POD-COOH	5.0	71.0	-45.2	46.6

Fig.5 Water contact angles of the POD(a), POD-COOH(b), 1%NH2-MIL-125/POD-COOH(c), 3%NH2-MIL-125/POD-COOH(d) and 5%NH2-MIL-125/POD-COOH(e) forward osmosis membranes Insets: water contact angles of a—e.

Fig.6 Zeta potential of the NH2-MIL-125 nanoparticles(a) and POD(b), POD-COOH(c), 1%NH2-MIL-125/POD-COOH(d), 3%NH2-MIL-125/POD-COOH(e), 5%NH2-MIL-125/POD-COOH(f) forward osmosis membranes at different pH

Table 2 Effect of NH2-MIL-125 content on water flux and reverse salt flux of forward osmosis membranes

Membrane sample	J_w/(L·m^-2·h^-1)	J_s/(g·m^-2·h^-1)	J_s/J_w/(g·L^-1)
POD	12.2	22.8	1.87
POD-COOH	18.1	8.0	0.44
1%NH₂-MIL-125/POD-COOH	24.3	9.8	0.40
3%NH₂-MIL-125/POD-COOH	27.4	10.5	0.38
5%NH₂-MIL-125/POD-COOH	30.2	13.1	0.43
Commercial FO membrane(HTI-CTA)	9.4	4.7	0.50

Fig.7 Forward osmosis performance of the POD(a), POD-COOH(b), 1%NH2-MIL-125/POD-COOH(c), 3%NH2-MIL-125/POD-COOH(d) and 5%NH2-MIL-125/POD-COOH(e) forward osmosis membranes

Fig.8 Effects of Na2SO4 concentrations on Jw and Js of 3%NH2-MIL-125/POD-COOH compo-site forward osmosis membrane

Fig.9 Stability of 3%NH2-MIL-125/POD-COOH composite forward osmosis membrane

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自支撑NH₂-MIL-125/聚噁二唑复合正渗透膜的制备及性能

Preparation and Performance of Self-standing NH₂-MIL-125/polyoxadiazole Composite Forward Osmosis Membranes ^†

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