制备聚酰胺复合膜中界面聚合反应添加剂研究进展

doi:10.16085/j.issn.1000-6613.2021-2399

摘要/Abstract

摘要：

聚酰胺复合膜以其优良的稳定性及良好的分离选择性成为水处理和化工分离领域应用范围最广的分离材料之一。聚酰胺复合膜一般采用界面聚合法制备，由于界面聚合反应活性高、反应参数多，致使界面层结构难以控制，膜的渗透性或选择性不理想。因此，如何有效调控膜结构，实现膜的高渗透性或选择性是目前面临的重要挑战。近期诸多研究表明，在水相或有机相中引入添加剂可以改变油水界面张力进而调控单体界面扩散速率及界面分布，或通过改变反应机理影响聚合反应速率，最终实现对界面层结构和膜性能的调控。本文从添加剂种类、性质和调控作用等角度总结了近年来添加剂对复合膜结构及性能调控的研究进展，分析了现有研究存在的问题，并建议从微观层面探究界面过程的物理化学性质以及开发高时间分辨率原位表征方法等。

关键词: 界面聚合, 膜, 添加剂, 聚酰胺复合膜

Abstract:

Polyamide composite membrane has become one of the most widely-used materials in the field of water treatment and chemical engineering separation due to its excellent stability and separation selectivity. Generally, polyamide composite membrane is fabricated by interfacial polymerization. Due to the high reactivity and numerous reaction parameters of interfacial polymerization, the structure of interfacial layer is difficult to control, and the permeability or selectivity of membrane is not satisfactory. Thus, it is a great challenge to regulate the structure of the membrane and achieve a membrane with high permeability or separation performance. Recent research indicates that addition of additives into the organic phase or aqueous phase solution is to change the interfacial tension. In this case, the monomer diffusion rate and the distribution can therefore be modified. The mechanism of the polymerization might be changed as well and the reaction rate can be regulated. Consequently, the structure of the interfacial layer and the performance of the membrane can be regulated. This review summarizes the recent progress from the perspective of the type, function and effect of additives. On the basis of recent research progress, it is suggested to explore the physicochemical properties of interfacial process at microscale and develop high time-resolution in-situ characterization methods.

Key words: interfacial polymerization, membranes, additives, polyamide composite membrane

中图分类号:

TB33

张赛晖, 李校阳, 高慧, 王丽丽. 制备聚酰胺复合膜中界面聚合反应添加剂研究进展[J]. 化工进展, 2022, 41(9): 4884-4894.

ZHANG Saihui, LI Xiaoyang, GAO Hui, WANG Lili. Recent progress in additives in interfacial polymerization for the preparation of polyamide composite membrane[J]. Chemical Industry and Engineering Progress, 2022, 41(9): 4884-4894.

图/表 5

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添加剂种类	添加剂名称	作用机理以及对分离层的影响	油相/水相	膜性能	参考文献
共溶剂	甲醇、乙醇、乙二醇、木糖醇等	提高间苯二胺（MPD）单体的扩散速率	水相	水通量提高5~10倍	［19-20］
	二甲基亚砜（DMSO）	改变界面张力，提高反应速率	水相	水通量大幅度提高，脱盐率略有下降	［21-25］
	六亚甲基磷酰胺（HMPA）	提高MPD向有机相的扩散速率	水相	水通量为3.33L/(m²·h·bar)，NaCl截留率为98.27%	［26］
	丙酮、乙酸乙酯、N,N二甲基甲酰胺（DMF）等	减小MPD和均苯三甲酰氯（TMC）之间的溶解度差异和界面张力	油相	水通量显著提高	［27-31］
	甲酸乙酯	使两相之间形成一层混溶区，影响MPD到有机相的扩散	油相	水通量增加2.6倍	［32］
极性有机化合物	磷酸三苯酯（TPP）	与TMC形成配合物，增加TMC的亲水性，提高MPD在有机相中的溶解度	油相	水通量增加，没有明显的脱盐率损失	［33-34］
	1，3-丙烷磺内酯（PS）	通过氢键作用阻碍MPD的扩散	油相	水通量为3.13L/(m²·h·bar)，NaCl截留率为99.39%	［35］
	冠醚	促进MPD单体向有机相的扩散	水相	水通量提高了164%	［37］
	葡萄糖、蔗糖、棉子糖	通过氢键进入聚酰胺（PA）层	水相	水通量提高86%	［38］
	单宁酸（TA）	通过质子化反应和氢键阻止哌嗪（PIP）向有机界面扩散	水相	水通量增加了13.4%，Na₂SO₄和MgSO₄的截留率分别为97.0%和94.4%	［39］
	甘油	增加黏度，抑制PIP向反应界面的扩散	水相	水通量提高了51%，Na₂SO₄的截留率保持在99.4%以上	［40］
	多巴胺	氨基和邻苯二酚基团与TMC的酰氯基团发生反应	水相	水通量为3.4L/(m²·h·bar)，NaCl截留率为99.4%	［41］
	氨基酸	氨基酸中氨基及羟基基团与TMC发生反应，降低PA层的致密性	水相	水通量增大，脱盐率降低	［42］
	精氨酸	与MPD分子结成亲水性离子对，降低其扩散速率	水相	水通量从2.90L/(m²·h·bar)增至3.38 L/(m²·h·bar)，NaCl截留率从96.34%提高到98.36%	［43］
表面活性剂	十二烷基硫酸钠（SDS）	降低界面张力，提高MPD的扩散速率	水相	水通量为4.76L/(m²·h·bar)，NaCl截留率为93.6%	［45］
	十六烷基三甲基氯化铵（HTAC）	增加IP反应速率	水相	水通量为0.93L/(m²·h·bar)，NaCl截留率为95.1%	［46］
	Tritonx-100	吸收PIP，提高其扩散速率	油相	水通量为5.3L/(m²·h·bar)	［47］
	十六烷基三甲基溴化铵（CTAB）	促进 PIP 扩散到有机相中，形成更厚、更致密的薄膜	水相	水通量从0.83L/(m²·h·bar)增至2.09 L/(m²·h·bar)，脱盐率不变	［48］
无机盐	NaCl	改变界面张力，促进TMC水解	水相	水通量达21.5L/(m²·h·bar)，Na₂SO₄截留率为99.10%	［49］
	LiCl	与TMC的羰基络合，促进TMC的水解	水相	水通量显著提高	［51］
	CaCl₂	与TMC的羰基络合，促进TMC的水解	水相	水通量为(2.44±0.05)L/(m²·h·bar)，NaCl 截留率为97.9%±0.3%	［52］
	CuSO₄、NiSO₄、MgSO₄、 Al₂（SO₄）₃	金属离子与聚乙烯亚胺（PEI）发生络合，影响IP反应	水相	NaCl截留率在94%以上，MgSO₄截留率达到97%以上	［53］
	NaHCO_₃、NH₄HCO₃	消耗聚合反应产生的HCl并产生CO₂，加快反应速率，形成较疏松的PA表面	水相	NaHCO₃质量分数为1.5%，NH₄HCO₃质量分数为0.5%时，具有较好的水通量和脱盐率	［54-55］
	Na₃PO₄	消耗聚合反应产生的HCl，加快反应速率	水相	水通量约为4.83 L/(m²·h·bar)，MgSO₄截留率约为93.5%	［56］
亲水性大分子	PVA	降低水相单体的扩散速率	水相	形成Turing结构，水通量提高，脱盐率稳定	［16］
	PEG	提高PIP的扩散速率	水相	PEG分子量为200Da所制备的膜，水通量提高了41%	［59］
	PVP	降低PIP扩散速率，降低IP反应速率	水相	水通量约为14.1~23.8L/(m²·h·bar)，Na₂SO₄截留率大于98.4%	［60］
纳米材料	SiO₂	干扰IP聚合过程，降低PIP与TMC反应速率，导致交联度低及PA层缺陷	油相	水通量为(9.72±0.78)L/(m²·h·bar)，不同盐截留率分别为Na₂SO₄ 99.0%±0.6%、MgCl₂ 67.3%±1.3%、MgSO₄ 96.5%±2.6%、NaCl 42.6%±2.3%	［62］
	TiO₂	限制MPD的扩散	水相	水通量为2.94L/(m²·h·bar)，NaCl截留率为94.2%	［63］
	Cu-Al层状双氢氧化物	降低PIP的扩散速率	油相	水通量为7.01L/(m²·h·bar)，不同盐的截留率分别为Na₂SO₄ 96.8%、MgCl₂ 95.6%、MgSO₄95.4%、NaCl 60.8%	［64］
	纳米Ag	吸附MPD，导致交联度增加	水相	水通量增加了两倍	［65］
	沸石	促进MPD向界面的扩散	油相	水通量增加了一倍，NO₃^-截留率从63%提高到85%	［66］
	氧化石墨烯（GO）	降低PIP的扩散速率	水相	水通量达到8L/(m²·h·bar)，Na₂SO₄截留率为96.1%	［68］
	氮掺杂GO量子点（N-GOQD）	削弱MPD和TMC单体之间的反应，降低PA的交联度	水相	水通量提高了近3倍，脱盐率保持不变	［71］
	GO-羧酸型超支化聚合物（HBE-COOH）	降低PIP的扩散速率	水相	水通量为8L/(m²·h·bar)，脱盐率维持不变	［72］
	羧基化GO（CFGO）	阻碍PIP向TMC的扩散，影响聚合反应速率	水相	水通量为11.04L/(m²·h·bar)，NaCl截留率为25.0%	［73］
	多壁碳纳米管（MWNT）	吸附MPD，稳定聚合物网络，降低溶胀性	水相	脱盐率保持不变，提高膜的耐氯性	［74］
	UiO-66	增加TMC-正己烷溶液的黏度，阻碍了PIP扩散到有机相中，减慢IP速率，形成低交联度的PA层	油相	水通量达14.64L/(m²·h·bar)	［76］
	MIL-101（Cr）@GO	影响MPD与TMC反应，使IP反应不完全，降低PA的交联度	水相	水通量从1.02L/(m²·h·bar)增加到1.90L/(m²·h·bar)	［77］
	磺酸化氧化石墨烯（SGO）@ UiO-66	通过化学反应和氢键吸附MPD，减弱其与TMC聚合反应	油相	水通量提高了41%	［78］
	季铵化SiO₂@多金属氧酸盐（QNP@WPOM）	限制MPD的扩散	水相	水通量从2.19L/(m²·h·bar)增至5.07 L/(m²·h·bar)	［79］

添加剂种类	添加剂名称	作用机理以及对分离层的影响	油相/水相	膜性能	参考文献
共溶剂	甲醇、乙醇、乙二醇、木糖醇等	提高间苯二胺（MPD）单体的扩散速率	水相	水通量提高5~10倍	［19-20］
	二甲基亚砜（DMSO）	改变界面张力，提高反应速率	水相	水通量大幅度提高，脱盐率略有下降	［21-25］
	六亚甲基磷酰胺（HMPA）	提高MPD向有机相的扩散速率	水相	水通量为3.33L/(m²·h·bar)，NaCl截留率为98.27%	［26］
	丙酮、乙酸乙酯、N,N二甲基甲酰胺（DMF）等	减小MPD和均苯三甲酰氯（TMC）之间的溶解度差异和界面张力	油相	水通量显著提高	［27-31］
	甲酸乙酯	使两相之间形成一层混溶区，影响MPD到有机相的扩散	油相	水通量增加2.6倍	［32］
极性有机化合物	磷酸三苯酯（TPP）	与TMC形成配合物，增加TMC的亲水性，提高MPD在有机相中的溶解度	油相	水通量增加，没有明显的脱盐率损失	［33-34］
	1，3-丙烷磺内酯（PS）	通过氢键作用阻碍MPD的扩散	油相	水通量为3.13L/(m²·h·bar)，NaCl截留率为99.39%	［35］
	冠醚	促进MPD单体向有机相的扩散	水相	水通量提高了164%	［37］
	葡萄糖、蔗糖、棉子糖	通过氢键进入聚酰胺（PA）层	水相	水通量提高86%	［38］
	单宁酸（TA）	通过质子化反应和氢键阻止哌嗪（PIP）向有机界面扩散	水相	水通量增加了13.4%，Na₂SO₄和MgSO₄的截留率分别为97.0%和94.4%	［39］
	甘油	增加黏度，抑制PIP向反应界面的扩散	水相	水通量提高了51%，Na₂SO₄的截留率保持在99.4%以上	［40］
	多巴胺	氨基和邻苯二酚基团与TMC的酰氯基团发生反应	水相	水通量为3.4L/(m²·h·bar)，NaCl截留率为99.4%	［41］
	氨基酸	氨基酸中氨基及羟基基团与TMC发生反应，降低PA层的致密性	水相	水通量增大，脱盐率降低	［42］
	精氨酸	与MPD分子结成亲水性离子对，降低其扩散速率	水相	水通量从2.90L/(m²·h·bar)增至3.38 L/(m²·h·bar)，NaCl截留率从96.34%提高到98.36%	［43］
表面活性剂	十二烷基硫酸钠（SDS）	降低界面张力，提高MPD的扩散速率	水相	水通量为4.76L/(m²·h·bar)，NaCl截留率为93.6%	［45］
	十六烷基三甲基氯化铵（HTAC）	增加IP反应速率	水相	水通量为0.93L/(m²·h·bar)，NaCl截留率为95.1%	［46］
	Tritonx-100	吸收PIP，提高其扩散速率	油相	水通量为5.3L/(m²·h·bar)	［47］
	十六烷基三甲基溴化铵（CTAB）	促进 PIP 扩散到有机相中，形成更厚、更致密的薄膜	水相	水通量从0.83L/(m²·h·bar)增至2.09 L/(m²·h·bar)，脱盐率不变	［48］
无机盐	NaCl	改变界面张力，促进TMC水解	水相	水通量达21.5L/(m²·h·bar)，Na₂SO₄截留率为99.10%	［49］
	LiCl	与TMC的羰基络合，促进TMC的水解	水相	水通量显著提高	［51］
	CaCl₂	与TMC的羰基络合，促进TMC的水解	水相	水通量为(2.44±0.05)L/(m²·h·bar)，NaCl 截留率为97.9%±0.3%	［52］
	CuSO₄、NiSO₄、MgSO₄、 Al₂（SO₄）₃	金属离子与聚乙烯亚胺（PEI）发生络合，影响IP反应	水相	NaCl截留率在94%以上，MgSO₄截留率达到97%以上	［53］
	NaHCO_₃、NH₄HCO₃	消耗聚合反应产生的HCl并产生CO₂，加快反应速率，形成较疏松的PA表面	水相	NaHCO₃质量分数为1.5%，NH₄HCO₃质量分数为0.5%时，具有较好的水通量和脱盐率	［54-55］
	Na₃PO₄	消耗聚合反应产生的HCl，加快反应速率	水相	水通量约为4.83 L/(m²·h·bar)，MgSO₄截留率约为93.5%	［56］
亲水性大分子	PVA	降低水相单体的扩散速率	水相	形成Turing结构，水通量提高，脱盐率稳定	［16］
	PEG	提高PIP的扩散速率	水相	PEG分子量为200Da所制备的膜，水通量提高了41%	［59］
	PVP	降低PIP扩散速率，降低IP反应速率	水相	水通量约为14.1~23.8L/(m²·h·bar)，Na₂SO₄截留率大于98.4%	［60］
纳米材料	SiO₂	干扰IP聚合过程，降低PIP与TMC反应速率，导致交联度低及PA层缺陷	油相	水通量为(9.72±0.78)L/(m²·h·bar)，不同盐截留率分别为Na₂SO₄ 99.0%±0.6%、MgCl₂ 67.3%±1.3%、MgSO₄ 96.5%±2.6%、NaCl 42.6%±2.3%	［62］
	TiO₂	限制MPD的扩散	水相	水通量为2.94L/(m²·h·bar)，NaCl截留率为94.2%	［63］
	Cu-Al层状双氢氧化物	降低PIP的扩散速率	油相	水通量为7.01L/(m²·h·bar)，不同盐的截留率分别为Na₂SO₄ 96.8%、MgCl₂ 95.6%、MgSO₄95.4%、NaCl 60.8%	［64］
	纳米Ag	吸附MPD，导致交联度增加	水相	水通量增加了两倍	［65］
	沸石	促进MPD向界面的扩散	油相	水通量增加了一倍，NO₃^-截留率从63%提高到85%	［66］
	氧化石墨烯（GO）	降低PIP的扩散速率	水相	水通量达到8L/(m²·h·bar)，Na₂SO₄截留率为96.1%	［68］
	氮掺杂GO量子点（N-GOQD）	削弱MPD和TMC单体之间的反应，降低PA的交联度	水相	水通量提高了近3倍，脱盐率保持不变	［71］
	GO-羧酸型超支化聚合物（HBE-COOH）	降低PIP的扩散速率	水相	水通量为8L/(m²·h·bar)，脱盐率维持不变	［72］
	羧基化GO（CFGO）	阻碍PIP向TMC的扩散，影响聚合反应速率	水相	水通量为11.04L/(m²·h·bar)，NaCl截留率为25.0%	［73］
	多壁碳纳米管（MWNT）	吸附MPD，稳定聚合物网络，降低溶胀性	水相	脱盐率保持不变，提高膜的耐氯性	［74］
	UiO-66	增加TMC-正己烷溶液的黏度，阻碍了PIP扩散到有机相中，减慢IP速率，形成低交联度的PA层	油相	水通量达14.64L/(m²·h·bar)	［76］
	MIL-101（Cr）@GO	影响MPD与TMC反应，使IP反应不完全，降低PA的交联度	水相	水通量从1.02L/(m²·h·bar)增加到1.90L/(m²·h·bar)	［77］
	磺酸化氧化石墨烯（SGO）@ UiO-66	通过化学反应和氢键吸附MPD，减弱其与TMC聚合反应	油相	水通量提高了41%	［78］
	季铵化SiO₂@多金属氧酸盐（QNP@WPOM）	限制MPD的扩散	水相	水通量从2.19L/(m²·h·bar)增至5.07 L/(m²·h·bar)	［79］

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