浸渍-界面聚合法制备荷电镶嵌膜

以聚醚砜为基膜,以荷正电的高分子材料聚环氧氯丙烷胺及荷负电的2,5-二胺基苯磺酸混合水溶液(无机相)与三酰氯的正己烷溶液(有机相)通过浸渍-界面聚合反应,合成了一种新型的荷电镶嵌膜.实验考察了荷电剂浓度、单体的浓度、界面聚合反应时间和热处理温度等因素对膜性能的影响.研究结果表明,优化工艺下所制备的荷电镶嵌膜具有良好的性能.在0.4 MPa下,膜对无机盐的截留率均低于40%,对PEG1000的截留率则达到了94.02%,该膜的纯水通量为11.1 L·m-2·h-1;能截留低分子量有机物而透过盐,表明该膜可以用于有机物与盐混合溶液的分离.     

聚哌嗪酰胺复合纳滤膜制备及其性能表征

以聚砜超滤膜为基膜,采用界面聚合方法制备了聚哌嗪酰胺复合纳滤膜,并对其膜性能进行了表征。实验重点考察了基膜性质、聚合单体浓度、聚合反应时间、表面活性剂浓度、酸受体添加量等因素对纳滤膜性能的影响,确定了纳滤膜制备过程的界面聚合优化条件,即:水相单体(哌嗪)浓度0.08~0.12molL-1;有机相单体(间苯二甲酰氯和均苯三甲酰氯混合物)浓度0.08~0.1molL-1;聚合反应时间3~5min。在0.4MPa、25℃条件下,实验测得复合纳滤膜的水通量为4.12Lm-2h-1bar-1,膜对浓度为0.01molL-1的NaCl的截留率为30%~40%,对浓度为0.005molL-1的Na2SO4的截留率为80%~90%;对分子量不低于300gmol-1的有机物的截留率高于95%。该膜的分离性能接近于商业纳滤膜,其分离机理主要表现为“筛分机理以及膜与电解质之间的荷电作用。     

基于树状分子聚酰胺-胺(PAMAM)的复合纳滤膜制备及性能研究

以聚砜超滤膜为支撑膜,通过聚酰胺-胺(PAMAM,G0)与均苯三甲酰氯(TMC)的界面聚合反应制备复合纳滤膜。首先优化了界面聚合过程,并通过场发射扫描电子显微镜(FESEM)进行了膜的表面形貌分析,最后考察了纳滤膜对Na2SO4、不同分子量聚乙二醇及小分子有机物的分离性能。结果表明:较优的纳滤膜制备条件为:PAMAM浓度0.25%(wt),TMC浓度0.3%(wt),界面聚合时间90 s,热处理温度60℃。FESEM分析表明经界面聚合反应后,超滤膜表面形成了一层致密的活性层。随着操作压力的增加及Na2SO4浓度的降低,膜对盐的截留率均不断增大。复合纳滤膜可有效截留盐,且其截留分子量(MWCO)处于600~1000 g mol 1。     

聚偏氟乙烯-聚酰胺管式复合膜的分离性能研究

以聚偏氟乙烯(PVDF)管式超滤膜为基膜,无水哌嗪(PIP)为水相单体,均苯三甲基酰氯(TMC)为有机相单体,采用界面聚合法制备了不同截留性能的PVDF/聚酰胺(PA)管式复合膜.研究了不同性能管式复合膜的截留分子量、膜表面荷电性测试、对无机盐的截留性能,以及染料废水脱盐的应用.实验结果表明,截留率R(MgSO4)由9...     

界面聚合制备复合荷电镶嵌膜

以聚醚砜中空纤维膜为支撑膜,通过界面聚合方法制备了能有效传递电解质而截留低分子量有机物的复合荷电镶嵌膜。水相单体溶液含有2,5-二胺基苯磺酸、聚乙烯亚胺;有机相单体溶液含有均苯三甲酰氯和4-氯甲基苯酰氯;通过三甲胺溶液化学修饰将界面聚合复合层中的氯甲基基团转换为阳离子季胺盐基团。讨论了界面聚合条件和操作条件对荷电镶嵌膜分离性能的影响,分别采用原子力显微镜(AFM)、扫描电镜(SEM)及压汞仪等现代分析手段,对荷电镶嵌膜断面结构、表面形貌及孔径尺寸进行了系列表征。研究结果表明：界面聚合时间越长,生成的复合选择层越厚,所得膜的水通量越小,膜对无机盐的截留率也就越高;而界面聚合单体浓度增加,膜的水通量及膜对无机盐的截留率都会减小;另外,操作压力增大,膜的水通量及膜对无机盐的截留率均会增加。在操作压力为0．2MPa条件下,复合荷电镶嵌膜对无机盐的截留率均小于20％,而对二价酚橙和甲基绿的截留率均大于95％。     

聚环氧氯丙烷胺的合成及其在荷电镶嵌膜中的应用

以环氧氯丙烷、二甲胺、乙二胺为原料制备荷正电的高分子材料聚环氧氯丙烷胺.红外光谱分析表明聚环氧氯丙烷胺含有季铵盐基团,可以作为荷正电剂使用.实验以聚环氧氯丙烷胺及2,5-二胺基苯磺酸的混合水溶液为无机相,三酰氯的正己烷溶液为有机相,在聚醚砜超滤基膜上,通过界面聚合制备了一种新型复合荷电镶嵌膜.由图谱可以确定,2,5-二胺基苯磺酸与三酰氯的界面聚合产物是一种带有阳离子交换基团磺酸基团的芳香族聚酰胺类物质;同时由于膜制备过程中荷正电材料聚环氧氯丙烷胺的加入,使得膜的表层带有阴离子交换基团.复合膜由于带有阴阳离子交换基团而具有荷电镶嵌膜的特征.     

界面聚合制备壳聚糖和均苯三甲酰氯复合纳滤膜

以低分子量有机物脱盐为目标,实验以壳聚糖(CS)和均苯三甲酰氯(TMC)为反应单体,通过界面聚合反应在聚砜(PSF)/聚醚砜(PES)共混超滤膜上形成复合层制备纳滤膜.SEM扫描结果表明,该界面聚合反应可以在基膜的表面形成致密选择层;而红外检测结果表明该反应主要是CS分子上的-NH2与TMC分子上的酰氯基发生了酰化反应.实验结果表明:CS在醋酸水溶液中质量分数增大,TMC在正己烷中质量分数增大,界面聚合时间增长和热处理温度增高,都会导致膜的通量降低,同时膜对有机物和电解质的截留率增大.实验优化的界面聚合工艺条件为:CS 0.5%(wt);TMC 0.2%(wt); CS溶液浸没基膜10 min后与TMC溶液进行界面聚合反应2 min,在70℃下热处理10 min后浸泡在0.2%SDS溶液中2 h后晾干.在优化条件下,膜对PEG2000的截留率可达到92%,对NaCl、MgCl2、MgSO4和Na2SO4的截留率分别为7.8%、19.4%、23%和32.8%,该膜对于低分子量有机物与电解质的分离可能会有较好的结果.     

聚酰胺复合纳滤膜的制备与表征

以间苯二甲胺（m-XDA）和均苯三甲酰氟（TMC）分别为水相和油相反应单体，通过界面聚合制备聚酰胺复合纳滤膜。研究了界面聚合反应中水相单体浓度、水相pH值、油相单体浓度、反应时间、后处理温度及时间等因素对所制备的复合膜分离性能的影响。用红外光谱（FT-IR）和扫描电子显微镜（SEM）对所制备的膜进行结构和形态表征。     

双选择层复合正渗透膜制备及其表征

以聚丙烯腈制备基膜,聚氮杂环丙烷、聚-4-苯乙烯磺酸钠为聚阳阴电解质,间苯二胺、均苯酰氯为水相和油相单体,依次用层层自组装(Lb L)和界面聚合制备双选择层正渗透膜,研究Lb L和界面聚合影响膜性能的典型因素。结果表明,优化条件,PEI和PSS的质量浓度均为1.0 g/L,Na Cl浓度为1.0 mol/L,Cu~(2+)浓度为0.20 mol/L,聚电解质单层沉积时间为10.0 min,MPD、TMC的质量浓度分别为20.0、0.25 g/L,单体反应时间均为2.0 min,Lb L3个聚电解质双层,界面聚合1次。在此优化条件下,所得正渗透膜水通量为42.40 L/(m~2·h),反向盐通量为10.86 g/(m~2·h)。结合石英晶体微天平说明Lb L中聚电解质层最为密实,其性能对膜影响较大。这种新的制备方法为提高正渗透工艺展现了一种新途径。     

界面聚合工艺条件对反渗透复合膜性能的影响

以聚砜超滤膜为支撑膜,间苯二胺(MPD)为水相功能单体,均苯三甲酰氯(TMC)为油相功能单体,通过界面聚合法制备了反渗透复合膜。研究了功能单体浓度、界面聚合反应时间、界面聚合成膜后热处理时间和温度等条件对复合膜分离性能的影响;并对在水相中添加相转移催化剂对复合膜分离性能的影响和相转移催化机理进行了初步探讨。首先在单因素实验条件下确定工艺条件的优化范围,然后经过正交实验得到最佳工艺条件,实验结果表明, 油相中TMC浓度为3 g•L^-1、水相中MPD浓度为20 g•L^-1、界面聚合反应时间为30 s、界面聚合成膜后热处理温度为90 ℃、后处理时间15 min时,所制备的反渗透复合膜表现出良好的分离性能,通量达14.91 L•m^-2•h^-1,截留率为0.951(测试条件: 压力1.6 MPa, 温度25 ℃, NaCl浓度20000 mg•L^-1);当水相中MPD浓度较低时,加入适量的相转移催化剂,能有效地改善膜的分离性能。     

荷电纳滤膜的制备研究

以2,5-二氨基苯磺酸（DIA）和聚乙烯亚胺（PEI）的混合溶液为无机相反应单体,以均苯三甲酰氯（TMC）为有机相单体,以水和正己烷分别作为两相溶剂,通过界面聚合技术制备复合荷电纳滤膜。在PEI浓度1．5％的前提下,确定了界面聚合的优化工艺条件：界面聚合时间3min,2,5-二氨基苯磺酸浓度0．25％,酸接受剂浓度（碳酸钠和氢氧化钠以质量比2：1混合）0．15％。     

聚酰胺荷电镶嵌膜的制备及表征(英文)

A novel composite charged mosaic membrane(CCMM) was prepared via interfacial polymerization(IP) of polyamine[poly(epichlorohydrin amine) ]and trimesoyl chloride(TMC) on the polyethersulfone(PES) support. Fourier transform infrared spectroscopy(FT-IR) ,environmental scanning electron microscopy(ESEM) ,atomic force microscopy(AFM) and water contact angle analysis were applied to characterize the resulted CCMM.The FT-IR spectrum indicates that TMC reacts sufficiently with polyamine.ESEM and AFM pictures show that the IP process produces a dense selective layer on the support membrane.The water contact angle of the CCMM is smaller than that of the substrate membrane because of the cross-linked hydrophilic polyamine network.Several factors affecting the IP reaction and the performance of the CCMM,such as monomer concentration,reaction time,pH value of aqueous phase solution and post-treatment,were studied.The pure water flux of the optimized CCMM is 14.73 L·m -2 ·h -1 ·MPa -1 at the operating pressure of 0.4 MPa.The values of separation factorαfor NaCl/PEG1000/water and MgCl2/PEG1000/water are 11.89 and 9.96,respectively.These results demonstrate that CCMM is promising for the separation of low-molecular-weight organics from their salt aqueous solutions.     

Fabrication of anti-fouling polyamide nanofiltration membrane by incorporating streptomycin as a novel co-monomer

Polyamide (PA) thin-film composite (TFC) nanofiltration (NF) membrane has extremely broad application prospects in separation of monovalent/divalent inorganic salts mixed solution. However, membrane fouling is the main obstacle to the application of PA, TFC and NF membrane. Streptomycin (SM) is a hydrophilic antibiotic containing a large number of hydroxyl and amino groups. In this work, the NF membrane was prepared via interfacial polymerization (IP) between trimesoyl chloride (TMC) in the organicphaseand SM/piperazine (PIP) mixture in theaqueousphase. The NF membrane structure and performance were characterized in detail. The results showed that SM successfully participated in the IP. The negative charge and hydrophilicity of membrane surface were improved. The prepared membrane exhibited good anti-adhesion and anti-bacterial performance. Additionally, when the SM concentration was 2%, the prepared membrane exhibited the optimal permselectivity. The water permeance was 89.4 L·m^-2·h^-1·MPa^-1. The rejection of NaCl and Na₂SO₄ were 17.17% and 97.84%, respectively. The NaCl/Na₂SO₄ separation factor of the SM2-PIP/TMC membrane in 1000 mg·L^-1 NaCl and 1000 mg·L^-1 Na₂SO₄ mixed solution was 40, which was 3.3 times that of PIP/TMC membrane. It indicated that SM2-PIP/TMC demonstrated excellent monovalent/divalent salts separation performance. This work provided an easy and effective approach to preparing anti-fouling NF membrane while possessing superior monovalent/divalent salts separation performance.     

Nanofiltration thin-film-composite polyesteramide membranes based on bulky diols

Polyesteramide thin-film-composite (TFC) membranes have promise for diafiltration applications due to their relatively good oxidative resistance coupled with the ability to tailor the membrane rejection profile by varying the ester/amide ratio. The incorporation ofester linkages in interfaciallyprepared polyesteramide TFC membranes has been previously shown to increase the oxidation resistance of the membrane. It was also found that polyesteramide TFC membranes incorporating hydroquinone (HQ) or bisphenol-A (Bis-A) had high rejection for monovalent salts, i.e., their rejection profiles matched those of reverse osmosis rather than nanofiltration membranes. We report the properties of polyesteramide TFC membranes incorporating bulky diols such as phenolphthalein (Phe) and terabromobisphenol-A (TBrBis-A). The data were used to correlate the influence of different ester fanctionalities on membrane flux and rejection characteristics. Membranes incorporating TBrBis-A had relativelyhigh rejections for monovalent salts coupled with low water permeance. By contrast, membranes incorporating Phe showed 10 times higher flux and a rejection profile which appears to be of interest for diafiltration applications involving the separation of organics with molecular weight >400 grnol⁻¹ from low-molecular-weight organics and salts. The Phe-based membranes show rejection characteristics for monovalent and multivalent salts typical of negatively charged membranes.     

A study on the characteristics and pervaporation performance of polyamide thin‐film composite membranes with modified polyacrylonitrile as substrate for bioethanol dehydration

To improve the pervaporation performance in separating an aqueous ethanol solution, polyamide thin‐film composite (TFC) membranes (m‐tolidine‐H‐TMC/mPAN) were prepared through the interfacial polymerization reaction between trimesoyl chloride (TMC) and 2,2'‐dimethylbenzidine hydrochloride (m‐tolidine‐H) on the surface of a modified polyacrylonitrile (mPAN) membrane. The effects of the feed ethanol concentration on the pervaporation performance and the durability of m‐tolidine‐H‐TMC/mPAN TFC membranes were investigated. To choose the optimal mPAN membrane as the TFC substrate, the effect of hydrolysis time on the chemical properties and separation performance of an mPAN substrate was also studied. An appropriate hydrolysis time of 15 min was chosen to obtain the mPAN substrate due to the corresponding high permeation flux. The m‐tolidine‐H‐TMC/mPAN TFC membrane exhibited a high pervaporation performance for ethanol dehydration. A positron annihilation lifetime spectroscopy experiment was used to estimate the mean free‐volume radius of the m‐tolidine‐H‐TMC polyamide selective layer, which lay between the radii of the water and ethanol molecules. © 2013 Society of Chemical Industry     

TMC/TMPIP纳滤超薄复合膜的制备

基于哌嗪(PIP)与均苯三甲酰氯(TMC)界面聚合制备纳滤膜的原理,设计并合成了具有支化结构的三亚胺功能基团水相单体--均苯三甲酰哌嗪(TMPIP)盐酸盐,并与TMC界面聚合制得分子结构与TMC/PIP相同的TMC/TMPIP超薄纳滤复合膜。采用傅里叶红外光谱(FTIR)和扫描电镜(SEM)表征了复合膜皮层的化学结构和表面形貌,结果表明在聚砜底膜表面形成了膜厚为100 nm左右的TMC/TMPIP超薄皮层。通过与TMC/PIP复合膜对PEG 200水溶液的分离性能相比较发现,TMC/TMPIP复合膜因其高度的网络化结构和超薄皮层,因而具有更高的截留率和水通量。考察了TMC/TMPIP复合膜对水中不同盐的截留性能,其截留率顺序与TMC/PIP复合膜相同,而通量和截留率均优于后者。     

Synthesis of 4-Aminobenzoylpiperazine for Preparing the Thin Film Composite Nanofiltration Membrane by Interfacial Polymerization with TMC

A new synthesis method of aromatic diamine, 4-aminobenzoylpiperazine (4-ABP), was studied from 4-aminobenzoic acid and 1-formyl piperazine for the preparation of nanofiltration membrane. The structure of 4-ABP was identified by FT-IR spectra and ¹H NMR spectra. The resulting 4-ABP was used as aqueous monomer to fabricate a thin film on porous polyethersulfone (PES) ultra filtration membranes by interfacial polymerization (IP) with trimesoyl chloride (TMC) as organic monomer. The salt rejection order of these thin film composite (TFC) nanofiltration(NF) membranes is Na₂SO₄>MgSO₄>MgCl₂>NaCl. This sequence indicated that the membranes were negatively charged.     

Effects of the polymerization and pervaporation operating conditions on the dehydration performance of interfacially polymerized thin‐film composite membranes

The disadvantage of dense polyamide membranes when applied in the pervaporation separation process is their low permeation rates. To improve the pervaporation performance, polyamide thin‐film composite membranes were prepared via the interfacial polymerization reaction between ethylenediamine (EDA) and trimesoyl chloride (TMC) on the surface of modified polyacrylonitrile (mPAN) membranes. These composite membranes were applied in the pervaporation separation of alcohol aqueous solutions. On the basis of the best pervaporation performance, the desired polymerization conditions for preparing the polyamide thin‐film composite membranes (EDA–TMC/mPAN) were as follows: (1) the respective concentration and contact time of the EDA aqueous solution were 5 wt % and 30 min and (2) the respective concentration of and immersion time in the TMC organic solution were 1 wt % and 3 min. The polyamide thin‐film composite membranes (EDA–TMC/mPAN) exhibited membrane durability when applied in the pervaporation separation of a 90 wt % isopropyl alcohol aqueous solution at 70°C, which indicated that the polyamide thin film composite (TFC) membranes were suitable for the pervaporation separation process at a high operating temperature. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

3,5-二氧基苯甲酰哌嗪和均苯三甲酰氯界面聚合法制备复合纳滤膜

A new aromatic diamine,3,5-diaminobenzoylpiperazine (3,5-DABP),was synthesized from 3,5-diaminobenzoic acid and 1-formyl piperazine.The structure of 3,5-DABP was identified by FT-IR spectra and 1H NMR spectra.With 3,5-DABP as aqueous monomer and trimesoyl chloride (TMC) as organic monomer,thin film composite (TFC) nanofiltration membranes were prepared by interfacial polymerization technology.The salt rejection order of these TFC membranes is Na2SO4>MgSO4>MgCl2>NaCl.This sequence indicates that the membranes are negatively charged.