界面预湿处理对异质增强型PVDF中空纤维膜结构与性能的影响

以熔融纺丝聚氯乙烯(PVC)中空纤维多孔膜为增强体,聚偏氟乙烯(PVDF)为成膜聚合物,聚乙烯吡咯烷酮(PVP)为添加剂,N,N-二甲基乙酰胺(DMAc)为溶剂,配置铸膜液,采用同心圆牵引-涂覆法制备了异质增强型PVDF中空纤维膜.制备过程中,采用预湿溶液对增强体基膜表面进行预处理,研究了预湿溶液组成及含量对异质增强型PVDF中空纤维膜结构与性能的影响.结果表明,未经预湿处理的异质增强型PVDF中空纤维膜具有较厚的致密界面层;预湿溶液可对基膜表面孔起到保护作用,使异质增强型PVDF中空纤维膜的界面层变薄或形成多孔界面层,有益于改善增强型PVDF中空纤维膜的通透性能;与二甲基乙酰胺(DMAc)水溶液相比,以乙醇水溶液为预湿溶液所得异质增强型PVDF中空纤维膜的性能较优;当预湿液中乙醇含量为60 wt%时,所得增强型PVDF中空纤维膜的渗透性能较优,拉伸强度可达8.61 MPa.     

PVDF亲水复合膜的制备及表征

聚偏氟乙烯(PVDF)膜材料存在强疏水性的缺陷,亲水化改性是解决该问题的主要途径。以PVDF为基膜材料、聚乙烯醇(PVA)为共混材料、N,N-二甲基乙酰胺(DMAc)为溶剂,采用相转化法制备PVDF/PVA复合膜。考察了复合膜的PVDF/PVA共混比、固含量、低分子化合物添加剂、聚合物添加剂等非溶剂添加剂对复合膜接触角的影响。结果表明,当PVDF/PVA共混比为7/3,固含量为13%时,制备的复合膜接触角为22.92°;当添加剂为无水氯化锂、纳米二氧化硅、聚乙烯吡咯烷酮(PVP)时,复合膜接触角分别从53.12°、30.51°和41.89°都降低到了0°,亲水性提高,其中纳米二氧化硅作为添加剂时复合膜亲水性最好;当添加剂为丙三醇、PMMA、PEG时,复合膜接触角都增大,亲水性变差。     

聚偏氟乙烯涂料的研究

用聚偏氟乙烯(PVDF)树脂制备了溶剂型氟碳涂料,筛选并优化了PVDF涂料的溶剂组成。采用丙烯酸树脂对PVDF进行改性,并研究颜填料钛白粉对涂膜性能的影响。结果表明,由甲苯、甲基异丁基酮、乙二醇乙醚乙酸酯、2,2,4-三甲基-1,3-戊二醇单异丁酸酯及邻苯二甲酸二甲酯组成的溶剂体系的涂料综合性能比较好,而丙烯酸树脂和钛白粉的加入明显地改善了PVDF涂膜的性能。     

以聚偏氟乙烯为基底的高渗透选择性聚酰胺/酯纳滤膜的制备与表征

以亲水性聚(N-羟乙基丙烯酰胺)(PHEAA)、疏水性聚甲基丙烯酸甲酯(PMMA)为链段的两亲性三嵌段共聚物PHEAA-b-PMMA-b-PHEAA(PHMH)为改性剂,以聚偏氟乙烯(PVDF)为基底膜材料,利用非溶剂诱导相分离法制备了PVDF/PHMH基底.与未改性PVDF基底相比,PVDF/PHMH基底表面孔径变小,孔隙率和亲水性增加;与PVDF基底纳滤膜N0相比,通过界面聚合制备的PVDF/PHMH基底纳滤膜N1表面粗糙度大、亲水性强、截留分子量小,N1纳滤膜对Na₂SO₄的截留率为96.0%,水渗透通量高达304 L·m^-2·h^-1·MPa^-1,优于商业化纳滤膜的渗透选择性.     

TEP-DMAc混合溶剂对PVDF膜性能的影响

利用非溶剂相转化法(NIPS)制备聚偏氟乙烯(PVDF)膜,考察了聚乙二醇(PEG200)与N,N-二甲基乙酰胺(DMAc)的质量比对膜分相速率和膜性能的影响,讨论了以磷酸三乙酯(TEP)和DMAc的混合液作溶剂对PVDF膜凝胶速率、膜结构和膜通量的影响。结果表明:PEG200的加入减弱了溶剂对聚合物的溶解能力,但铸膜液的分相行为由延迟分相转变为瞬时分相,膜通量提高。随着混合溶剂中TEP含量的增大,铸膜液的黏度增大,分相速率减慢;在高质量比m(TEP)/m(DMAc)时,膜表面的孔增多,指状孔膜结构逐渐消失,整个膜截面呈海绵状,膜通量变大,力学性能提高。     

热致相分离法制聚偏氟乙烯微孔膜稀释剂的选择

依据聚偏氟乙烯(PVDF)、邻苯二甲酸二甲酯、水杨酸甲酯、卡必醇醋酸酯、三醋酸甘油酯、邻苯二甲酸二正丁酯(DBP)、苯乙酮和二苯甲酮(DPK)的Hansen溶度参数及其相对介电常数, 选择能与PVDF以液-液相分离机理进行热致分相的稀释剂, 制备了具有双连续结构的微孔膜. 通过比较PVDF-稀释剂间的溶度参数及相对介电常数的差异, 发现PVDF-DBP体系和PVDF-DPK体系有发生热致液-液相分离的可能. 实时观察上述两个体系的分相过程并测定其结晶温度, 当PVDF质量分数低于30%时, 随着温度的降低, PVDF-DPK体系发生液-液相分离. 根据PVDF-DPK体系相图, 通过控制PVDF含量和降温条件, 无须添加非溶剂或拉伸工艺, 就可以制备出具有双连续结构的PVDF微孔膜.     

复合,多孔PVDF-HFP聚合物电解质膜的制备及其性能研究

采用溶剂/非溶剂方法—即相转移法制得PVDF＿HFP微孔膜,比较了DMC,DEC和PC等3种增塑剂的制孔作用.结果表明:DEC最好,DMC次之,而PC效果最差.聚合物的导电率为1.86×10-3Sm-1(LiPF6＿1mol/L;EC/DMC:1/1wt).     

三嵌段两亲性聚乳酸共聚物的合成及其PVDF共混膜的制备

利用原子转移自由基聚合法(ATRP)合成三嵌段两亲性聚乳酸共聚物聚乙烯吡咯烷酮-聚乳酸-聚乙烯吡咯烷酮(PVP-b-PLA b-PVP),然后将其与聚偏氟乙烯(PVDF)进行其混,制备PVP-b-PLA-b-PVP/PVDF共混膜.结果表明:PVDF膜表面致密,膜断面中指状大孔和海绵状孔同时存在,而共混膜表面多孔,指状大孔贯穿整个断面;与PVDF膜相比,共混膜的孔隙率和孔径增大,水通量提高了158.87％,接触角下降了16.70％,抗污染指标下降了64.7％.     

掺铕多孔硅的恒电位电解法制备及其光致发光

首次报道掺稀土多孔硅的恒电位电解法和稀土硝酸盐－支持电解质－非乙醇有机溶剂的电解体系,这一新方法和新体系具有易于控制电解产物,可掺入高浓度稀土（１０＾２１／ｃｍ＾３以上）,自主控制掺人稀土的浓度并显著增强多孔硅室温光致发光的优点。研究了溶剂、外加电压、Ｅｕ（ＮＯ３）３浓度及电解时间对多孔硅（ＰＳ）室温光致发光的影响,优化了恒电位电解法制备掺铕多孔硅的条件,获得了室温光致发光强度高于多孔硅的ＰＳ：Ｅ     

气息图案法制备规整多孔薄膜的研究进展

气息图案法是一种制备规整多孔薄膜的新方法,该方法在高湿度环境下进行,并使用高挥发、非水溶性的溶剂.通过溶剂快速挥发所引起的暂时低温,诱使水蒸气在溶液表面凝结成规整水滴阵列,从而引导溶质围绕阵列自发形成规整多孔薄膜,全过程廉价、便捷.为促进该方法广泛而深人的研究,本文针对其近年来的研究现状,尤其是面向实用的特点,着重从其...     

细菌纤维素膜的制备与性能

以细菌纤维素为原料,氯化锂(LiCl)/二甲基乙酰胺(DMAc)为溶剂,通过相转化法制备了细菌纤维素膜.用单纤维强力仪对膜的拉伸强度和伸长率进行测试,分析了细菌纤维素浓度、凝固浴温度、凝固浴浓度、凝固时间及塑化条件对膜力学性能的影响.结果表明:在一定范围内,随着制膜液中细菌纤维素浓度的增加、凝固浴温度的降低和凝固浴浓度的增大,膜的拉伸强度和伸长率均提高;随着甘油浓度的增大和塑化时间的延长,膜的拉伸强度逐渐减小,伸长率逐渐增大.     

Improved protein-adsorption-resistant property of PES/SPC blend membrane by adjustment of coagulation bath composition

To improve surface protein-adsorption-resistant property of polyethersulfone (PES) membranes, soybean phosphatidylcholine (SPC) was added to PES casting solution. The blend membranes were prepared by a phase inversion method in a wet process. The surface of PES/SPC blend membranes was characterized by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). XPS data revealed that the phosphorylcholine (PC) groups were concentrated at the surface by changing the composition of coagulation bath. Addition of N,N-dimethylformamide (DMF) in coagulation bath could prolong coagulation time and facilitate the migration of SPC from polymer bulk to membrane surface. The PES/SPC blend membranes dramatically reduced BSA and fibrinogen adsorption compared to PES control membrane due to effective immobilization of PC groups at the surface of PES/SPC blend membranes.     

Preparation and characterization of asymmetric polyethersulfone (PES) membranes

Flat‐sheet asymmetric polyethersulfone (PES) membranes were prepared from polyethersulfone (PES)/ polyethylene glycol (PEG)/ N‐methyl‐2‐pyrrolidone (NMP) system via phase inversion induced by immersion precipitation in water coagulation bath. Effects of propionic acid (PA) as a non‐solvent additive (NSA) on morphology and performance of the membranes prepared from PES/PEG 6000/NMP system in water coagulation bath were investigated. The cross section morphology of the membranes was studied by scanning electron microscopy (SEM). In addition, performance of the membranes was studied by water content measurements and separation experiments using pure water and human serum albumin (HSA) protein solution as feeds. According to SEM analysis, it was found out that the NSA has a significant influence on the structure of the skin layer and the sublayer. The obtained results indicated that addition of PA to the casting solution decreases permeation flux of the prepared membranes. Copyright © 2009 John Wiley & Sons, Ltd.     

Porous membranes modified by hyperbranched polymers: I. Preparation and characterization of PVDF membrane using hyperbranched polyglycerol as additive

Porous membranes were prepared via phase inversion process from casting solution composed of poly(vinylidene fluoride) (PVDF), N,N-dimethylacetamide (DMAc), and hyperbranched polyglycerol (HPG). The membranes were characterized in terms of surface and bulk chemical compositions, morphology, water contact angle, porosity, and water flux. The effects of HPG content on membrane structures and properties were investigated. The effect of HPG addition on the hydrophilicity was discussed as well when the compositions of coagulation bath were changed. To better understand the special effects of HPG on the structures and properties of the membranes, PVDF membranes prepared using HPG as the additive were compared with those prepared using polyethylene glycol (PEG) as the additive.     

A novel positively charged asymmetry membranes from poly(2,6-dimethyl-1,4-phenylene oxide) by benzyl bromination and in situ amination: Part II: Effect of charged group species on membrane performance and morphologies

Positively charged membrane with various charged groups were prepared by in situ amination and phase inversion in which the amine-organic solution and bromomethylated poly(2,6-dimethyl-1,4-phenylene oxide) (BPPO) was cast and immerged into an ethanol coagulation bath. The separation performance and morphologies were examined to investigate the effect of hydrophilicity of charged groups on the selective properties and the structure formation of the membranes. Positively charged groups introduced in the membranes were trimethylbenzylammonium, triethylbenzylammonium, tri-n-propylbenzylammonium and tri-n-butylbenzylammonium, in order of increasing hydrophobicity. Pure water flux and rejection to gelatin of the membranes at three pH values changed remarkably with increasing chain length of alkyl groups. The tendency of the change was mainly explained by coagulation value of the casting solution. The streaming potential and ion exchange capacity of the membranes were determined and the results showed that the membranes were all positively charged. Furthermore, water content, pore size distribution and SEM images of the membranes were examined as well.     

Influence of coagulation temperature on pore size and properties of cellulose membranes prepared from NaOH–urea aqueous solution

The morphology and structure of the regenerated cellulose membranes prepared from its NaOH–urea aqueous solution by coagulating with 5 wt% H₂SO₄–10 wt% Na₂SO₄ aqueous solution with different temperatures and times were investigated. The pore size, water permeability and physical properties of the membranes were measured with scanning electron micrograph (SEM), wide X-ray diffraction (WXRD), Fourier transfer infrared spectroscopy (FTIR), flow rate method, and tensile testing. The SEM observation revealed that the structure and pore size of the membranes changed drastically as a function of the coagulation temperature. The membranes coagulated at lower temperatures tended to form the relatively small pore size than those at higher temperatures. On the contrary, the membranes coagulated at different times exhibited similar pore size. Interestingly, the mean pore size and water permeability of the membranes increased from 110 nm with standard deviation (SD) of 25 nm and 12 ml h⁻¹ m⁻² mmHg⁻¹ respectively to 1,230 nm with SD of 180 nm and 43 ml h⁻¹ m⁻² mmHg⁻¹ with an increase in coagulation temperature from 10 to 60°C. However, the membranes regenerated below 20°C exhibited the dense structure as well as good tensile strength and elongation at break. The result from FTIR and ultraviolet-visible (UV-vis) spectroscopy indicated that the relatively strong intermolecular hydrogen bonds exist in the cellulose membranes prepared at lower coagulation temperatures. This work provided a promising way to prepare cellulose materials with different pore sizes and physical properties by controlling the coagulation temperature.     

Structure and properties of the regenerated cellulose membranes prepared from cellulose carbamate in NaOH/ZnO aqueous solution

Regenerated cellulose (RC) membranes were prepared from cellulose carbamate—NaOH/ZnO aqueous solutions by coagulating with H₂SO₄ solution. Structure, morphology and properties of the membranes were investigated by using scanning electron micrograph (SEM), X-ray diffraction, Fourier transform infrared spectroscopy, flow rate method, and tensile testing. The results from SEM and water permeability revealed that the pore size and water permeability of the membranes in wet state changed drastically as a function of the concentration of H₂SO₄ and coagulation temperature, whereas they hardly changed with the coagulation time. RC membranes coagulated with the relatively dilute H₂SO₄ solution at relatively low temperature exhibited better mechanical properties. This work provided a promising way to prepare cellulose membranes with different pore sizes and good physical properties.     

Effect of PEG additive on membrane formation by phase inversion

This study investigates the effect of PEG additive as a pore-former on the structure formation of membranes and their permeation properties connected with the changes of thermodynamic and kinetic properties in phase inversion process. The membranes were prepared by using polysulfone (PSf)/N-methyl-2-pyrrolidone (NMP)/poly(ethylene glycol) (PEG) casting solution and water coagulant. The resulting membranes prepared by changing the molecular weight of PEG additive and the ratio of PEG to NMP were characterized by scanning electron microscope observations, measurements of water flux and PEG rejection. The thermodynamic and kinetic properties of membrane-forming system were studied through coagulation value, light transmittance and viscosity. The correlations between the final membrane structure/permeation properties and thermodynamic/kinetic properties of membrane forming system are discussed extensively.     

Structure and performance of polyamide-6 membranes prepared by thermally induced phase separation

<正>The asymmetric polyamide-6(PA6) membranes were prepared by thermally induced phase separation.From the scanning electron microscopy(SEM) images,it is observed that with the increase of silicon dioxide(SiO_2) content the structure of obtained membranes gradually varied from cellular structure to large ball-shaped cluster aggregates. Subsequently,with the addition of SiO_2,pure water flux increased first and then decreased,while rejection showed the opposite trend.Besides,raising the coagulation bath temperature was favorable to increase pure water flux.Consequently, different membrane morphologies and performance were obtained by changing SiO_2 content and coagulation bath temperature.     

凝固浴温度对纤维素中空纤维膜结构及气体渗透分离性能影响研究

利用新型溶解工艺,在不同的凝固浴温度(0～60℃)下制备了纤维素中空纤维膜,考察了凝固浴温度对纤维素中空纤维膜结晶结构、机械性能和气体渗透分离性能的影响.扫描电镜表征表明凝固浴温度的升高使得纤维素中空纤维膜更加疏松,并且内侧的指状孔变大变多;膜的机械性能随凝固浴温度的升高而变差;XRD谱图显示凝固浴温度对纤维素中空纤维...