双向拉伸法制备聚醚砜中空纤维

采用双向拉伸的方法制备了聚醚砜中空纤维,探讨了工艺条件对聚醚砜中空纤维取向度和水通量的影响。结果表明:随着纺丝速度的提高,纤维的取向度上升,水通量下降;在总拉伸倍数不变的前提下,随着凝固浴拉伸倍数的提高,纤维的取向度和水通量都减小;随着填充液压力的提高,纤维的取向度下降,水通量增加;随着凝固浴中二甲基亚砜含量的提高,纤维的取向度先增大后减小,出现了一个最大值,水通量先减少后增加,出现了一个最小值。     

聚醚砜中空纤维膜的制备

讨论了在二次成形聚醚砜(PES)中空纤维膜的制备中,PES浓度和不同的填充液对中空纤维膜结构和性能的影响。结果发现:随着PES浓度的增大,中空纤维膜的水通量呈下降的趋势,确定了二次成形PES中空纤维膜制备中PES最佳浓度为24%;不同填充液与溶剂之间的相互扩散速率不同,得到了具有不同结构的聚醚砜中空纤维膜。随着填充液压力的提高,纤维的内径、外径增加,壁厚减小,水通量增大,一般填充液压力为0.020MPa。     

凝固浴质量分数对聚醚砜中空纤维膜结构和性能的影响

采用干喷湿纺法纺制成聚醚砜中空纤维膜，研究了凝固浴质量分数与PES中空纤维结构和性能之间的关系。结果表明：在凝固浴质量分数10％～40％的范围内，中空纤维膜的水通量先减少再增加；中空纤维的取向度则先增大后减小；膜表面孔的数量及孔径都有一个先减后增的现象。     

聚醚砜中空纤维的成形条件对其宏观结构的影响

主要讨论了纺速、填充液压力、凝固浴浓度和拉伸率成形条件的设置对中空纤维的宏观结构的影响 ,为设计具有合理的宏观结构的中空纤维膜提供参考     

中空纤维陶瓷膜的制备及表面修饰

以YSZ粉末、聚醚砜(PES)、N,N-二甲基吡咯烷酮(NMP)为原料,聚乙烯吡咯烷酮(PVP)为添加剂,NMP与水的混合溶液为芯液,自来水为外凝固液,利用相转化法制备了中空纤维陶瓷膜,并研究了PVP质量、芯液组成、涂膜次数对中空纤维陶瓷膜结构和性能的影响。结果表明:随着PVP质量的增加,中空纤维陶瓷膜的抗弯强度逐渐增加,孔隙率与水通量逐渐减小;随着芯液中NMP质量分数的减小,膜的抗弯强度逐渐增强,其水通量和透气率逐渐减小,膜的管壁逐渐变厚;随着涂膜次数的增加,中空纤维陶瓷膜的抗弯强度随之增大,透气率随之减小,修饰层逐渐变厚,膜外表面的孔径和孔数逐渐减少,膜外表面变得越来越致密。     

凝固浴浓度对离子液体法纤维素纤维结构以及性能的影响

探讨了以离子液体1-丁基-3-甲基咪唑氯盐([BMIM]Cl)为溶剂制备的纤维素纤维纺丝工艺条件中凝固浴浓度对纤维结晶结构以及力学性能的影响。实验表明:在相同拉伸比和气隙条件下,凝固浴浓度对再生纤维素纤维的结构以及性能影响较大。随着凝固浴浓度的增加,纤维的结晶度和无定形取向都呈现先增大后减小的趋势,纤维的横向晶粒变小,拉伸强度、初始模量也呈先增大后减小的趋势。     

凝固与拉伸条件对PAN纤维结构形态的影响

应用X射线衍射仪、声速仪、密度梯度管及扫描电子显微镜研究了在不同凝固条件下拉伸对聚丙烯腈(PAN)纤维结构及表面形态的影响规律。结果表明,拉伸对纤维结构形态的影响受凝固条件不同而不同。在凝固速度较慢时,随着拉伸倍数的增加,纤维的结晶度和晶粒尺寸减小,纤维的取向增加先快后慢;在凝固速度较快时,随着拉伸倍数的增加,纤维结晶度先增加后减小,晶粒尺寸一直减小,取向增加呈S型。拉伸倍数的增大使得纤维的直径变细、表面粗糙度增加、密度增加。     

凝固浴体系对PVDF超滤膜性能与结构的影响

利用非溶剂相转化法(NIPS),以聚偏氟乙烯(PVDF)、聚乙烯基吡咯烷酮(PVP)为铸膜液,水、二甲基乙酰胺(DMAC)、PVP体系为凝固浴,制备外压中空纤维超滤膜。研究了凝固浴中DMAC和PVP含量以及凝固浴温度对膜性能和结构的影响。结果表明,凝固浴中DMAC含量的增加可以提高超滤膜的通量、断裂伸长率和表面的孔径,降低膜丝拉力;PVP含量对膜通量、拉力与断裂伸长率有非线性影响,当着PVP的质量分数大于12%时,支撑层孔径明显增加;凝固浴温度升高可以增加膜的通量,而对孔隙率、拉力和断裂伸长率则影响不大。当凝固浴中DMAC和PVP的质量分数分别为35%和12%、凝固浴温度为70℃时,可以得到性能较好得超滤膜。     

基于膜蒸馏技术的PTFE中空纤维膜处理印染反渗透浓水

通过调节挤出头的尺寸和拉伸倍数,制备出4种不同壁厚和孔径的聚四氟乙烯(PTFE)中空纤维膜。采用真空膜蒸馏(VMD)技术处理印染反渗透(RO)浓水,研究了壁厚和孔径、料液温度、浓缩倍数等对处理效果的影响;并进行了连续运行20 d测试。结果表明,减小膜丝壁厚、增加膜孔径和料液温度均可增加产水通量,浓缩倍数增加会降低产水通量;产水通量随工作时间的延长而减小,膜丝经HCl水溶液清洗后,产水通量能恢复至初始通量的95%以上;产水TDS、COD和色度的去除率均保持在95%以上。     

复合中空纤维超滤膜的研制

本文就复合中空纤维超滤膜的制备工艺和成膜条件对膜性能影响进行了系统的研究，实验表明，对外压式中空纤维膜，内凝固液条件的改变，主要影响复合膜的内致密层，进而影响膜的透过通量，但对膜的截留孔径无影响，随空中行走距离增大，膜的透过通量减小，截留孔径增大。另外，通过基膜的选定与内凝固液的调节，复合中空纤维膜的分离孔径主要取决于复合层膜，即在适宜的条件下，基膜不影响复合膜的分离孔径，同时也不决定复合中空纤维     

Preparation of a heterogeneous hollow‐fiber affinity membrane modified with a mercapto chelating resin

A high‐quality, heterogeneous hollow‐fiber affinity membranes modified with mercapto was prepared through phase separation with blends of a chelating resin and polysulfone as membrane materials, poly(ethylene glycol) as an additive, N,N‐dimethylacetamide as a solvent, and water as an extraction solvent. The effects of the blending ratio and chelating resin grain size on the structure of the hollow‐fiber affinity membrane were studied. The effects of the composition of the spin‐cast solution and process parameters of dry–wet spinning on the structure of the heterogeneous hollow‐fiber affinity membrane were investigated. The pore size, porosity, and water flux of the hollow‐fiber affinity membrane all decreased with an increase in the additive content, bore liquid, and dry‐spinning distance. With an increase in the extrusion volume outflow, the external diameter, wall thickness, and porosity of the hollow‐fiber affinity membrane all increased, but the pore size and water flux of the hollow‐fiber affinity membrane decreased. It was also found that the effects of the internal coagulant composition and external coagulant composition on the structure of the heterogeneous hollow‐fiber affinity membrane were different. The experimental results showed that thermal drawing could increase the mechanical properties of the heterogeneous hollow‐fiber affinity membrane and decrease the pore size, porosity, and water flux of the heterogeneous hollow‐fiber affinity membrane, and the thermal treatment could increase the homogeneity and stability of the structure of the heterogeneous hollow‐fiber affinity membrane. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Preparation of polysulfone hollow fiber affinity membrane modified with mercapto and its recovery properties. I. Synthesis and preparation of hollow fiber matrix membrane

Several kinds of chloromethyl polysulfones (CMPSF) with different chlorinity and reactive groups were synthesized by Friedel‐Crafts reaction, which could be utilized as reactively matrix membrane materials. The CMPSF hollow matrix membranes were prepared with phase inversion by utilization of the CMPSF/additive/DMAC casting solution and CMPSF as membrane materials. The rheological behavior of CMPSF/additives/DMAC spinning casting solution was studied. The experimental results showed that the spinning casting solution was a pseudoplastic fluid, the apparent viscosity of the spinning casting solution decreased with the increase of shearing rate, and the viscous flow activity energy of the spinning casting solution was inclined to unchange at high shearing rate. The effects of composition of spinning casting solution and process parameters of dry–wet spinning on the structure of CMPSF hollow fiber matrix membrane were investigated. The pore size, porosity, and water flux of membrane decreased with the increase of additive content, bore liquid, and dry spinning distance. With the increase of extrusion volume outflow, the external diameter, wall thickness, and porosity of the hollow fiber matrix membrane increased, but the pore size and water flux of the membrane decreased. It was also found that the effects of internal coagulant composition and external coagulant composition on the structure of CMPSF hollow fiber matrix membrane were different. The experimental results showed that thermal drawing could increase the mechanical properties of CMPSF hollow fiber matrix membrane and decrease the pore size, porosity, and water flux of the CMPSF hollow fiber matrix membrane, and the thermal treatment could increase the homogeneity and stability of the structure of the CMPSF hollow fiber matrix membrane. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 758–771, 2006     

PVPK30和Tween80对中空纤维超滤膜结构和性能的影响

通过考察添加剂-聚乙烯吡咯烷酮（PVPK30）和Tween80对杂萘联苯聚醚砜酮（PPESK）中空纤维超滤膜结构和分离性能的影响，发现：随高分子添加剂聚乙烯吡咯烷酮K30浓度的升高，膜水通量减小，截留率基本无变化，膜结构逐渐由指状结构转变成海绵状结构。有机大分子添加剂Tween80可以提高膜的水通量，但膜结构不随添加剂浓度而改变，均为指状结构。当Tween80浓度小于5wt％时，随Tween80浓度的增加，膜水通量升高，截留率下降。比较不同凝胶浴温度下的膜分离性能可以看到，凝胶浴温度提高可以显著提升膜的纯水通量。     

溶胀对中空纤维膜萃取器中的流动和传质性能的影响

溶胀是中空纤维膜萃取工业化必须要解决的关键问题之一。本文通过拍摄电镜照片，观察了溶胀前后中空纤维膜表面形态，孔隙率，膜孔径，膜孔道弯曲状况等微观结构的变化。结果表明，溶胀会使中空纤维膜孔隙率减小，膜孔径变小，弯曲因子增大，通过测量发现，溶胀后膜长度增加，而膜的内外径，膜厚基本不变。本文还研究了溶胀时间对中空纤维膜器中的流动及传质效果的影响，通过测量聚丙烯和聚砜中空纤维膜器管程和壳程的停留时间分布曲线表明，对于装填密度较高的膜器，溶胀时间对壳程和管程中的流动状况的影响可以忽略。此外，本文以正辛醇－苯胺－水为实验体系，在中空纤维膜器中进行了循环逆流传质实验。实验证明，由于溶胀使纤维膜阻增加，膜器的传质性能随时间的增加而下降。     

Effect of the preparation conditions on the morphology and performance of poly(imide) hollow fiber membranes

Poly(imide) (PI) hollow fiber membranes were prepared by using classical phase inversion process. Effects of different external coagulation bath temperatures (ECBT) and various bore flow rates (BFR) on the morphology and separation performance of the membranes were studied. Cross‐section, inner and outer structures were characterized by using scanning electron microscope and atomic force microscopy (AFM). Mean pore size, pore size distribution, and mean roughness of the PI hollow fibers surfaces were estimated by AFM. It was found that the hollow fibers morphology composed of sponge‐like and finger‐like structures with different ECBT and BFR. A circular shape of the nodules with different sizes was observed in the outer surface of the PI hollow fibers. Mean pore size of the outer surface increases with increasing ECBT and BFR. The important result observed in this study is that the ECBT clearly has the largest effect on hollow fiber PI membrane roughness compared with the BFR. Pure water permeability of the PI hollow fibers was improved with increase of ECBT and BFR. The solute rejection (R%) was reduced when the ECBT and BFR was increased. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40428.     

Use of hollow polysulfone fibres in the process of dehydrating acetic acid by evaporation through a membrane

Conclusions By use of the double coagulation bath method, membranes have been made from polysulfone having an effective selective layer thickness of 2.5 µm. The limiting size of hollow fibres is as follows: external diameter, 1 mm; internal diameter, 0.6 mm. It was not possible to obtain a surface layer free of defects on increasing the diameter.In the membranes prepared, more than 50% of the resistance to mass-transfer is concentrated in the porous layer.It has been found that the selective layer of the membrane has a critical thickness (which depends of the nature of the polymer, the solvent, and other factors), below which selectivity begins to decrease.In evaporation through a membrane, a dependence of the result of studies on the internal diameter — hollow fibre length was discovered.In an experiment on evaporation through a membrane at 36 K, for the system 80% acetic acid — water, using hollow fibres a selectivity of 116 and a flux of 0.1 kg/m² were obtained.Translated from Khimicheskie Volokna, No. 3, pp. 38–41, May–June, 1993.     

Absorption of SO<Subscript>2</Subscript> using PVDF hollow fiber membranes with PEG as an additive

In this study, removal of SO₂ from gas stream was carried out by using microporous polyvinylidene fluoride (PVDF) asymmetric hollow fiber membrane modules as gas-liquid contactor. The asymmetric hollow fiber membranes used in this study were prepared polyvinylidene fluoride by a wet phase inversion method. Water was used as an internal coagulant and external coagulation bath for all spinning runs. An aqueous solution containing 0.02 M NaOH was used as the absorbent. This study attempts to assess the influence of PEG additive, absorbent flow rate, SO₂ concentration, gas flow rate and gas flow direction on the SO₂ removal efficiency and overall mass transfer coefficient. The effect of liquid flow rate on SO₂ removal efficiency shows that at very low liquid flow rate, the NaOH available at the membrane surface for reacting with SO₂ is limited due to the liquid phase resistance. As liquid flow rate is above the minimum flow rate which overcomes the liquid phase resistance, the SO₂ absorption rate is controlled by resistance in the gas phase and the membrane. The SO₂ absorption rate with inlet SO₂ concentration was sharply increased by using hollow fiber membranes compared to a conventional wetted wall column because the former has higher gas liquid contacting area than the latter. The mass transfer coefficient is independent of pressure. When the gas mixture was fed in the shell side, the removal efficiency of SO₂ declined because of channeling problems on the shell side. Also, the addition of PEG in polymer dopes increased SO₂ removal efficiency. This work was presented at the 6 ^th Korea-China Workshop on Clean Energy Technology held at Busan, Korea, July 4–7, 2006.     

湿纺工艺纺制PAN中空纤维成形机理研究

利用C型喷丝板进行挤出凝固,采用湿法纺丝工艺制备聚丙烯腈(PAN)中空纤维,从PAN/二甲基亚砜(DMSO)纺丝原液的流变性能和凝固过程的相分离两个方面探讨了PAN中空纤维的成形机理。结果表明:纺丝液随剪切速率(γ)的增加逐渐发生由粘性向弹性的转变是挤出胀大的主要原因,其粘弹转变点随着温度的升高而向高γ移动,在60℃下的纺丝液弧片接触成孔的理论临界γ为212 s~(-1);纺丝液在凝固浴中表层成膜是PAN-DMSO-H_2O三元体系相分离的结果,纺丝液细流表面成膜速度是影响孔结构闭合的重要因素,可以通过凝固浴浓度和凝固浴调节剂来控制。