Effect of Extractant and Cold-drawing on the Structure and Performance of HDPE Hollow Fiber Membranes Fabricated via Thermally Induced Phase Separation Method

Microporous polyolefin hollow fiber membranes were prepared from high density polyethylene （HDPE）-paraffin solution via thermally induced phase separation （TIPS） method. Effects of extraction and cold-drawing condition on membrane structure and performance were investigated.Five volatile solvents were used as extractant. Dimension of hollow fiber and gas permeation rate of membrane were measured. Mierostructure of membrane was examined by Scanning Electronic Microscope （SEM）. The results show that the membrane treated by pentane possesses a higher porosity, nitrogen permeability and lower shrinkage than those of membranes extracted by other three extractants. It is also found that the membrane stretched 133% shows the highest porosity and gas permeability in this study.

Construction of Renewable Superhydrophobic Surfaces via Thermally Induced Phase Separation and Mechanical Peeling

We report a simple preparation method of a renewable superhydrophobic surface by thermally induced phase separation （TIPS） and mechanical peeling. Porous polyvinylidene fluoride （PVDF） membranes with hierarchical structures were prepared by a TIPS process under different cooling conditions, which were confirmed by scanning electron microscopy and mercury intrusion porosimetry. After peeling off the top layer, rough structures with hundreds of nanometers to several microns were obtained. A digital microscopy determines that the surface roughness of peeled PVDF membranes is much higher than that of the original PVDF membrane, which is important to obtain the superhydrophobicity. Water contact angle and sliding angle measurements demonstrate that the peeled membrane surfaces display super- hydrophobicity with a high contact angle （152°） and a low sliding angle （7.2°）. Moreover, the superhydrophobicity can be easily recovered for many times by a simple mechanical peeling, identical to the original superhydrophobicity. This simple preparation method is low cost, and suitable for large-scale industrialization, which may offer more opportunities for practical applications.

PREPARATION OF MICROPOROUS ULTRA HIGH MOLECULAR WEIGHT POLYETHYLENE (UHMWPE) BY THERMALLY INDUCED PHASE SEPARATION OF A UHMWPE/LIQUID PARAFFIN MIXTURE

Ultra-high molecular weight polyethylene (UHMWPE) with a microporous structure was prepared via thermally induced phase separation (TIPS).Liquid paraffin (LP) was used as a diluent in the preparation of microporous UHMWPE. Small angle laser light scattering (SALLS) and differential scanning calorimetry (DSC) were used to determine the phase separation temperatures,i.e.the cloud points and the dynamic crystallization temperatures,respectively.It was found that the cloudI points were coincident with the cryst...

Effect of Diluent on the Morphology and Performance of IPP Hollow Fiber Microporous Membrane via Thermally Induced Phase Separation

Isotactic polypropylene （iPP） hollow fiber microporous membranes were prepared using thermally induced phase separation （TIPS） method. Di-n-butyl phthalate （DBP）, dioctyl phthalate （DOP）, and the mixed solvent were used as diluents. The effect of α （DOP mass fraction in diluent） on the morphology and performance of the hollow fiber was investigated. With increasing α, the morphology of the resulting hollow fiber changes from typical cellular structure to mixed structure, and then to typical particulate structure. As a result, the permeability of the hollow fiber increases sharply, and the mechanical properties of the hollow fiber decrease obviously. It is suggested that the morphology and performances of iPP hollow fiber microporous membrane can be controlled via adjusting the compatibility between iPP and diluent.

Effects of F127 on Properties of PVB/F127 Blend Hollow Fiber Membrane via Thermally Induced Phase Separation

Hydrophilic poly(vinyl butyral)(PVB) /Pluronic F127(F127) blend hollow fiber membranes were prepared via thermally induced phase separation(TIPS) ,and the effects of blend composition on the performance of hydrophilic PVB/F127 blend hollow fiber membrane were investigated.The addition of F127 to PVB/polyethylene glycol(PEG) system decreases the cloud point temperature,while the cloud point temperature increases slightly with the addition of F127 to 20%(by mass) PVB/F127/PEG200 system when the concentration of F127 is not higher than 5%(by mass) .Light scattering results show that the initial inter-phase periodic distance formed from the phase separation of 20%(by mass) PVB/F127/PEG200 system decreases with the addition of F127,so does the growth rate during cooling process.The blend hollow fiber membrane prepared at air-gap 5mm,of which the water permeability increases and the rejection changes little with the increase of F127 concentration.For the membrane prepared at zero air-gap,both water permeability and rejection of the PVB/F127 blend membrane are greater than those of PVB membrane,while the tensile strength changes little.Elementary analysis shows that most F127 in the polymer solution can firmly exist in the polymer matrix,increasing the hydrophilicity of the blend membrane prepared at air-gap of 5mm.

PREPARATION OF HIGH DENSITY POLYETHYLENE/POLYETHYLENE-BLOCK-POLY(ETHYLENE GLYCOL)COPOLYMER BLEND POROUS MEMBRANES VIA THERMALLY INDUCED PHASE SEPARATION PROCESS AND THEIR PROPERTIES

High density polyethylene （HDPE）/polyethylene-block-poly（ethylene glycol） （PE-b-PEG） blend porous membranes were prepared via thermally induced phase separation （TIPS） process using diphenyl ether （DPE） as diluent. The phase diagrams of HDPE/PE-b-PEG/DPE systems were determined by optical microscopy and differential scanning calorimetry （DSC）. By varying the content of PE-b-PEG, the effects of PE-b-PEG copolymer on morphology and crystalline structure of membranes were studied by scanning electron microscopy （SEM） and wide angle X-ray diffraction （WAXD）. The chemical compositions of whole membranes and surface layers were characterized by elementary analysis, Fourier transform infrared spectroscopy-attenuated total reflection （FTIR-ATR） and X-ray photoelectron spectroscopy （XPS）. Water contact angle, static protein adsorption and water flux experiments were used to evaluate the hydrophilicity, antifouling and water permeation properties of the membranes. It was found that the addition of PE-b-PEG increased the pore size of the obtained blend membranes. In the investigated range of PE-b-PEG content, the PEG blocks could not aggregate into obviously separated domains in membrane matrix. More importantly, PE-b-PEG could not only be retained stably in the membrane matrix during membrane formation, but also enrich at the membrane surface layer. Such stability and surface enrichment of PE-b-PEG endowed the blend membranes with improved hydrophilicity, protein absorption resistance and water permeation properties, which would be substantially beneficial to HDPE membranes for water treatment application.

Fabrication of poly(vinylidene fluoride) membrane via thermally induced phase separation using ionic liquid as green diluent

Ionic liquid(IL),1-butyl-3-methylimidazolium hexafluorophosphate([BMIM]PF6)as a new and environmentally friendly diluent was introduced to prepare poly(vinylidene fluoride)(PVDF)membranes via thermally induced phase separation(TIPS).Phase diagram of PVDF/[BMIM]PF6 was measured.The effects of polymer concentration and quenching temperature on the morphologies,properties,and performances of the PVDF membranes were investigated.When the polymer concentration was 15 wt%,the pure water flux of the fabricated membrane was up to nearly 2000 L·m-2·h-1,along with adequate mechanical strength.With the increasing of PVDF concentration and quenching temperature,mean pore size and water permeability of the membrane decreased.SEM results showed that PVDF membranes manufactured by ionic liquid(BMIm PF6)presented spherulite structure.And the PVDF membranes were represented asβphase by XRD and FTIR characterization.It provides a new way to prepare PVDF membranes with piezoelectric properties.

Synergistic action of non-solvent induced phase separation in preparation of poly(vinyl butyral) hollow fiber membrane via thermally induced phase separation

A systematic study of air gap distance effects on the structure and properties of poly(vinyl butyral)hollow fiber membrane via thermally induced phase separation(TIPS)has been carried out.The results show that the hollow fiber membrane prepared at air gap zero has no skin layer; the pore size near the outer surface is larger than that near the inner surface; and the special pore channel-like structure near the outer surface is formed,which is quite different with the typical sponge-like structure caused by TIPS and the finger-like structure caused by non-solvent induced phase separation(NIPS),because of the synergistic action of non-solvent induced phase separation at air gap zero.The pore size gradually decreases from outer surface layer to the intermediate layer,but increases gradually from intermediate layer to the inner surface layer.With the increase of air gap distance,the pore size near the outer surface gets smaller and a dense skin layer is formed,and the pore size gradually increases from the outer surface layer to the inner surface layer.Water permeability of the hollow fiber membrane decreases with air gap distance,the water permeability decreases sharply from 45.50×10-7 to 4.52×10-7 m3/(m2·s·kPa)as air gap increases from 0 to 10 mm at take-up speed of 0.236 m/s,further decreases from 4.52×10-7 to 1.00×10-8 m3/(m2·s·kPa)as the air gap increases from 10 to 40 mm.Both the breaking strength and the elongation increase with the increase of air gap distance.The breaking strength increases from 2.25 MPa to 4.19 MPa and the elongation increases from 33.9% to 132.6% as air gap increases from 0 mm to 40 mm at take-up speed 0.236 m/s.

Effects of coagulation bath temperature on structure and performance of poly(vinyl butyral) hollow fiber membranes via thermally induced phase separation

Poly （vinyl butyral） （PVB） hollow fiber membranes were fabricated via thermally induced phase separation （TIPS）. The effects of coagulation bath temperature （CBT） on the structure and performance of membranes were investigated in detail. The morphologies of the membranes were studied by scanning electron microscopy （SEM）, the performances of water permeability, rejection, breaking strength and elongation were measured, respectively. The results indicate that all the membranes have the asymmetric morphology and the thickness of the skin layer decreases and the pore size of the outer layer increases with the increase of CBT. The permeability of membranes prepared at air gap 1.0 cm and take-up speed 0.253 m/s increases from 1.047×10-7 to 5.909×10-7 m3/（m2·s-kPa） with the CBT increasing from 20 ℃ to 40℃, and sharply increases to 35.226×10 7 m3/（m2.s.kPa）once the CBT arrives at 50 ℃. While the carbonic ink rejections have no significant decrease, totally exceed 98%, but that of acid-maleic acid copolymer greatly decreases with the increase of CBT. Both the breaking strength and elongation decrease with the increase of CBT.

Fabrication of Poly(vinylidene fluoride) /Polysulfone Flat Blend Membranes via Thermally Induced Phase Separation Process for Water Treatment

Poly(vinylidene fluoride) /polysulfone(PVDF/PSF) flat blend membrane was prepared via thermally induced phase separation(TIPS) technique.The membrane formation mechanism and membrane structure were investigated and the effects of PSF/PVDF weight ratio on morphology,crystallinity,porosity,and mechanical properties of the membrane were discussed.The relationship between membrane structure and performances,such as pure water flux and the rejection of carbonic black,was also discussed.It was found that solid-liquid(S-L) phase separation occurred for the PVDF/PSF/diluent system.The addition of PSF influences structure and crystallinity of the membrane,which in turn influences mechanical properties and performances of the membrane.The results reveal that it is possible to obtain network structure via S-L phase separation by blending the polymer,which has a partial compatibility with PVDF.

基于改性逆向热致相分离法聚砜微孔膜的制备与性能

针对逆向热致相分离法(RTIPS)制备聚砜(PSF)微孔膜成膜体系稳定性较差的问题,首先对亲水性的端羟基型超支化聚酯(HBPE)进行封端,然后以PSF为膜材料,通过添加亲水剂封端HBPE构建四元低临界共溶温度(LCST)成膜体系PSF/HBPE/N,N-二甲基乙酰胺/聚乙二醇400,采用改性逆向热致相分离法(m-RTIPS)一步制备了亲水性PSF微孔膜。对封端HBPE进行了结构分析和分子量测试,分析了HBPE的封端率对四元成膜体系浊点和黏度的影响,研究了HBPE的封端率对PSF微孔膜的形貌、渗透性、亲水性、抗污染性和力学性能的影响。结果表明,成功对HBPE进行了封端,封端后HBPE的分子量增加;成膜体系的浊点和黏度随HBPE封端率的升高而增大,但黏度上升的幅度较小;3种添加不同封端率HBPE的PSF微孔膜的纯水通量、截留率、亲水性和力学性能都优于纯PSF微孔膜;随HBPE封端率的增加,膜的纯水通量下降,但截留率差别很小。当HBPE封端率为30%时,PSF膜纯水通量恢复率达88%,抗污染性最佳。添加不同封端率HBPE都可制得表面多孔的膜,当HBPE封端率为50%时,PSF膜具有全双连续结构的形貌,其拉伸强度、拉伸弹性模量和断裂伸长率分别为4.86,143.92 MPa和22.68%,综合力学性能优异。

形状回复力对抑制破骨细胞形成的调控作用

破骨细胞是骨吸收的主要功能细胞,具有力学敏感性。本研究旨在利用形状记忆聚合物(SMPs)的形状回复力原位调控破骨细胞的形成。首先将纯聚乳酸(PLA)、不同质量比(7∶3、5∶5、3∶7)的PLA和聚己内酯(PCL)通过热致相分离法(TIPS)制备PLA/PCL 3D支架,并表征其形貌、结构、热性能;然后,将筛选的PLA/PCL(5∶5)支架在45℃下压缩塑形(压缩比分别为0、50%、75%)和4℃下冷却固定,并表征形状记忆性能;最后,通过基于RAW264.7巨噬细胞的破骨分化实验验证了形状回复力对抑制破骨细胞形成的调控作用。结果表明:PLA/PCL(5∶5)材料体系的形状回复温度接近人体体温,适合制备3D支架;形状回复力与塑形应变相关,压缩比75%组的支架产生的形状回复力为50%组的1.7倍;形状回复力可抑制巨噬细胞的融合分化及相关功能表达,对破骨细胞形成的抑制作用与回复力大小有关。

压缩二氧化硅/聚乙烯气凝胶复合薄膜的辐射制冷性质

利用热诱导相分离法和简单的压缩工艺制备了压缩二氧化硅/聚乙烯(SiO_(2)/PE)气凝胶复合薄膜,通过表征薄膜的微观结构和光学性能,研究了SiO_(2)添加量和气凝胶压缩程度对薄膜光学性能的影响。当纳米SiO_(2)、微米SiO_(2)、聚乙烯的质量比为0.5∶1∶1,压缩比(压缩后气凝胶薄膜厚度与未压缩气凝胶厚度之比)为1/9时,可得最佳样品。最佳样品具有96.4%的太阳光谱平均反射率和95%的大气窗口平均发射率,能通过自身辐射制冷能力获得最高6.5℃的温度降低,可对亚环境进行全天候冷却。

表面特性对棘齿型Knudsen泵气体分离特性影响的模拟研究

Knudsen泵作为一种微型泵,在微机电系统(MEMS)中具有广泛应用。本文提出了一种具有不同表面反射系数的棘齿型Knudsen泵,通过直接模拟蒙特卡罗(DSMC)方法对该泵内He-Xe混合气体流动特性进行了数值模拟研究。结果表明:表面反射特性对Knudsen泵内的流场特性和气体分离特性影响巨大,不同的表面反射特性导致了Knudsen泵内不同的热驱流动机理;三角形倾斜边的α_(n)=σ_(t)=0时Knudsen泵内主要热驱流动为辐射流,有利于气体分离,而α_(n)=σ_(t)=1时Knudsen泵内主要热驱流动为热边缘流,对气体分离没有明显有利作用;三角形倾斜边的α_(n)=σ_(t)=0时He和Xe的速度和扩散速度在三角形棘齿上顶点附近差异最大,而α_(n)=σ_(t)=1时在三角形棘齿左侧顶点附近差异最大;越轻的气体流动速度和扩散速度越快。本文可为实际工程应用中微型气体分离装置的设计和生产提供理论依据。

低温热致相分离法制备PVDF-CTFE多孔膜的研究

利用低温热致相分离法制备了PVDF-CTFE多孔膜,重点考察了甘油含量和凝固浴温度对成膜机理和性能的影响.结果表明,甘油有促进热致相分离(TIPS)和非溶剂致相分离(NIPS)的双重作用.甘油含量的提高,一方面作为非溶剂使铸膜液浊点温度与凝固浴温度的温差变大,加强了TIPS效应,使膜结构呈TIPS效应为主的双连续结构,避免了NIPS效应所致典型的指状孔结构;另一方面作为NIPS的致孔剂,会加强NIPS效应,促使发生双扩散,生成更多孔结构,二者竞争共同作用.最终甘油含量的提高使TIPS效应占主导,NIPS所致的皮层结构变薄,膜断面结构从致密堆积状向多孔蜂窝状结构转变,提高了膜的通透性.当甘油添加量为7.5%(质量分数)时,PVDF-CTFE中空纤维多孔膜综合性能最佳,拉伸断裂强度达2.6 MPa,纯水通量达860 L/(m^(2)·h·MPa).凝固浴温度的提高,减少了铸膜液浊点温度与凝固浴的温差,减弱了TIPS效应,加强了NIPS效应的传质过程,使膜结构从蜂窝状结构向指状孔结构转变,皮层厚度增加,导致膜孔隙率和纯水通量提高,力学性能下降.当凝固浴温度为80℃时,PVDF-CTFE平板多孔膜的纯水通量为1510 L/(m^(2)·h·MPa),拉伸断裂强度为2.1 MPa.

热处理工艺对PES亲水膜性能的影响研究

采用非溶剂致相分离法,以聚醚砜(PES)、聚乙烯吡咯烷酮(PVP-K90)、N,N-二甲基乙酰胺(DMAc)为原料制备PES亲水平板膜,探讨和分析了热处理工艺对PES亲水膜性能的影响。结果表明:热处理工艺对膜PVP溶出值影响较大,热处理温度越高,热处理时间越长,膜PVP溶出值越低。热处理温度对膜力学性能影响不大。随着热处理时间的增加,膜亲水性逐渐升高。热处理有利于膜水通量的提升,当热处理温度为80℃时,膜水通量为最大值。

超高分子质量聚乙烯纤维纺丝工艺的研究进展

结合国内外生产研究现状,对超高分子质量聚乙烯(UHMWPE)纤维的发展历程、工艺路线、纺丝原理及其应用进行了梳理,从分子链聚集态结构变化的角度对冻胶纤维的超倍热拉伸和热定形进行解读,通过热致相分离的原理对冻胶丝成形进行阐述。并针对国内外现有研究工艺中的不足,对提高UHMWPE纤维力学性能、抗蠕变性等方面提出工艺改进方案,以期为UHMWPE纤维在不同领域中的应用和发展提供有益参考。

Formation of microporous polymeric membranes via thermally induced phase separation： A review

A review of recent research related to micro- porous polymeric membranes formed via thermally induced phase separation （TIPS） and the morphologies of these membranes is presented. A summary of polymers and suitable diluents that can be used to prepare these microporous membranes via TIPS are summarized. The effects of different kinds of polymer materials, diluent types, cooling conditions, extractants and additive agents on the morphology and performance of TIPS membranes are also discussed. Finally new developments in TIPS technology are summarized.

Poly(vinylidene fluoride-co-hexafluoro propylene) membranes prepared via thermally induced phase separation and application in direct contact membrane distillation

A non-toxic and environmentally safe diluent,acetyl tributyl citrate,was employed to prepare poly(vinylidene fluoride)-co-hexafluoropropylene membranes via thermally induced phase separation.Effects of the polymer concentration on the phase diagram,membrane morphology,hydrophobicity,pore size,porosity and mechanical properties(tensile stress and elongation at break)were investigated.The results showed that the pore size and porosity tended to decrease with increasing polymer concentration,whereas the contact angle,liquid entry pressure and mechanical properties showed the opposite trend.In direct contact membrane distillation operation with 3.5 wt-%sodium chloride solution as the feed solution,the prepared membranes performed high salt rejection(>99.9%).Furthermore,the prepared membranes retained excellent performance in long-term stability tests regarding the permeate flux and salt rejection. ne distillation.