热致相分离法制备聚苯硫醚微孔膜

采用热致相分离法,以己内酰胺为溶剂,制备得到了聚苯硫醚微孔膜并对薄膜性能表征.聚苯硫醚-己内酰胺体系制膜的优点之一是溶剂己内酰胺是水溶性的,可以采用纯水作为后处理的萃取剂.选择了合适的浓度,利用压制成型法制备聚苯硫醚平板膜;研究了体系冷却时的相行为,并考察了降温速率、聚合物浓度等因素对微孔形态与薄膜性能的影响.研究表明,聚苯硫醚-己内酰胺体系以固液分相为主,萃取后形成球晶状的微孔结构.降温速率对薄膜的微孔形态、孔径以及连通性有重要影响;当体系以较低降温速率冷却时,多孔形态为枝叶状,形成了更多的开孔结构并获得了更大的孔径,这是获得高通量微孔膜的主要原因.通过控制降温速率可以制备纯水通量大于100 L/m2h,孔径约4～5μm且连通性良好的聚苯硫醚微孔膜;研究了聚合物浓度的影响,薄膜的纯水通量随着聚合物浓度的增大而减小,并且当聚苯硫醚浓度>50 wt%时,由于大于临界浓度而失去渗透性.     

热诱导相分离法制备亲水性乙烯-丙烯酸共聚物微孔膜

选择 3种不同丙烯酸含量的乙烯 丙烯酸共聚物 (EAA)为原材料 ,二苯醚 (DPE)为稀释剂 ,采用热诱导相分离法 (TIPS)制备了亲水性高分子微孔膜 .接触角实验证明 ,EAA为亲水性高分子材料 .利用熔点仪根据浊度的变化测绘出 3种不同EAA/DPE体系的双结点线以及通过DSC得出相应 3体系的结晶温度曲线 .实验结果还表明 ,随着乙烯 丙烯酸共聚物中丙烯酸含量的增加 ,结晶温度曲线向低温方向移动 ,相对应的膜孔直径也增加 .此外 ,随着EAA DPE体系中EAA初始浓度的逐渐增加 ,膜孔直径逐渐变小 ,当体系中EAA初始浓度高于 5 0 %时 ,不再出现微孔结构     

MICROPOROUS PVDF-HFP-BASED POLYMER MEMBRANES FORMED FROM SUPERCRITICAL CO2 INDUCED PHASE SEPARATION

Microporous poly(vinylidene fluoride-co-hexafluoropropylene)(PVDF-HFP)membranes following supercritical CO_2 induced phase separation process were prepared using four solvents.The solid electrolytes of PVDF-HFP were formed by microporous PVDF-HFP membranes filled and swollen by a liquid electrolyte.The effect of the solvents on the morphology and structure,electrolyte absorptions and lithium ionic conductivity of the activated membranes were investigated.It was approved that all the membrane had the simi...     

FORMATION AND MICROSTRUCTURE OF POLYETHYLENE MICROPOROUS MEMBRANES THROUGH THERMALLY INDUCED PHASE SEPARATION*

Microporous membranes of low-high density polyethylene and their blends were prepared bythermally-induced phase separation of polymer/long-aliphatic chain alcohol (diluent) mixtures.The microstructures of this particular membrane, which depends on the diluent properties,polymer concentration and cooling rate, were observed by scanning electron microscopy."Beehive-type,"leafy-like, and lacy porous structure morphologies can be formed,depending onthe blend composition and phase separation conditions, which were discussed by the polymer anddiluent crystallization processes.     

热致相分离技术制备聚氨酯多孔膜的条件控制

采用自制的模具 ,利用热致相分离 (TIPS)的原理制备了聚氨酯 (PU)多孔膜 ,并重点研究了聚合物浓度对多孔膜的表面形貌、孔度大小、孔隙率和透湿率的影响 .在不同的聚合物浓度条件下制备的PU多孔膜的共同特征是底面 (与成膜平台接触面 )光滑平整 ,孔洞尺寸较小 ,为纳米级 ;而表面 (与空气接触的自由面 )的形貌结构较为复杂 ,但都有明显的孔洞出现 ,且孔洞的尺度大于底面 ,在微米级以上 .聚氨酯 1,4 二氧六环 (DO)形成的是上临界共溶温度 (UCST)体系 ,在发生相分离后底面与表面粗化时间的不同是导致形貌结构差异的主要原因 .改变冷台温度或调整DO H2 O的比例也会对PU多孔膜的孔度大小和形貌结构产生明显的影响     

聚丙烯分子量对热致相分离制备微孔膜的影响

通过对等规聚丙烯与邻苯二甲酸二戊酯体系的相分离过程进行研究,绘制了3种分子量等规聚丙烯与邻苯二甲酸二戊酯体系的相图.研究结果表明,聚丙烯分子量的增大导致聚合物单个分子占据的晶格数Np增加,总分子数减少,使混合熵对混合自由能的贡献降低,因此浊点曲线向高温方向移动,而结晶曲线基本不变.聚丙烯分子量的增大延长了聚合物贫相分散液滴的生长时间、增加了聚合物富相黏度和过冷度.聚丙烯分子量变化不仅改变了微孔尺寸,而且改变了微孔结构.在相同淬冷条件下,微孔平均尺寸的变化趋势是贫相分散液滴的生长时间、聚合物富相黏度和过冷度3种因素共同作用的结果.     

纳米碳酸钙/庚二酸复合成核剂对热致相分离法制备聚丙烯微孔膜的影响

以大豆油/邻苯二甲酸二丁酯(DBP)为混合稀释剂,采用热致相分离法(TIPS)制备聚丙烯(PP)微孔膜.研究了纳米碳酸钙成核剂、纳米碳酸钙/庚二酸复合成核剂对PP/大豆油/DBP(30/42/28,质量比)混合体系中PP结晶、熔融性能和PP微孔膜微观结构的影响.结果表明,单一纳米碳酸钙成核剂加入量为PP的0%~4%(质量百分率)时,PP/DBP/大豆油体系中PP熔融曲线上对应的峰值温度(Tpm)降到150.7~151.3℃,而纯PP的熔融峰值温度为165℃;DSC实验结果还显示加入1%~4%纳米碳酸钙和0.5%庚二酸后,导致PP的熔融曲线上出现了熔融双峰,说明纳米碳酸钙/庚二酸复合成核剂与单一成核剂相比有明显地促进β晶生成的作用,宽角X射线衍射(WAXD)实验进一步证实了β晶的存在.单一纳米碳酸钙成核剂对PP微孔膜的球晶结构和微观孔结构影响不大;加入纳米碳酸钙/庚二酸复合成核剂明显影响PP微孔膜的球晶结构和微观孔结构,其中0.5%庚二酸和1%纳米碳酸钙组成的复合成核剂制得的PP微孔膜的球晶结构明显,微孔膜孔径小且分布均匀;进一步增加纳米碳酸钙用量,PP微孔膜生成了许多细小的边界模糊的不规则结晶,微孔膜孔径不规则且尺寸较大,这与此时PP形成β晶结构有关.     

动力学因素对热诱导相分离法制备亲水性乙烯-丙烯酸共聚物微孔膜结构的影响

选择 3种不同丙烯酸含量的乙烯 丙烯酸共聚物 (EAA)为原材料 ,二苯醚 (DPE)为稀释剂 ,研究了淬冷温度、粗化时间等影响液滴生长的动力学因素对热诱导相分离法 (TIPS)制备EAA DPE亲水性高分子微孔膜结构的影响 .淬冷温度的高低决定了EAA DPE体系是发生液 液相分离还是固 液相分离 ,而产生相分离的机理不同将影响稀释剂液滴的生长 ,最终影响微孔膜的孔径 .实验结果表明 ,在相同粗化时间的条件下 ,随着EAA1 41 0 DPE、EAA3 0 0 2 DPE、EAA3 0 0 3 DPE三体系冷却温度的逐渐升高 ,孔径逐渐变大 .在结晶温度以下 ( 0℃、3 0℃、60℃ )粗化时间相同时 ,温度对微孔膜的孔径影响较小 ,例如 0℃和 3 0℃的恒温条件粗化 1 0min,微孔膜的孔径在 1～ 3 μm之间 ;在 60℃的恒温条件粗化 1 0min ,微孔膜的孔径在 3～ 5 μm之间 .而在 90℃的恒温条件粗化相同的时间 ,由于体系始终处于结晶温度线以上 ,体系始终处在液 液相分离区域 ,最终得到微孔膜的孔径达到了 6～8μm .在结晶温度以下 ( 3 0℃ )进行恒温粗化 ,由于体系的过冷程度很大 ,液滴相的粗化过程被抑制住 ,所以粗化时间对微孔膜的孔径影响不大 ;而在结晶温度以上 ( 90℃ )进行恒温粗化时 ,则是随着粗化时间的延长 ,微孔膜的孔径逐渐变大     

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 cr...     

双连续相微乳液辐射聚合制备多孔材料的研究

利用6 0 Co γ射线在室温下辐照双连续相微乳液体系以制备多孔聚合物材料 ,试图在控制多孔材料的微孔结构形态和减少微乳液聚合过程中的相分离方面做一些探索 .通过电导率的测量分析微乳液的结构类型 ,并确定微乳液的双连续相区域范围 .微乳液聚合后所得的样品的孔结构和聚合前的微乳液结构类型有关 ,扫描电镜和热重分析的结果表明双连续相微乳液在聚合时容易发生相分离 ,未必能够得到开孔结构的聚合物 .但适当控制聚合前微乳液的组成 ,如选择合适的水油比例、交联剂的用量和加入一些功能性单体 (如甲基丙烯酸或丙烯酸钠 ) ,可以有效地抑制相分离 ,调节所得聚合物的结构形态 .     

EFFECT OF DILUENTS ON CRYSTALLIZATION OF POLY(VINYLIDENE FLUORIDE) AND PHASE SEPARATED STRUCTURE IN A TERNARY SYSTEM via THERMALLY INDUCED PHASE SEPARATION

The phase diagram of a ternary system of PVDF,dibutyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP) was determined in terms of a pseudo binary system with the same polymer concentration and different DBP content in diluent mixture.The experimental results showed that as the DBP content increased in diluent mixture,the phase separation changed from liquid-liquid phase separation to solid-liquid phase separation,and both the cloudy point for L-L phase separation and crystallization temperature shif...     

聚偏氟乙烯电纺膜及其电化学性能的研究

用电纺的方法制备了聚偏氟乙烯纳米纤维膜,它们具有多微孔结构,能够作为锂电池聚合物电解质.电纺中聚合物溶液的浓度对制备的电纺膜的结构形态有很大的影响,低浓度(10 wt%)时得到珠丝结构的膜,浓度15 wt%时则为纤维结构,而高浓度(18 wt%)时,电纺膜为交联的网状结构.用电纺法制备的聚偏氟乙烯纳米纤维微孔膜具有较高的孔隙率,而且它们与锂金属电极具有良好的界面稳定性;在25℃时吸液率最高可达340%,以这种膜制备的聚合物电解质室温电导率可达到1.57×10-3S.cm-1;由该电解质组装的扣式电池以0.5 mA.cm-2恒流充放电,25℃时50次循环后几乎无容量损失,具有良好的循环性能;即使60℃时,电池仍能保持良好的工作稳定性.     

采用静电纺丝/非溶剂致相分离制备聚丙烯腈多孔超细纤维的研究

以聚丙烯腈/二甲基亚砜/N,N'-二甲基甲酰胺三元体系为纺丝液、3℃水浴为接收介质,通过静电纺丝制备了具有纳米孔结构的静电纺聚丙烯腈多孔超细纤维.探讨了溶剂比例、接收介质、聚丙烯腈浓度、纺丝电压及接收距离等因素对纤维直径和表面孔隙率的影响.结果表明最佳制备条件为混合溶剂质量比1∶1、纺丝电压16 kV、聚丙烯腈浓度15 wt%、接收距离5 cm、纺丝速率0.7 mL/h、环境温度25℃、相对湿度40%～70%.在此条件下得到的聚丙烯腈多孔超细纤维直径在420～490 nm,平均直径468 nm,表面孔隙率3.4%,纤维内部形成大量孔径为8～30 nm的孔结构,且孔径分布均匀,孔形状相对一致.N2吸附脱附测试表明,聚丙烯腈多孔纤维的BET比表面积达43.86 m2/g,是相同直径无孔聚丙烯腈纤维比表面积理论值的6倍.通过研究聚丙烯腈/(二甲基亚砜+N,N'-二甲基甲酰胺)/水的三元相图,提出非溶剂致相分离是主要成孔机理.     

PREPARATION OF ASYMMETRIC POLYETHERKETONE FLAT AND HOLLOW FIBER MEMBRANES FOR GAS SEPARATION USING ACETIC ACID BASED COAGULANTS

Membranes for gas separation have developed significantly in the last twenty years,however,there is still a need for high temperature and chemically resistant membranes that exhibit good selectivity and gas permeability.Our study examines the fundamental properties of polyetherketone (PEK,a thermally stable and chemically resistant polymer) membranes prepared using concentrated sulphuric acid (98% H_2SO_4) as the solvent.Non-solvents used in the work included acetic acid,ethanol,methanol,glycerol,and wat...     

离子交换法分离固相合成胸腺五肽

采用离子交换法分离纯化,对影响分离的多种因素包括吸附动力学、pH值、缓冲液和树脂的种类进行了深入讨论.结果发现,采用SP sepharose FF树脂、pH 4.4的醋酸缓冲液分离效果较好,经过方案优化,在pH 4.4醋酸缓冲液平衡、盐梯度洗脱条件下纯化TP5,HPLC和质谱分析表明,一步分离纯度可达98%以上.该法可以满足大规模制备的要求.     

PREPARATION OF PVA/PAN PERVAPORATION COMPOSITE MEMBRANES AND THEIR SEPARATION PROPERTIES

制备了活性层厚度为１～１０μｍ的ＰＶＡ／ＰＡＮ渗透汽化复合膜并将其用于乙醇水混合物的分离。实验结果表明，热处理条件对复合膜的分离选择性、渗透通量及分离指数具有明显影响。确定了最佳热处理条件。     

螯合树脂／聚砜复合滤膜的制备研究

本文以聚砜（PS）／螯合树脂（D418）作为膜材料,用相转化法制备了共混螯合平板滤器。考察了聚合物共混比例、凝固浴的组成、膜在空气中的蒸发时间,以及制膜液温度等工艺参数的变化对膜结构性能的影响。     

PREPARATION OF POLYVINYLIDENE FLUORIDE／POLYVINYL DIMETHYLSILOXANE COMPOSITE HOLLOW FIBER MEMBRANES AND THEIR SEPARATION PROPERTIES

Microporous polyvinylidene fluoride (PVDF) hollow fibre membranes were spun using the dry-wet phase inversion method. By means of dip-coating technique, a uniform coating with thickness of around 5-12μm of polyvinyl dimethylsiloxane (PVDMS) was formed on the surface of porous PVDF hollow fibers. The structural parameters of PVDF substrate membrane were estimated by gas permeation test. Using N2/O2 as the medium, the separation properties of PVDMS-PVDF composite hollow fiber membranes were also evaluated experimentally. The experimental data of both permeability and selectivity are in good agreement with the theoretical results predicted by the presented pore-distribution model, in order to obtain the compact composite membrane free of defects by the dip-coating technique, the thickness of PVDMS skin must be higher than 5μm.     

SEPARATION OF PROPANE FROM PROPANE/NITROGEN MIXTURES USING PDMS COMPOSITE MEMBRANES BY VAPOR PERMEATION

This study deals with polydimethylsiloxane(PDMS)/polyvinylidene fluoride(PVDF) composite membranes for propane separation from propane/nitrogen mixtures,which is relevant to the recovery of propane in petroleum and chemical industry.The surface and cross-section morphology of PDMS/PVDF composite membranes was observed by scanning electron microscope(SEM).The surface morphology of PDMS/PVDF composite membranes is very dense.There are three layers,the thin dense top layer,finger-like porous middle layer an...     

SEPARATION OF PROPANE FROM PROPANE/NITROGEN MIXTURES USING PDMS COMPOSITE MEMBRANES BY VAPOUR PERMEATION

 This study deals with polydimethylsiloxane (PDMS)/polyvinylidene fluoride (PVDF) composite membranes for propane separation from propane/nitrogen mixtures, which is relevant to the recovery of propane in petroleum and chemical industry. The surface and cross-section morphology of PDMS/PVDF composite membranes was observed by scanning electron microscope (SEM). The surface morphology of PDMS/PVDF composite membranes is very dense. There are three layers, the thin dense top layer, finger-like porous middle layer and sponge-like under layer in the cross-section SEM image of PDMS/PVDF composite membranes. The effects of the types of cross-linking agents and pressure on the membrane permselectivity were investigated. The permeability of nitrogen was independent of feed pressure. However, the permeability of propane increased with the pressure increasing for all membranes. The membrane cured by a tri-functional crosslinker with attached vinyl groups had better performance than the tetra-functional one, in both selectivity and permeation flux. The total permeation flux is 1.769× 10^-2 cm³(STP)/(cm²·s) and the separation factor is 19.17 when the mole percent of propane in the gas mixture is 10 at the 0.2 MPa pressure difference and 25°C.