CN102164658A - 浇铸在针织品上的不对称和复合分离膜 - Google Patents

浇铸在针织品上的不对称和复合分离膜 Download PDF

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CN102164658A
CN102164658A CN2009801375064A CN200980137506A CN102164658A CN 102164658 A CN102164658 A CN 102164658A CN 2009801375064 A CN2009801375064 A CN 2009801375064A CN 200980137506 A CN200980137506 A CN 200980137506A CN 102164658 A CN102164658 A CN 102164658A
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film
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M-W·唐
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Honeywell UOP LLC
Universal Oil Products Co
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Abstract

本发明涉及用于气体和液体分离的膜的制备，其中将聚合物层直接施加到代替常规布或玻璃或金属基底的针织品织物上。

Description

浇铸在针织品上的不对称和复合分离膜
发明背景
为开发用于超滤、纳滤、全蒸发、反渗透和气体分离的不对称和复合膜做出了大量的努力。溶剂浇铸转相方法通常用于制备平片膜。在该方法中，选择合适聚合物、溶剂和非溶剂(溶胀剂)并以合适比例混合以对膜提供所需形态。不对称膜通过使用刮刀将聚合物溶液(常称作“浇铸涂布漆”(casting dope))铺展到光滑基底顶上的薄膜中，随后在水性浴中沉淀并在升高的温度下干燥而形成。浇铸到光滑基底如玻璃、金属、金属板或层压有塑料如聚乙烯的金属或涂覆有试剂的基底上并随后从其剥离的膜称为“自支撑”(free-standing)膜。除了脆度外，由于干燥时不均匀收缩的起皱的问题处理也是在大规模生产“自支撑”膜时遇到的主要障碍。这类选择性膜可非常昂贵地开发和生产，因此它们具有高价格。浇铸在非剥离性基底上的膜称作“浇铸在布上”(cast-on-cloth)的膜，并且该“浇铸在布上”的膜的性能主要取决于需对整个膜提供适当机械强度和结构完整性的织物的性质。基底的选择因此对需要容许其操作中遇到且必要的跨膜压降，或者在预期操作环境中以完整材料保持合理寿命的膜种类来说尤其重要。
发明概述
本领域熟练技术人员熟知能够提供满足膜要求的该种性能的基底的有限选择。这是因为不对称或复合膜仅通过织物基底最佳预成型，该织物基底(1)将对膜提供适当机械强度和结构完整性；(2)呈现光滑、均匀、平坦的(平的)表面而不露出纤维，不对称膜可以在其上形成而具有最少量的针孔和其他缺陷；(3)对化学反应呈惰性，和(4)为多孔的且具有高渗透性，从而不降低整个膜的通量。通常合适的基底织物具有约100-125微米的厚度。优选使用由Nylon或
Figure BDA0000051839840000012
聚酯制成的织造布。可使用的其他织物包括：
Figure BDA0000051839840000021
增强纸和
Figure BDA0000051839840000022
非织造聚酯。本发明的目的是为选择性不对称或复合膜提供一种基底，其组合下列特征(1)可通过常规转相浇铸技术廉价地制备，(2)显示优异的渗透性和选择性，(3)在操作条件下维持膜的寿命，和(4)提高了螺旋缠绕型或板和框架模件构造的填充密度。
发明详述
本发明为一种制备不对称分离膜的方法，该不对称分离膜包括涂覆有在大于200℃的温度下交联的基于“双酚A”的环氧化物的针织品(tricot)支撑基底、在宽范围的温度和压力下提供高渗透性和选择性的聚合物涂布漆和通过用可热固化或可UV固化聚硅氧烷或其他合适涂料涂覆不对称膜表面的罩面漆。不对称或复合分离膜包括纤维素膜如乙酸-丁酸纤维素、丙酸纤维素、乙基纤维素、甲基纤维素、硝酸纤维素和由其他聚合物涂布漆如聚砜、聚醚砜、聚酰胺、聚酰亚胺、聚醚酰亚胺、聚酰胺/酰亚胺；聚醚酮；聚醚醚酮、聚亚芳基氧；聚(酯酰胺-二异氰酸酯)；聚氨酯；聚苯并苯并咪唑；聚酰肼；聚二唑(polyoxadiazoles)；聚***；聚苯并咪唑；聚碳二亚胺；聚膦嗪；微孔聚合物、聚碳酸酯、聚苯乙烯、聚丙烯、全氟聚合物、聚丙烯酸、多芳基化合物、聚对苯二甲酸乙二酯、聚硅氧烷、聚丙烯腈、聚甲基丙烯腈、聚乙烯醇、聚硫化物、聚苯并
Figure BDA0000051839840000024
唑、聚偏二氟乙烯及其混合物形成的膜。
更具体地，将形成膜的聚合物薄膜(film)直接浇铸到针织品织物层的光滑侧，其中使形成膜的聚合物薄膜永久且整体地粘合。通常用于制备本发明不对称和复合膜的针织品基底具有交联的环氧化物涂层，范围为10-50重量％的环氧树脂。优选20-30重量％的环氧化物涂层。针织品的透气性为1-20cm3/(sec.cm2)，在本实施方案中优选使用透气性为2-5cm3/(sec.cm2)的针织品。针织品基底的厚度应为100-500微米，优选250-400微米。针织品基底的密度应为50-200gm/平方米，优选100-150gm/平方米。由于针织品基底为细网眼针织物设计，其中纤维在采用交织成圈纱线模式的同时纵向编织，其中一侧特征为细罗纹以纵向模式编织，而另一侧的特征为罗纹以交叉方向编织，其在罗纹侧应具有5-30纵行/cm，优选10-15纵行/cm。此外，在针织品的光滑侧，它应具有5-40横列/cm，在本发明中优选15-25横列/cm。“浇铸在针织品上(cast-on-tricot)”的不对称或复合膜的总厚度应为400-800微米，优选500-650微米。根据本发明优选实施方案，“浇铸在针织品上”的膜通过在针织品基底上浇铸聚合物涂布漆从而形成溶液薄层，使该膜在0-25℃，通常优选0℃的低温或环境温度的水中沉淀，然后在25-90℃，通常优选86℃的高温水中退火而制备。干燥膜可通过在或大于上述的环境温度(范围为25-80℃，通常65-70℃)下蒸发水而实现。干燥的“浇铸在针织品上”的不对称膜可用含有2-15重量％，通常优选8-10重量％环氧硅氧烷(epoxy silicone)溶液的环氧硅氧烷溶液涂覆。该硅氧烷溶剂含有比例为1∶1-1∶5，通常优选1∶3的己烷和庚烷溶剂。然后使该环氧硅氧烷涂料在环境温度下暴露于UV源1-10分钟，通常优选2-4分钟，从而在硅氧烷溶剂蒸发生产环氧硅氧烷的同时，固化该涂料。得到的“浇铸在针织品上”的不对称和复合膜适用于水由反渗透脱盐、非水液体分离、超滤、纳滤、全蒸发和所有已知的气体分离终端用途。使用针织品作为背衬基底的其他优点包括降低了从进料到渗透侧的压降；增加了螺旋缠绕型模件的填充密度，最小化了在使用布织物中遇到的膜卷曲问题以及降低了制备该膜的材料成本。
与由Dutton US 0034294A1所教导的将针织品在螺旋缠绕型膜的模件设置中用作渗透隔板不同，在本发明中将针织品在转相方法中用作不对称膜的支撑织物。更重要地是，虽然针织品的光滑侧用于支撑不对称膜，但可将针织品的罗纹侧在螺旋缠绕型或板和框架型结构模件构造中用作渗透隔板。
下列实施例旨在说明本发明的一个或多个优选实施方案，但本发明不限于这些实施方案。可对下列实施例所做的众多变体均属于本发明范围。
实施例1
二乙酸纤维素(CA)&三乙酸纤维素(CTA)不对称膜
由包含(以近似重量百分数计)8％三乙酸纤维素，8％二乙酸纤维素，32％1，3-二氧杂环戊烷，2％NMP，24％丙酮，12％甲醇，2％马来酸和3％正癸烷的浇铸涂布漆制备乙酸纤维素/三乙酸纤维素不对称膜。将薄膜浇铸到针织品网上，然后通过在0℃的水浴中浸没10分钟而胶凝，然后在86℃的热水浴中退火5分钟。使得到的湿膜在70℃的温度下干燥以除去水。用含有2重量％环氧硅氧烷溶液的环氧硅氧烷溶液涂覆干燥的不对称纤维素膜。该硅氧烷溶剂含有比例为1∶3的己烷和庚烷。使该环氧硅氧烷涂料在环境温度下暴露于UV源2-4分钟，从而在该硅氧烷溶剂蒸发的同时，使该涂料固化，由此产生本发明的环氧硅氧烷涂覆膜。
在6.89MPa(1000psig)的进料压力和50℃下使用含有10体积％CO2和90体积％CH4的进料气体对环氧硅氧烷涂覆膜的气体传输性能进行评价。表1显示的是致密膜的CO2渗透性和选择性(α)(固有特性)与不对称膜性能的比较。
表1气体传输性能
  膜   CO2   CO2/CH4的选择性
  致密膜   7.2Barrers＊   21.9
  不对称膜   199(GPU＊＊)   14.2
＊Barrer＝10-10cm3(STP)cm/sec.cm3.cmHg
＊＊气体渗透单元(GPU)＝10-6em3(STP)/cm2sec.cmHg
实施例2
二乙酸纤维素(CA)&三乙酸纤维素(CTA)不对称膜
由包含(以近似重量百分数计)8％三乙酸纤维素，8％二乙酸纤维素，32％1，3-二氧杂环戊烷，2％NMP，24％丙酮，12％甲醇，2％马来酸和3％正癸烷的浇铸涂布漆制备乙酸纤维素/三乙酸纤维素不对称膜。将薄膜浇铸到针织品网上，然后通过在0℃的水浴中浸没10分钟而胶凝，然后在86℃的热水浴中退火5分钟。使得到的湿膜在70℃的温度下干燥以除去水。表2显示的是致密膜的CO2渗透性和选择性(α)(固有特性)与不对称膜性能的比较。
表2气体传输性能
  膜   CO2   CO2/CH4的选择性
  致密膜   7.2Barrers＊   21.9＊
  不对称膜   53GPU   14.9
＊致密膜在690kPa(100psig)，50℃和纯气体下测试。
实施例3
P84聚酰亚胺/聚醚砜共混的不对称膜
由包含(以近似重量百分数计)6.5％聚醚砜，12.2％P84聚酰亚胺，50.5％1，3-二氧杂环戊烷，24.3％NMP，3.7％丙酮和2.8％甲醇的浇铸涂布漆制备P84聚酰亚胺/聚醚砜共混的不对称膜。将薄膜浇铸到针织品网上，然后通过在0℃的水浴中浸没10分钟而胶凝，然后在86℃的热水浴中退火5分钟。使得到的湿膜在65-70℃的温度下干燥以除去水。用含有8重量％环氧硅氧烷溶液的环氧硅氧烷溶液涂覆干燥的不对称膜。该硅氧烷溶剂具有比例为1∶3的己烷和庚烷。使该环氧硅氧烷涂料在环境温度下暴露于UV源2-4分钟，在该硅氧烷溶剂蒸发同时，使该涂料固化，从而产生本发明的环氧硅氧烷涂覆膜。
在6.89MPa(1000psig)的进料压力和50℃下使用含有10体积％CO2和90体积％CH4的进料气体对环氧硅氧烷涂覆膜的气体传输性能进行评价。表3显示的是致密膜的CO2渗透性和选择性(α)(固有特性)与不对称膜性能的比较。表3显示的是致密膜的CO2渗透性和选择性(α)(固有特性)与不对称膜性能的比较。
表3气体传输性能
  膜   CO2   CO2/CH4的选择性
  致密膜   2.7Barrers＊   33.7＊
  不对称膜   51GPU   24.7
＊致密膜在690kPa(100psig)，50℃和纯气体下测试。

Claims (10)

1.一种制备膜的方法，包括将聚合物溶液施加到织物片材的一侧和在所述聚合物溶液施加之后从所述聚合物溶液中除去溶剂成分，其中所述织物包含一系列在一个方向上交联的线圈和在垂直方向上的线圈线。
2.根据权利要求1的方法，其中所述聚合物选自聚砜、聚醚砜、聚醚酰亚胺、纤维素聚合物、聚酰胺、聚酰亚胺、聚酰胺/酰亚胺、聚醚酮、聚醚醚酮、聚亚芳基氧、聚(酯酰胺-二异氰酸酯)、聚氨酯、聚苯并苯并咪唑、聚酰肼、聚
Figure FDA0000051839830000011
二唑、聚***、聚苯并咪唑、聚碳二亚胺、聚膦嗪、微孔聚合物、聚硅氧烷、聚丙烯腈、聚甲基丙烯腈、聚乙烯醇、聚硫化物、聚苯并
Figure FDA0000051839830000012
唑、聚偏二氟乙烯及其混合物。
3.根据权利要求1的方法，其中所述织物片材已经用水基环氧化物层涂覆且热交联。
4.根据权利要求3的方法，其中所述环氧化物为双酚A。
5.根据权利要求2的方法，其中所述纤维素聚合物包括二乙酸纤维素或三乙酸纤维素。
6.根据权利要求2的方法，其中所述聚合物包括聚酰亚胺。
7.根据权利要求6的方法，其中所述聚合物另外包括聚砜。
8.根据权利要求1的方法，其中所述织物片材为针织品织物。
9.根据权利要求1的方法，其另外包括施加可UV辐射交联涂料到所述聚合物上，然后使所述可UV辐射交联涂料交联。
10.一种由权利要求1-9中任一项的方法制备的不对称膜。
CN2009801375064A 2008-09-25 2009-08-04 浇铸在针织品上的不对称和复合分离膜 Pending CN102164658A (zh)

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