CN106925141B - 一种隔氧光引发水凝胶复合膜的制备方法 - Google Patents
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Abstract
本发明公开了一种新型隔氧光引发水凝胶复合膜的制备方法,属于膜科学与技术领域。将聚乙二醇双丙烯酸酯、N‐异丙基丙烯酰胺、光引发剂制备成复合膜的涂膜预聚物;选取基膜材料及尺寸,并将其进行预处理;本发明的制备方法制备了具有3D网格结构的柔性水凝胶复合膜。新型隔氧光引发水凝胶复合膜制膜方法不仅解决了复合膜表面功能层均匀铺展的问题,还提供了隔氧条件促进了交联反应,另外新型制膜方法对复合层厚度可控,进一步增大了复合膜界面牢固性。并且该复合膜的制备方法简单,成本低廉,为今后复合膜的合成提供了一种新的思路。
Description
技术领域
本发明属于膜科学与技术领域,涉及一种隔氧光引发水凝胶复合膜的制备方法。
背景技术
复合膜是以微孔膜或超滤膜作支撑层,在其表面覆盖以厚度仅为0.1~0.25微米的均质膜作皮层构成的分离膜。在膜科学领域,膜制备的方法有很多种,例如,(1)层压法,首先制备很薄的致密均质膜,而后层压于微孔支撑层上。(2)浸涂法,把聚合物溶液浸涂于微孔膜上,然后干燥而成,也可以把活性单体或预聚物溶液浸涂于微孔膜上,用热或辐射固化。(3)等离子体气相沉积法,用等离子辉光使微孔支撑膜的表面产生致密的均质膜。(4)界面聚合法,在微孔支撑膜表面上,用活性单体进行界面聚合等等。不同的制备方法适合不同的制膜体系。
膜结晶技术是化工分离以及膜科学领域中的一种新型技术,它的基本原理是通过膜蒸馏来去除溶液中的溶剂到达过饱和状态,从而完成浓缩结晶的目的。尤其在结晶困难的生物大分子蛋白质领域,膜结晶有其独特的优势及特点。为了解蛋白质的具体功能和作用机制,需在原子分辨率水平下观察三维结构,蛋白质晶体三维结构的确定对于了解其分子功能和设计病理学中有特殊靶点的新型药物有着重要的作用。目前,能否获得高质量适合于X射线衍射的晶体是确定蛋白质三维结构的主要瓶颈。
现阶段对于蛋白质膜结晶的研究仅仅局限在商业用膜领域,膜改性方面的研究尚未出现。将膜结晶用膜进行改性可以促进非均相成核进行,根据蛋白质结构不同,可利用不同的改性手段和改性材料,促进多种晶型的晶体形成,并且尽可能增大晶体尺寸,降低诱导时间,减小初始浓度,从而降低了蛋白质的结晶难度,提升了膜结晶的生产效率和晶型多样性。膜改性的探索对生物大分子蛋白质膜结晶有很大的发展空间和研究意义。
水凝胶是一种具有3D网格结构的柔性聚合物材料,由于它独特的网格结构而具有溶胀通透性,通过改变单体和交联剂的种类和比例合成不同性能不同网格尺寸的水凝胶。水凝胶涂覆在PP,PVDF等机械强度好的疏水微孔膜可形成对蛋白质结晶有促进作用的水凝胶复合膜,网格结构的存在可促进蛋白质结晶成核,降低蛋白质的初始浓度,增大蛋白质结晶尺寸,对蛋白质结晶有很重要的意义。
发明内容
本发明提出一种隔氧光引发水凝胶复合膜制膜方法。本方法是在商业膜作为基膜的条件下,利用玻璃板,基膜,预聚物三者形成的整体解决疏水性基膜和亲水性预聚物的不亲和问题、水凝胶复合膜表面的均匀铺展问题以及预聚物交联反应所需的隔氧问题。通过引入新的制膜方法,解决了水凝胶复合膜制备过程的三大问题。
本发明的技术方案:
一种隔氧光引发水凝胶复合膜的制备方法,步骤如下:
(1)将聚乙二醇双丙烯酸酯和N-异丙基丙烯酰胺按照摩尔比为5~50:1混合,形成复合膜涂膜预聚物;再加入复合膜涂膜预聚物质量分数为0.1~2%的光引发剂,搅拌至溶解完全,得到预聚物;其中,聚乙二醇双丙烯酸酯中聚乙二醇的分子量为400或200;
(2)选取基膜材料及尺寸,预处理;
(3)将步骤(1)得到的预聚物均匀滴加到玻璃板表面,再将裁剪好的基膜覆盖于预聚物上,使用滚筒在基膜表面来回滚动,使玻璃板和基膜之间的预聚物均匀铺展,并达到隔氧状态;将玻璃板、预聚物、基膜三者形成的整体置于紫外灯下进行紫外光照射交联10~60min,反应完全即得水凝胶复合膜;将水凝胶复合膜洗涤,在30~70℃温度条件下干燥,直至水凝胶复合膜质量不再变化。
所述的光引发剂为适用于不饱和聚酯的水性体系并且具有较低挥发度和气味的光引发剂,进一步确定为Irgacure2959。
所述的基膜材料为平板膜、有机膜和无机膜,进一步,有机膜包括PTFE(聚四氟乙烯)、PVDF(聚偏氟乙烯)、PEI(聚醚酰亚胺)、PVA(聚乙烯醇)、PVC(聚氯乙烯)、PVF(聚氟乙烯)、PE(聚乙烯)、PP(聚丙烯)、PI(聚酰亚胺)、PU(聚氨酯)和CA(醋酸纤维素);无机膜包括陶瓷膜、沸石膜、金属氧化物膜和NaA型分子筛膜。
所用的紫外灯是一种低压汞灯,利用低压汞蒸汽(<10-2Pa)被激发后发射紫外线。
本发明的有益效果:
(1)新的制膜方法解决了亲水性预聚物不能在疏水性基膜上均匀铺展的问题,制得了具有均匀表面功能层的水凝胶复合膜;
(2)新的制膜方法提供了预聚物交联需要的隔氧环境,不需要引入其他隔氧预处理步骤,简化了制膜过程和制膜装置;
(3)新的制膜方法可以通过改变预聚物体积、紫外光强度和照射时间便捷地控制复合层厚度和结合强度。
具体实施方式
以下结合技术方案,进一步说明本发明的具体实施方式。
实施例1
制备水凝胶复合膜预聚物,聚乙二醇双丙烯酸酯:N-异丙基丙烯酰胺=5:1的摩尔比,加入质量分数为2%的光引发剂Irgacure2959,磁力搅拌直至溶解完全,得到涂膜预聚物。其中,聚乙二醇双丙烯酸酯中聚乙二醇的分子量为400。
选取基膜材料及尺寸:选用面积为10×10cm2的PP平板膜为基膜。
将洗净的玻璃板平整放于桌面,将所配置的预聚物用滴管取2ml,均匀滴加在玻璃板表面。
将裁剪好的基膜覆盖于预聚物上,使用滚筒在基膜表面来回滚动,使玻璃板和基膜之间的预聚物能均匀平整地铺展,此时三者形成的整体已经达到隔氧条件。
将玻璃板、预聚物、基膜三者形成的整体使基膜在上置于紫外灯365nm波长下进行紫外光照射交联30min,反应完全。
取出已完成交联反应的水凝胶复合膜,将水凝胶复合膜置于去离子水中洗涤从而去除光引发剂。洗涤干净后置于烘箱中50℃烘干,直至水凝胶复合膜质量不再变化。
实施例2
制备水凝胶复合膜预聚物,聚乙二醇(200)双丙烯酸酯:N-异丙基丙烯酰胺=10:1的摩尔比,加入质量分数为2%的光引发剂Irgacure2959,磁力搅拌直至溶解完全,得到涂膜预聚物。其中,聚乙二醇双丙烯酸酯中聚乙二醇的分子量为200。
选取基膜材料及尺寸:选用面积为10×10cm2的PP平板膜为基膜。
将洗净的玻璃板平整放于桌面,将所配置的预聚物用滴管取2ml,均匀滴加在玻璃板表面。
将裁剪好的基膜覆盖于预聚物上,使用滚筒在基膜表面来回滚动,使玻璃板和基膜之间的预聚物能均匀平整地铺展,此时三者形成的整体已经达到隔氧条件。
将玻璃板、预聚物、基膜三者形成的整体使玻璃板在上置于紫外灯365nm波长下进行紫外光照射交联30min,反应完全。
取出已完成交联反应的水凝胶复合膜,将水凝胶复合膜置于去离子水中洗涤从而去除光引发剂。洗涤干净后置于烘箱中60℃烘干,直至水凝胶复合膜质量不再变化。
Claims (6)
1.一种隔氧光引发水凝胶复合膜的制备方法,其特征在于,步骤如下:
(1)将聚乙二醇双丙烯酸酯和N-异丙基丙烯酰胺按照摩尔比为5~50:1混合,形成复合膜涂膜预聚物;再加入复合膜涂膜预聚物的质量分数为0.1~2%的光引发剂,搅拌至溶解完全,得到预聚物;其中,聚乙二醇双丙烯酸酯中聚乙二醇的分子量为400或200;
(2)选取基膜材料及尺寸,预处理;
(3)将步骤(1)得到的预聚物均匀滴加到玻璃板表面,再将裁剪好的基膜覆盖于预聚物上,使用滚筒在基膜表面来回滚动,使玻璃板和基膜之间的预聚物均匀铺展,并达到隔氧状态;将玻璃板、预聚物、基膜三者形成的整体置于紫外灯下进行紫外光照射交联10~60min,反应完全即得水凝胶复合膜;将水凝胶复合膜洗涤,在30~70℃温度条件下干燥,直至水凝胶复合膜质量不再变化。
2.根据权利要求1所述的制备方法,其特征在于,所述的光引发剂为适用于不饱和聚酯的水性体系并且具有较低挥发度和气味的光引发剂。
3.根据权利要求2所述的制备方法,其特征在于,所述的光引发剂为Irgacure2959。
4.根据权利要求1-3任一所述的制备方法,其特征在于,所述的基膜材料为有机膜或无机膜。
5.根据权利要求4所述的制备方法,其特征在于,所述的有机膜,包括PTFE、PVDF、PEI、PVA、PVC、PVF、PE、PP、PI、PU和CA;所述的无机膜,包括陶瓷膜、沸石膜、金属氧化物膜。
6.根据权利要求5所述的制备方法,其特征在于,所述的沸石膜为NaA型分子筛膜。
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