CN106378010B - 一种含壳聚糖季铵盐的吸附超滤膜及制备方法 - Google Patents
一种含壳聚糖季铵盐的吸附超滤膜及制备方法 Download PDFInfo
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Abstract
本发明提供了一种含壳聚糖季铵盐的吸附超滤膜及制备方法。所述的含壳聚糖季铵盐的吸附超滤膜包含交联壳聚糖季铵盐(3‑50wt%)和聚合物(97‑‑50wt%)。其制备方法为:将溶剂、致孔剂、交联壳聚糖季铵盐和聚合物混合,搅拌待聚合物溶解后,采用浸没沉淀相转化法制备具有吸附功能的超滤膜。该超滤膜可用于水质净化,以除去水中的大分子、胶体和有害的阴离子,具有吸附快、再生效果好的特点。
Description
技术领域:
本发明涉及到化学工程领域,具体涉及到一种含壳聚糖季铵盐的吸附超滤膜及制备方法。
背景技术:
水体中通常含有一些有害或有毒的物质,如阴离子表面活性剂、铬酸根、亚砷酸根、硝酸根、腐殖酸、氟离子和染料等。采用混凝、絮凝和超滤等常规方法难以除去,而吸附、纳滤和反渗透虽可以除去,但运行成本高。超滤膜孔径在2~50 nm范围,远大于一般的离子;直接使用超滤不能除去这些有毒有害物质。为了除去这些有害或有毒的离子,采用胶束强化超滤和聚合物强化超滤的方法能达到很好的除去效果,但胶束和所加的聚合物后处理难,限制了其应用。吸附膜是将吸附与膜分离相结合,具有去除率高、处理能力强、吸附速度快、可重复使用的特点.将膜吸附和膜分离有机结合,可强化超滤过程对水质的净化效果。包一翔等人做出的氨基化MCM-41介孔分子筛改性超滤膜去除水中Cr(VI)的研究,【华南师范大学学报(自然科学版), 2015,47(6):58—62.】采用氨基化介孔分子筛(NHMCM-41)接枝改性聚偏氟乙烯(PVDF)制备了超滤膜,并研究了其除水中重金属Cr(VI)的效果。
壳聚糖季铵盐是指在壳聚糖的氨基上通过引入基团转换成季铵盐或者把一个低分子季铵盐接到氨基上而得到的一类壳聚糖衍生物,其溶解性和pH 值适应范围均比壳聚糖有所提高,而且壳聚糖季铵盐的正电性和阳离子强度也大大提高,对水体中阴离子的吸附具有更宽的适用范围和更好的吸附效果,是一种环境友好的吸附材料。
壳聚糖季铵盐是一种良好的吸附材料,大量文献报道其可用于除去水体中的有害离子。多数壳聚糖季铵盐溶于水的,但吸附剂需要反复循环使用,不溶于水更便于回收利用。不溶于水的壳聚糖季铵盐通常采用交联法制得,交联剂主要为戊二醛、甲醛和环氧氯丙烷【谢燕华等人做出的改性壳聚糖季铵盐的研制及其对高氯酸盐的吸附研究,环境科学,2011,32(9):2537-2542】,可在水、乙醇或乳液等介质中交联制得。如魏峣等人做出的交联壳聚糖季铵盐对水体中硝酸盐的吸附去除研究,【水处理技术,2012,38(9):21-24】在乙醇中用戊二醛交联制备了交联壳聚糖季铵盐,研究了其对水体中的硝酸根离子吸附,在10分钟可以达到吸附平衡,共存离子的影响顺序为Cl->SO4 2-> HCO3 -,采用1%的氯化钠再生。沈俊菊等人做出的季铵化壳聚糖微球的制备及其对酸性媒介黑PV的吸附性能研究,【山西师范大学学报(自然科学版),2009,23(3):43-48.】先用甲醛保护氨基制备交联的壳聚糖,然后脱甲醛,再季铵化,制备直径在0.20-0.35微米的季铵盐壳微球。周耀珍等人做出的交联壳聚糖季铵盐吸附剂的制备及其对重金属离子的吸附,【化工环保,2014,34(2):170-175】 以壳聚糖为原料、DMDAAC为接枝单体、甲醛为预交联剂、环氧氯丙烷为交联剂,通过反相乳液聚合制备出交联壳聚糖季铵盐吸附剂,研究了交联壳聚糖季铵盐对Ni(Ⅱ)和Cr(Ⅵ)的吸附效果,采用1mol/L的盐酸再生。池伟林等人做出的壳聚糖/壳聚糖季铵盐共混微球吸附五氯酚钠的报道【孝感学院学报,2008,28(3):38-41】将壳聚糖与壳聚糖季铵盐按不同比例溶于酸性水液液中,采用环氧氯丙烷交联,研究了交联微球对农药五氯酚钠的吸附效果,采用3%的盐酸与氢氧化钠再生可恢复吸附剂的吸附能力。黄晓东等人做出的季铵盐壳聚糖膜对水体中十二烷基苯磺酸钠吸附的研究,【环境科学与技术,2012,35(11):65-69. 】将壳聚糖季铵盐在溶于醋酸水溶液中后用戊二醛交联后制膜,研究了其对十二烷基苯磺酸钠的吸附。
利用壳聚糖季铵盐制备吸附超滤膜未见文献报道。
发明内容:
本发明目的在于提供一种含壳聚糖季铵盐的吸附超滤膜及制备方法。为实现该目的,采用浸没沉淀相转化制备吸附超滤膜。
为实现上述目的,本发明的技术方案为
一种含壳聚糖季铵盐的吸附超滤膜,其特征在于:所述的吸附超滤膜包含交联壳聚糖季铵盐(3-50wt%)和聚合物(97--50wt%)。
所述的聚合物为聚偏氟乙烯、聚氯乙烯、聚砜、聚醚砜、醋酸纤维素和聚丙烯腈中的任意一种或任意比例的几种。
所述的交联壳聚糖季铵盐不溶于水,交联剂采用戊二醛或环氧氯丙烷中的一种。
所述吸附超滤膜具有中空纤维、平板和卷式等结构形式,能用于水质净化,除去水中的大分子、胶体和阴离子染料、溴酸根、腐殖酸、砷酸根、高氯酸跟、铬酸根、硝酸根、硫酸根和阴离子表面活性剂等各种阴离子。
一种含壳聚糖季铵盐的吸附超滤膜的制备方法,所述方法按以下步骤进行:
1、按重量百分比分别取30-88%溶剂、0-15%致孔剂、0.37-35%交联壳聚糖季铵盐和12-35%聚合物混合、搅拌,在50-80℃恒温12-36小时,得到聚合物溶液;
2、以水或水溶液为凝胶介质,将上述聚合物溶液通过浸没沉淀法纺丝或涂敷的方法制备超滤膜,凝胶时间控制在12-48小时。
所述的溶剂为N-N二甲基甲酰胺、N-N二甲基乙酰胺、二甲亚砜、N-甲基吡咯烷酮和四氢呋喃中的任意一种或任意比例的几种;所述的致孔剂为聚乙二醇和聚乙烯吡咯烷酮中的一种或两种;所述的水溶液为一定量溶剂的水溶液,水溶液中的溶剂与上述溶剂相同,其浓度在(0-80wt%)之间,在凝胶浴中加入一定量溶剂是调控超滤膜微观结构的一种手段。
本发明的积极效果为
1、本发明所制备的壳聚糖季铵盐吸附超滤膜,壳聚糖季铵盐在凝胶固化时被牢固地固定在微粒中;
2、由于壳聚糖季铵盐是一种亲水性强的物质,在水中凝胶时会向微粒表面迁移进而主要固定在微粒表面或孔通道的表面;
3、本发明提供的含壳聚糖季铵盐的吸附超滤膜及制备方法,所制超滤膜在除去水中大分子和胶体等物质的同时,可以有效除去水中有毒、有害的各种阴离子。
具体的实施方式
实施例1:
取14.5g聚乙烯比咯烷酮(K30)溶解于150mL N-N二甲基乙酰胺,加入不同质量交联的壳聚糖季铵盐(QCS),搅拌15分钟后,再将51.8g的聚醚砜加入到溶液中,在电热恒温干燥箱60℃下溶解12-36小时。
以水作为凝胶剂,在室温下刮膜,蒸发30s后放入水中凝胶12-48小时,膜的组成见表1。在0.10MPa下预压10分钟测定膜的纯水渗透通量(J0),用200mg/L的牛血清蛋白质水溶液测定其截留率(R0),然后用铬(VI)离子初始浓度为(1.0±0.1) mg /L的水溶液进行过滤试验,每5min取50mL透过液测定铬(VI)离子的浓度,多余透过液加入到原水箱,实验时间为两小时,并取5分钟与120分钟的浓缩液各50mL测定铬离子浓度(540nm,分光光度法测定);实验结束后用1M的氯化钠水溶液再生1.5小时,水洗后,重复实验。表2、表3分别给出了含5.0wt%和7.5wt%壳聚糖季铵盐膜过滤含铬水时透过液中铬离子浓度随时间的变化;表4给出了不同壳聚糖季铵盐含量膜过滤开始5分钟时对铬离子去除率及再生效果。
表1:聚醚砜膜中交联壳聚糖季铵盐的含量及膜的初始性能
表2:含5wt%壳聚糖季铵盐超滤膜过滤(1.0±0.1) mg /L含铬水溶液时透过液中铬离子浓度
表3:含7.5wt%壳聚糖季铵盐超滤膜过滤(1.0±0.1) mg /L含铬水溶液时透过液中铬离子浓度
表4:不同壳聚糖季铵盐含量膜过滤开始5分钟时对铬离子去除率及再生效果
实施例2
取10.0g聚乙二醇(600)溶解于110mL N-甲基吡咯烷酮,加入不同质量交联的壳聚糖季铵盐(QCS),搅拌15分钟后,再将20.0g的聚偏氟乙烯加入到溶液中,在电热恒温干燥箱70℃下溶解18小时。
以水作为凝胶剂,在室温下刮膜,蒸发20秒后放入水中凝胶30小时,膜的组成见表5。在0.10MPa下预压10分钟测定膜的纯水渗透通量(J0),用200mg/L的牛血清蛋白质水溶液测定其截留率(R0),然后用初始浓度为(0.50±0.01) mg /L的十二烷基硫酸钠水溶液进行过滤试验,取10分钟内的透过液测定十二烷基硫酸钠浓度,计算去除率[(初始浓度-透过液浓度)/初始浓度](R表),(见表5最后一栏)。
表5:膜中壳聚糖季铵盐的含量及膜的初始性能
实施例3
取0.37g 壳聚糖季铵盐和12.0g聚砜加入到装有87.64g N-N二甲基甲酰胺(DMF)的碘量瓶中,在电热恒温干燥箱50℃下溶解24小时。以含70wt% N-N二甲基甲酰胺的水溶液作为凝胶剂,在室温下刮膜,蒸发40秒后放入含70wt% N-N二甲基甲酰胺的水溶液凝胶36小时,然后再放入水中浸泡24小时得到超滤膜,其对牛血清蛋白的截留率为97.4%,纯水渗透通量为56.6L.m-2.h-1,其过滤含铅离子(3 mg /L)、铜离子(8 mg /L)和铝离子(15 mg /L)的水溶液时,10分钟时对Pb2、Cu2+和 Al3+的截留率分别为64.2%、58.7%和87.6%。
本说明书中公开的所有特征,或公开的所有方法或过程中的步骤,除了互相排斥的特征和/或步骤以外,均可以以任何方式组合。本说明书(包括任何附加权利要求、摘要)中公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换。即,除非特别叙述,每个特征只是一系列等效或类似特征中的一个例子而已。
以上所述仅是发明的非限定实施方式,还可以衍生出大量的实施例,对于本领域的普通技术人员来说,在不脱离本发明创造构思和不作出创造性劳动的前提下,还可以做出若干变形和改进的实施例,这些都属于本发明的保护范围。
Claims (2)
1.一种含壳聚糖季铵盐的吸附超滤膜的制备方法,其特征在于:所述方法按以下步骤进行:
(1)按重量百分比分别取30-88%溶剂和0-15%致孔剂、0.37-35%交联壳聚糖季铵盐和12-35%聚合物混合、搅拌,在50-80℃恒温12-36小时,得到聚合物溶液,其中聚合物为聚偏氟乙烯、聚氯乙烯、聚醚砜、醋酸纤维素和聚丙烯腈中的任意一种或几种;
(2)以水或水溶液为凝胶介质,将上述聚合物溶液通过浸没沉淀法纺丝或涂敷的方法制备超滤膜,凝胶时间控制在12-48小时。
2.根据权利要求1所述的含壳聚糖季铵盐的吸附剂的制备方法,其特征在于:所述方法步骤(1)中的溶剂为:N-N二甲基甲酰胺、N-N二甲基乙酰胺、二甲亚砜、N-甲基吡咯烷酮和四氢呋喃中的任意一种或几种;步骤(1)中所述的致孔剂为:聚乙二醇和聚乙烯吡咯烷酮中的一种或两种;步骤(2)中所述的水溶液为定量溶剂的水溶液,水溶液中的溶剂与上述溶剂相同,浓度在0-80wt%之间。
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