CN114044918A - 一种多孔结构的假酸浆胶/聚乙烯醇复合水凝胶的制备方法 - Google Patents
一种多孔结构的假酸浆胶/聚乙烯醇复合水凝胶的制备方法 Download PDFInfo
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Abstract
本发明公开了一种多孔结构的假酸浆胶/聚乙烯醇双网络复合水凝胶的制备方法,所述水凝胶制备原料质量比如下:假酸浆胶:聚乙烯醇:去离子水:戊二醛:钙离子:盐酸=0.001‑0.05g:0.95‑0.999g:6‑10g:50‑200μL:10‑600μL:100‑600μL。本发明多孔双网络水凝胶在太阳能净水技术中表现出稳定的脱盐效能和优异污水处理能力。
Description
技术领域
本发明属于双网络水凝胶材料的制备领域,特别涉及一种多孔结构的假酸浆胶/聚乙烯醇双网络水凝胶的制备方法。
背景技术
淡水是人类生存和发展不可或缺的资源,但目前全球正面临着日益严重的淡水资源危机。海水淡化或污水处理是目前获得淡水的有效途径,常用技术有反渗透、离子交换膜和膜蒸馏等。但以上净水技术往往面临着高能耗,难清洁,成本高等问题。因此,迫切需要开发高效、经济、可规模化的技术来实现海水淡化或污水处理。太阳能是一种储量大、来源广和易采集的绿色可再生能源,由太阳能驱动的水净化技术有着低能耗,自清洁,低成本等优点,而水凝胶界面光蒸发技术将热能控制在了水-空气界面,有效降低了净水能耗。其中水凝胶是界面光蒸发技术的核心材料,它具有物理或化学交联的聚合物网络,自身大量的功能基团可与水分子结合,为水分子的传输提供通道并有效降低水的蒸发焓,从而构成内部持续输水-界面低耗蒸馏的良性循环。
但传统水凝胶用于界面光蒸发还面临两大问题,一是一般水凝胶自身的光吸收能力较弱,二是其输水和锁水功能不够理想,导致蒸发速率较低。针对以上问题,本发明在水凝胶聚合物网络中嵌入具有高效光吸收能力和热转化能力的光吸收材料,并引入生物质高锁水材料假酸浆胶,以制备一种用于高效海水淡化或污水处理的新型多孔结构双网络复合水凝胶。
发明内容
1.本发明提供一种双网络复合水凝胶的制备方法,将物理交联与化学交联结合起来。通过碳正离子聚合形成凝胶骨架,同时引入钙离子实现协同配位,形成一种均匀多孔的双网络水凝胶。
2.本发明的一种多孔双网络水凝胶制备方法,包括:
(1)碳正离子缩合反应和钙离子交联作用共同制备得到复合水凝胶;
(2)将上述的复合水凝胶,在去离子水中浸泡24h,然后再用液氮反复冻融10次,得到多孔双网络水凝胶。
3.所述步骤(1)中碳正离子缩合反应和钙离子交联具体为:
将假酸浆胶,聚乙烯醇溶于水中,加入聚吡咯、戊二醛搅拌超声混合均匀后,加入盐酸和氯化钙溶液,再搅拌均匀;然后将混合溶液进行注模密封,放置凝胶,得到复合水凝胶;
其中,假酸浆胶:聚乙烯醇:去离子水按质量比为:0.001-0.05g:0.95-0.999g:6-10g。混合溶液中氯化钙(30wt%)10-600μL;戊二醛(50wt%)为50-200μL;盐酸(1.2mol/L)为100-600μL;聚吡咯质量浓度为10%。
4.所述步骤(1)假酸浆胶(冰粉)由假酸浆籽(冰粉籽)通过60℃水提法经过冷冻干燥得到。
5.所述步骤(1)聚乙烯醇溶解温度为30-80℃,时间为2h。
6.所述步骤(1)凝胶的反应温度为室温,反应时间为1-12h。
7.所述步骤(2)去离子水浸泡是为除去多余离子。
8.所述步骤(2)液氮冻融过程,溶解温度为30℃水浴。
9、本发明的一种所述方法制备多孔结构双网络水凝胶。
10、本发明还提供一种太阳能净化技术,所述太阳能净化材料为所述的多孔结构双网络水凝胶。
11、本发明提供一种所述多孔结构的双网络水凝胶在海水淡化、污水处理中的应用。
12、本发明的有益效果:
本发明的制备方法将物理交联与化学交联的网络结合起来,以聚乙烯醇聚合物链作为骨架,形成紧密的网络结构,通过钙离子交联假酸浆胶链,与聚乙烯醇链相互缠结形成物理交联点,合成壁面光滑、壁厚均匀的多孔双网络水凝胶。假酸浆胶/聚乙烯醇双网络水凝胶中含氧官能团不仅能与水形成氢键,形成更多的中间水团簇,降低水的蒸发焓;还能增强对废水中的金属离子和有机污染物的截留能力。
附图说明
图1是实施例1合成的聚乙烯醇水凝胶SEM照片;
图2是实施例3合成的假酸浆胶/聚乙烯醇双网络水凝胶SEM图。
具体实施方式
下面结合附图和实施例对本发明做进一步说明。
实施例1
加入1g聚乙烯醇60℃溶解后,搅拌至溶液均匀稳定后。加入125μL戊二醛和100 μL聚吡咯溶液,超声混合均匀后,搅拌加入500μL盐酸溶液和100μL氯化钙溶液。将混合溶液注模密封,室温凝胶2h后,去离子水浸泡24h得到水凝胶。将水凝胶经液氮冷冻, 30℃水浴解冻,反复冻融10次得到聚乙烯醇水凝胶。
实施例2
首先将0.005g假酸浆胶粉40℃溶于10mL去离子水中。再加入0.995g聚乙烯醇70℃溶解后,搅拌至溶液均匀稳定后。加入125μL戊二醛和100μL聚吡咯溶液,超声混合均匀后,搅拌加入500μL盐酸溶液和100μL氯化钙溶液。将混合溶液注模密封,室温凝胶2h后,去离子水浸泡24h得到复合水凝胶。将复合水凝胶经液氮冷冻,30℃水浴解冻,反复冻融10次得到双网络水凝胶。
实施例3
首先将0.025g假酸浆胶粉50℃溶于10mL去离子水中。再加入0.975g聚乙烯醇50℃溶解后,搅拌至溶液均匀稳定后。加入125μL戊二醛和100μL聚吡咯溶液,超声混合均匀后,搅拌加入500μL盐酸溶液和100μL氯化钙溶液。将混合溶液注模密封,室温凝胶 2h后,去离子水浸泡24h得到复合水凝胶。将复合水凝胶经液氮冷冻,30℃水浴解冻,反复冻融10次得到均匀多孔双网络水凝胶。
实施例4
首先将0.025g假酸浆胶粉60℃溶于10mL去离子水中。再加入0.975g聚乙烯醇40℃溶解后,搅拌至溶液均匀稳定后。加入100μL戊二醛和100μL聚吡咯溶液,超声混合均匀后,搅拌加入500μL盐酸溶液和100μL氯化钙溶液。将混合溶液注模密封,室温凝胶 2h后,去离子水浸泡24h得到复合水凝胶。将复合水凝胶经液氮冷冻,30℃水浴解冻,反复冻融10次得到双网络水凝胶。
综上所述,通过添加比例的假酸浆胶与聚乙烯醇比例,进行聚合反应,冻融后得到的水凝胶进行力学性能测试、冻干样品的扫描电镜测试、傅里叶红外光谱分析、热重分析,以及实验的验证,然后进行对比,可得实施例3为最佳方案,实施例3中投入的假酸浆胶与聚乙烯醇的质量比为0.025:0.975为最佳方案,因此水凝胶的制备方案为实施例3.
以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属于本发明涵盖的范围内。
Claims (10)
1.一种内部为多孔结构的复合水凝胶,其特征在于所述水凝胶内部为具有多孔结构的假酸浆胶/聚乙烯醇复合水凝胶。
2.一种内部为多孔结构的复合水凝胶的制备方法,包括:
(1)钙离子配位作用与碳正离子缩合反应制备得到假酸浆胶/聚乙烯醇水凝胶。
(2)将上述聚合得到的假酸浆胶/聚乙烯醇水凝胶在去离子水中浸泡24h,进行液氮反复冻融10次,得到内部多孔的复合水凝胶。
3.根据权利要求2所述制备方法,其特征在于,所述步骤中钙离子配位作用和碳正离子聚合反应具体为:
将假酸浆胶:聚乙烯醇:去离子水按质量比为:0.001-0.05g:0.95-0.999g:6-10g,溶于水中搅拌,得到均匀溶液后,加入聚吡咯,戊二醛超声分散均匀,再加入氯化钙溶液和盐酸,然后将混合溶液进行注模,密封进行凝胶反应得到水凝胶。
4.根据专利要求3所述制备方法特征在于,所述凝胶反应温度在室温,反应时间为1-12h。
5.根据专利要求3所述制备方法特征在于,假酸浆胶(冰粉)由假酸浆籽(冰粉籽)通过30-90℃水提法经过冷冻干燥得到。
6.根据专利要求3所述制备方法特征在于,聚乙烯醇溶解温度为30-80℃,溶解时间为2h。
7.根据专利要求3所述制备方法特征在于,钙离子质量浓度为30%。
8.一种权利要求2所述方法制备得到多孔结构的复合水凝胶。
9.一种太阳能水净化材料,其特征在于,所述太阳能水净化所用材料用于海水碳化、污水处理为专利要求8所述的多孔复合水凝胶。
10.一种权利要求9所述多孔水凝胶的应用。
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