CN110305232A - 一种基于改性凝胶多糖的吸水材料及其制备方法 - Google Patents
一种基于改性凝胶多糖的吸水材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于改性凝胶多糖的吸水材料及其制备方法,包括凝胶多糖嫁接羧基化合物的改性方法,所嫁接的多羧化合物包括乙二胺四乙酸(EDTA)、次氮基三乙酸(NTA)、柠檬酸(CA)、丁二酸(SA)、丙二酸(MA)、乙二酸(OA)、二乙三胺五乙酸(DTPA)和聚谷氨酸(PGLU)。本发明的产品吸水性能优异,且制备工艺绿色环保。
Description
技术领域
本发明属于多糖类强吸水材料领域,涉及一类以天然多糖为原料的吸水材料及其制备方法,具体为一种基于改性凝胶多糖羧基化的凝胶吸水材料和制备方法。
背景技术
凝胶吸水材料是指具有强吸水和锁水功能的高分子材料,其内部和表面存在强亲水基团。此类材料与通常的海绵、纸纤维及棉布等吸水性能不同,凝胶材料吸水量可以高达自身重量的百倍、甚至千倍,同时自身结构膨胀形成锁水形态的水凝胶。
吸水剂在医疗卫生、农林园艺、土木建筑、日用化工以及环境保护等工农业领域都有广阔的应用前景。传统吸水材料,诸如医疗卫生和日常生活使用的脱脂棉、海绵、餐巾、毛巾等存在着吸水能力小、保水能力差等问题。
近年来,具有较好吸水性和保湿性的高分子材料,作为新型吸水材料的研究与应用得到了较多关注。高分子吸水材料是一种含有羧基、羟基等强亲水性基团的高分子聚合物的交联体,其吸水能力强,吸水量可达自重的几百倍至数千倍,保水性能优异,同时又有良好的加工性能和使用性能。吸水前,高分子链相互靠拢缠在一起,彼此交联成网状结构,从而达到整体上的紧固。与水接触时,因为吸水材料中含有多个亲水基团(如羧基),故首先进行水润湿,然后水分子通过毛细作用及扩散作用渗透到材料中,链上的电离基团在水中电离,同离子之间的静电斥力而使高分子链伸展溶胀。由于电中性要求,反离子不能迁移到高分子外部,其内外部溶液间的离子浓度差形成反渗透压,水在反渗透压的作用下进一步进入吸水材料中,形成水凝胶。
但石油基类高分子材料往往是非环保型的,且生物相溶性差,这些限制了其作为吸水材料的研究与应用,尤其是在医疗卫生领域的应用。因此,寻求天然环保型的高分子材料来替代石油化工产业链中的合成高分子,从而开发出生物兼容性好的环境友好型吸水材料日益受到重视。凝胶多糖是葡聚糖家族典型成员,由D型葡糖糖借β-1,3糖苷键连接而成,主链具有独特的三维螺旋结构,是一种由微生物代谢产生的细胞外多糖。经化学和酶学分析确定,凝胶多糖由葡萄糖在C1和C3位上以β-1,3-糖苷键连接而成的无分支的多糖聚合物,聚合物由300~500个葡萄糖残基组成,其平均聚合度为450,相对分子量大约为74000。由于分子内部的羟基的相互作用与分子间的氢键作用,多糖主链可以形成更为复杂的三维结构。通常状态下,凝胶多糖是以圆环状的小颗粒形式存在,与淀粉的形态类似。凝胶多糖不溶于水,这极大限制了它的应用。凝胶多糖分子中存在大量羟基,因而通过化学改性可在重复单元上引入不同的基团,这些基团的引入不仅可以改善其溶解性,而且会赋予凝胶多糖新的性质与功能。当前凝胶多糖水溶性衍生物已见报道,这为凝胶多糖类吸水材料研究制备研究奠定了充分的基础。
综上所述,传统吸水材料存在吸水能力小、保水能力差等问题,凝胶多糖可作为传统合成高分子材料的替代物,提升吸水材料的环保性和生物相容性,进而提高了吸水材料的应用范围和研究领域。
发明内容
本发明要发布一类强吸水性凝胶多糖吸水材料,并提供一种此吸水材料适合的制备方法。这种制备方法以凝胶多糖为骨架,通过酰胺化反应嫁接乙二胺四乙酸(EDTA)等多羧基的物质,通过一定的生产工艺过程而制备适合用于吸水材料的凝胶多糖衍生物。
本发明要解决的技术问题是由如下方案解决的:一种以凝胶多糖为原料制备吸水材料的方法,首先将凝胶多糖叠氮化后用硼氢化钠还原制得氨基凝胶多糖,再用DIPEA(N,N-二异丙基乙胺)活化嫁接乙二胺四乙酸(EDTA)等多羧基化合物,将多羧基化合物与氨基凝胶多糖混合,搅拌均匀,反应过夜之后将其透析,三天之后冻干,既得产品。
本发明的优点是:1、凝胶多糖属于无色、无味、无毒的天然多糖。2、该吸水材料制备方法简单易行,吸水率高。
所述改性凝胶多糖吸水材料的部分结构式如下:
Cur-NTA | Cur-EDTA |
Cur-CA | Cur-SA |
Cur-MA | Cur-OA |
Cur-DTPA | Cur-PGLU |
附图说明
图1为本发明中凝胶多糖吸水材料Cur-EDTA的傅里叶红外变换图;
图2为本发明中凝胶多糖吸水材料Cur-EDTA的核磁共振图;
图3为本发明中凝胶多糖吸水材料Cur-NTA的傅里叶红外变换图;
图4为本发明中凝胶多糖吸水材料Cur-NTA的核磁共振图;
图5为本发明中凝胶多糖吸水材料Cur-CA/Cur-N3/Curdlan的傅里叶红外变换图;
图6为本发明中凝胶多糖吸水材料Cur-CA的核磁共振图;
图7为本发明中凝胶多糖吸水材料Cur-EDTA的吸水量对比图;
图8为本发明中凝胶多糖吸水材料Cur-NTA的吸水量对比图;
图9为本发明中凝胶多糖吸水材料Cur-CA的吸水量对比图;
具体实施方式
为能进一步了解本发明的发明内容、特点及功效,列举以下实施例,并配合附图详细说明如下:
实施例1:
一种以凝胶多糖和乙二胺四乙酸(EDTA)为原料制备吸水材料的方法,采用以下步骤:
(1)取凝胶多糖(提前真空干燥过夜)0.3g于反应器中,加入DMF溶解,油浴搅拌,使其充分溶解,反应30min,再加入0.93g的NaN3溶液于恒温油浴中搅拌,然后加入三苯基磷和四溴化碳,反应40h,然后用无水甲醇沉淀,分别用无水甲醇,无水乙醇,蒸馏水离心沉淀3次,最后用真空烘箱烘干,即所得样品,记作Cur-N3;
(2)取Cur-N3于反应器中,加入DMSO溶解,然后加入摩尔比12:1的NaBH4,油浴锅恒温搅拌,反应过夜,再加入无水乙醇,反应后,离心洗涤,在透析袋中透析3天,旋蒸冻干,记作Cur-NH2;
(3)先将乙二胺四乙酸(EDTA)于圆底烧瓶中,加入DMSO充分溶解,分别称取EDC(1-(3-二甲氨基丙基)-3-乙基碳二亚胺)和NHS(N-羟基琥珀酰亚胺),将二者混合加入,再加入DIPEA(N,N-二异丙基乙胺)活化,其中Cur-NH2:EDTA:EDC: NHS:DIPEA=1:2.5:3:3:3(摩尔比),再将(2)中生成的Cur-NH2,氮气保护,反应三天三夜,然后在蒸馏环境中透析,旋蒸冻干,最后生成乳白色水溶性物质,即为所制得吸水材料,记作Cur-EDTA;
(4)请参见图1、图2分别是Cur-EDTA的傅里叶红外变换图和核磁共振谱图,其中傅里叶红外变换图在1716cm-1的羰基伸缩振动峰1662 cm-1的N-H伸缩振动峰,1405 cm-1的C-N的伸缩振动峰以及核磁共振碳谱图中位移为175ppm处为羰基碳的峰,证明成功合成了EDTA改性的凝胶多糖衍生物。同时,此材料具有良好的吸水率,最高可达自身质量的1400倍,使其在可吸水材料上有良好的潜在应用价值。
实施例2:
一种以凝胶多糖和次氮基三乙酸(NTA)为原料制备吸水材料的方法,采用以下步骤:
(1)与实施例1的步骤(1)相同;
(2)与实施例1的步骤(2)相同;
(3)先将次氮基三乙酸(NTA)于圆底烧瓶中,加入DMSO充分溶解,分别称取EDC(1-(3-二甲氨基丙基)-3-乙基碳二亚胺)和NHS(N-羟基琥珀酰亚胺),将二者混合加入,再加入DIPEA(N,N-二异丙基乙胺)活化,其中Cur-NH2:NTA:EDC: NHS:DIPEA=1:2.5:3:3:3(摩尔比),再将(2)中生成的Cur-NH2,氮气保护,反应三天三夜,然后在蒸馏环境中透析,旋蒸冻干,最后生成乳白色水溶性物质,即为所制得吸水材料,记作Cur-NTA;
(4)请参见图3、图4分别是Cur-NTA的傅里叶红外变换图和核磁共振谱图,其中傅里叶红外变换图在1716cm-1的羰基伸缩振动峰1662 cm-1的N-H伸缩振动峰,1405 cm-1的C-N的伸缩振动峰以及核磁共振碳谱图中位移为175ppm处为羰基碳的峰,证明成功合成了NTA改性的凝胶多糖衍生物。上述吸水材料与实施案例1中的吸水材料一样,吸水效果优良,最高吸水量可达自身重量的1500倍,有良好的潜在应用价值。
实施例3:
一种以凝胶多糖和柠檬酸(CA)为原料制备吸水材料的方法,采用以下步骤:
(1)与实施例1的步骤(1)相同;
(2)与实施例1的步骤(2)相同;
(3)先将柠檬酸(CA)于圆底烧瓶中,加入DMSO充分溶解,分别称取EDC(1-(3-二甲氨基丙基)-3-乙基碳二亚胺)和NHS(N-羟基琥珀酰亚胺),将二者混合加入,再加入DIPEA(N,N-二异丙基乙胺)活化,其中Cur-NH2:CA:EDC: NHS:DIPEA=1:2.5:3:3:3(摩尔比),再将(2)中生成的Cur-NH2,氮气保护,反应三天三夜,然后在蒸馏环境中透析,旋蒸冻干,最后生成乳白色水溶性物质,即为所制得吸水材料,记作Cur-CA;
(4)请参见图5、图6分别是Cur-CA的傅里叶红外变换图和核磁共振谱图,其中傅里叶红外变换图在1716cm-1的羰基伸缩振动峰1662 cm-1的N-H伸缩振动峰,1405 cm-1的C-N的伸缩振动峰以及核磁共振碳谱图中位移为175ppm处为羰基碳的峰,证明成功合成了CA改性的凝胶多糖衍生物。上述吸水材料与实施案例1中的吸水材料一样,吸水效果优良,最高吸水量可达自身重量的1300倍,具有良好的潜在应用价值。
Claims (2)
1.基于凝胶多糖多羧基化改性的强吸水凝胶材料及其制备方法,改性所用的多羧基化合物包括乙二胺四乙酸(EDTA)、次氮基三乙酸(NTA)、柠檬酸(CA)、丁二酸(SA)、丙二酸(MA)、乙二酸(OA)、二乙三胺五乙酸(DTPA)和聚谷氨酸(PGLU)等。
2.改性凝胶多糖部分结构式R如下:
。
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