CN110343267A - 一种锂皂石无机凝胶及其用途 - Google Patents
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Abstract
本发明属于凝胶技术领域,涉及一种锂皂石无机凝胶及其用途,一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。本发明以色氨酸改性锂皂石,与淀粉接枝聚丙烯酰胺聚合物体系相结合,制备出的凝胶,成型度好,保水性好,在常温下维持凝胶状态时间长,不易断裂。
Description
技术领域
本发明属于凝胶技术领域,涉及一种锂皂石无机凝胶及其用途。
背景技术
锂皂石,又称硅酸镁锂,是一种三八面体层状黏土矿物材料,具有纳米特性,在水体系中具极强的成胶性能,具有优异的触变性、分散性、悬浮性和增稠性。在水分散体系中,硅酸镁锂矿物微细颗粒的晶面和晶棱结合,形成包含大量水分子的触变性凝胶,其成胶能力表现在较低的固含量下,能形成较高粘度的胶体。此外,锂皂石表面与层间含有负电荷,能够与溶液中阳离子相互作用,从而能起到协同增稠作用。因此,将纳米颗粒尤其是纳米锂皂石应用于聚合物网络中发挥无机材料与有机高分子材料的双重优势是发展高强度水凝胶新的发展方向。
为此,专利公开号为CN104341556A的中国发明专利于2015年2月11日公开了一种高强度双网络纳米锂皂石复合水凝胶的制备方法,利用纳米锂皂石与聚合物之间的相互作用提高了海藻酸钠/聚丙烯酰胺双网络的力学稳定性,实现上述高强度双网络纳米锂皂石复合水凝胶的制备。所制备的高强度水凝胶拉伸应变可达 2280%,拉伸强度可达0.307MPa,形变为0.9时的压缩强度可达2.38MPa。相较于传统传统海藻酸钠/聚丙烯酰胺双网络水凝胶有较大提升。
但是在使用过程中,在常温下易硬化、易断裂,保水性差。
发明内容
为了克服现有水凝胶存在的上述缺陷,本发明以色氨酸改性锂皂石,与淀粉接枝聚丙烯酰胺聚合物体系相结合,制备出的凝胶,保水性好,在常温下维持凝胶状态时间长,不易断裂。
为了上述目的,本发明所采取的技术方案如下:
一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。
色氨酸改性锂皂石,根据改性锂皂石表面zeta电位及电荷密度的变化,以及锂皂石水分散液pH值、电导率变化,推断色氨酸在锂皂石表面的吸附经历了不同的吸附阶段。色氨酸在强负电性锂皂石的诱导下,产生不同电离状态的色氨酸离子,在锂皂石表面形成不同的吸附。
在色氨酸用量较低的情况下,所有的色氨酸分子都吸附在锂皂石表面,色氨酸吸附的机理是阳离子交换和氢键结合,该吸附机理被普遍接受。此时由于锂皂石分散液的pH值较高,色氨酸的胺基仅有部分发生了质子化(--NH2→--NH3+),而大部分羧基发生了去质子化(电离,--COOH→--COO−)。吸附在锂皂石表面的氨基酸通过质子化的NH3+与锂皂石表面的平衡离子 Na+发生离子交换,未发生质子化的--NH2 则与锂皂石表面Si-O 键中的O原子形成氢键,使得氨基酸分子定向排列在锂皂石表面,去质子化的--COO−朝外定向,提高了锂皂石表面负电荷密度和zeta电位的绝对值。随着氨基酸浓度的提高,吸附在锂皂石表面的--COO− 数量增多,锂皂石表面电性增强,zeta电位及表面负电荷密度的绝对值快速提高。
改性后的锂皂石在锂皂石表面吸附,形成单层或多层吸附结构,水分子穿插在各层及相邻氨基酸之间,延长脱水时间,保水性好,在常温下维持凝胶状态时间长,不易断裂。
作为优选,所述色氨酸改性锂皂石的获得方法如下:
S-1.将锂皂石进行预处理;
S-2.将预处理后的锂皂石加入温度恒定在60-65℃的水中,搅拌使锂皂石均匀分散在水中,得到分散液;
S-3. 分散液冷却至室温后加适量去离子水,静置7-10天;
S-4.步骤S-3所得的分散液中加入色氨酸溶液,并补充去离子水使锂皂石浓度为 1%,超声波处理,得到色氨酸改性锂皂石。
作为优选,色氨酸的浓度为0.15-0.35M。
色氨酸的浓度达到0.15M时,氨基酸在锂皂石表面已经形成饱和的单层吸附,继续增加丙氨酸用量,丙氨酸在锂皂石表面的吸附形式发生变化,增加的丙氨酸分子主要通过丙氨酸分子间相互作用吸附于锂皂石表面,并形成双层甚至多层吸附,至浓度达到0.35M,继续增加浓度已吸附丙氨酸对其继续吸附产生屏蔽作用,导致第三层丙氨酸的吸附量减少,增加的丙氨酸主要以游离形式存在,吸附量增加不明显。
作为优选,超声波处理时间为5-8min,超声波频率为50-100MHz。
作为优选,预处理操作为粉碎、过120-150目筛、微波膨化。
作为优选,粉碎采用水磨粉碎。
作为优选,微波膨化时间为10-15秒。
作为优选,锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:15-35添加。
进一步优选,锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:15-30添加。
进一步优选,锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:20-30添加。
进一步优选,锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:25添加。
作为优选,所述淀粉接枝聚丙烯酰胺的接枝率为98%以上。
上述锂皂石无机凝胶用于医疗、化妆品,例如医疗敷料,凝胶面膜。
通过实施上述技术方案,本发明具有如下的优点:本发明以色氨酸改性锂皂石,与淀粉接枝聚丙烯酰胺聚合物体系相结合,制备出的凝胶,成型度好,保水性好,在常温下维持凝胶状态时间长,不易断裂。
具体实施方式
下面通过具体实施例,对本发明的技术方案作进一步详细说明。
实施例仅是对本发明的优选实施方式进行描述,并非对本发明的构思和范围进行限定。在不脱离本发明设计构思的前提下,本领域普通人员对本发明的技术方案做出的各种变型和改进,均应落入到本发明的保护范围,本发明请求保护的技术内容,已经全部记载在权利要求书中。
实施例1:
一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:15添加。
所述色氨酸改性锂皂石的获得方法如下:
S-1.将锂皂石进行水磨粉碎、过120目筛、微波膨化15秒;
S-2.将预处理后的锂皂石加入温度恒定在65℃的水中,搅拌使锂皂石均匀分散在水中,得到分散液;
S-3. 分散液冷却至室温后加适量去离子水,静置10天;
S-4.步骤S-3所得的分散液中加入浓度为0.35M的色氨酸溶液,并补充去离子水使锂皂石浓度为 1%,超声波处理,得到色氨酸改性锂皂石。超声波处理时间为5min,超声波频率为100MHz。
实施例2:
一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100: 35添加。
所述色氨酸改性锂皂石的获得方法如下:
S-1.将锂皂石进行水磨粉碎、过150目筛、微波膨化10秒;
S-2.将预处理后的锂皂石加入温度恒定在60℃的水中,搅拌使锂皂石均匀分散在水中,得到分散液;
S-3. 分散液冷却至室温后加适量去离子水,静置7天;
S-4.步骤S-3所得的分散液中加入浓度为0.15M的色氨酸溶液,并补充去离子水使锂皂石浓度为 1%,超声波处理,得到色氨酸改性锂皂石。超声波处理时间为8min,超声波频率为80MHz。
实施例3:
一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:30添加。淀粉接枝聚丙烯酰胺接枝率为99%。
所述色氨酸改性锂皂石的获得方法如下:
S-1.将锂皂石进行水磨粉碎、过130目筛、微波膨化12秒;
S-2.将预处理后的锂皂石加入温度恒定在62℃的水中,搅拌使锂皂石均匀分散在水中,得到分散液;
S-3. 分散液冷却至室温后加适量去离子水,静置8天;
S-4.步骤S-3所得的分散液中加入浓度为0.20M的色氨酸溶液,并补充去离子水使锂皂石浓度为 1%,超声波处理,得到色氨酸改性锂皂石。超声波处理时间为8min,超声波频率为50MHz。
实施例4:
一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:20添加。淀粉接枝聚丙烯酰胺接枝率为110%。
所述色氨酸改性锂皂石的获得方法如下:
S-1.将锂皂石进行水磨粉碎、过120目筛、微波膨化10秒;
S-2.将预处理后的锂皂石加入温度恒定在60℃的水中,搅拌使锂皂石均匀分散在水中,得到分散液;
S-3. 分散液冷却至室温后加适量去离子水,静置7天;
S-4.步骤S-3所得的分散液中加入浓度为0.35M的色氨酸溶液,并补充去离子水使锂皂石浓度为 1%,超声波处理,得到色氨酸改性锂皂石。超声波处理时间为5min,超声波频率为100MHz。
对比例1:
依据专利公开号为CN104341556A的中国发明专利的制备方法所获得的复合水凝胶。
对比例2:
一种锂皂石无机凝胶,包括锂皂石、淀粉接枝聚丙烯酰胺,按照重量比为5:1添加。
对比例3:
与实施例4的不同在于,锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:10添加。
对比例4:
与实施例4的不同在于,色氨酸的浓度为0.10M。
对比例5:
与实施例4的不同在于,色氨酸的浓度为0.40M。
对实施例和对比例所得的凝胶进行保水性能检测,检测方法及结果如下:
测试设备:江苏昆山庆声科技股份有限公司—恒温恒湿试验箱;
测试样品:实施例1-4、对比例1-5所述凝胶;
尺寸:90cm*140cm的保水凝胶;
测试方法:将样品称重后平铺在试验箱中部,分别设定如下条件进行测试。常温常湿(温度:25℃,湿度:50%)、高温常湿(温度:70℃,湿度:50%)环境中放置三周后称重,计算三周失水量和失水率,结果见表1。
Claims (10)
1.一种锂皂石无机凝胶,其特征在于,包括锂皂石、淀粉接枝聚丙烯酰胺,所述锂皂石采用色氨酸改性锂皂石。
2.根据权利要求1所述一种锂皂石无机凝胶,其特征在于,锂皂石、淀粉接枝聚丙烯酰胺按照重量比为100:15-35进行配比。
3.根据权利要求1或2所述一种锂皂石无机凝胶,其特征在于,所述淀粉接枝聚丙烯酰胺的接枝率为98%以上。
4.根据权利要求1所述一种锂皂石无机凝胶,其特征在于,所述色氨酸改性锂皂石的获得方法如下:
S-1.将锂皂石进行预处理;
S-2.将预处理后的锂皂石加入温度恒定在60-65℃的水中,搅拌使锂皂石均匀分散在水中,得到分散液;
S-3. 分散液冷却至室温后加适量去离子水,静置7-10天;
S-4.步骤S-3所得的分散液中加入色氨酸溶液,并补充去离子水使锂皂石浓度为 1%,超声波处理,得到色氨酸改性锂皂石。
5.根据权利要求4所述一种锂皂石无机凝胶,其特征在于,色氨酸的浓度为0.15-0.35M。
6.根据权利要求4所述一种锂皂石无机凝胶,其特征在于,超声波处理时间为5-8min,超声波频率为50-100MHz。
7.根据权利要求4所述一种锂皂石无机凝胶,其特征在于,预处理操作为粉碎、过120-150目筛、微波膨化。
8.根据权利要求7所述一种锂皂石无机凝胶,其特征在于,粉碎采用水磨粉碎。
9.根据权利要求7所述一种锂皂石无机凝胶,其特征在于,微波膨化时间为10-15秒。
10.如权利要求1所述一种锂皂石无机凝胶的用途,用于医疗敷料或者凝胶面膜。
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