CN110229269A - 一种抗冻智能水凝胶 - Google Patents
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Abstract
本发明是提供一种pH敏感的耐低温、抗冻智能水凝胶合成方法。本发明以α‑甲基丙烯酸、丙烯酰胺为聚合单体,N,N′‑亚甲基双丙烯酰胺(MBA)为交联剂,乙二醇和氯化钙为增强剂,原位自由基共聚合得到一种水凝胶,该产品既具有pH敏感水凝胶和一定结构强度、溶胀率适度,又具有耐低温能力。
Description
技术领域
本发明属于智能性水凝胶领域,确切说是一种pH敏感的耐低温水凝胶。
背景技术
环境敏感型水凝胶又称智能性水凝胶是一种主链或支链中含有亲水交联基团,在水中溶胀但不溶解的具有三维网络状结构的聚合物,在外界发生环境变化时(如温度、电场、pH值、光强度离子强度、GSH等物理或化学因素)其凝胶物理形态或化学结构随之发生明显变化。许多材料科学工作者对智能水凝胶作了大量研究。环境敏感型智能水凝胶在化学传感器、组织材料、软体机器人、化学反应开关、吸附分离、药物控释、化学反应开关等领域有重要的应用价值。
pH敏感水凝胶是最重要、研究最为广泛的响应性水凝胶之一。这种水凝胶的三维网络结构中通常情况下含有可离子化的碱性或者酸性基团,如羧基、磷酸基、胺基、磺酸基等。随着介质pH和离子强度的改变,基团将发生电离和水解等可逆过程,进而导致网络中的大分子链段间的氢键解离和形成,产生不连续的溶胀体积变化。
随着各类智能水凝胶应用的深入,在低温条件下pH敏感水凝胶的研究尤为迫切。我们研究发现各类pH敏感水凝胶往往不耐低温,凝固点大多在0℃左右,而pH响应性在凝固之前已消失。寻找一种pH敏感水凝胶的耐低温添加剂具有现实意义。
发明内容
本发明是提供一种pH敏感的耐低温、抗冻水凝胶以解决上面所列的技术问题。
本发明以α-甲基丙烯酸(MAA)、丙烯酰胺(AM)为聚合单体, N , N′-亚甲基双丙烯酰胺(MBA)为交联剂,乙二醇(CH2OH)2和氯化钙(CaCl2)为增强剂,原位自由基共聚合。得到一种水凝胶P(AM/MAA)/ CaCl2/ (CH2OH)2,既具有pH敏感性、结构强度、适度溶胀率,又具有耐低温抗冻能力。
技术方案
以下组份配比计算按质量比,玻璃模板容器中加入蒸馏水200份,于60℃水浴加热脱氧。冷却至室温后加入单体:5份α-甲基丙烯酸、10份AM、0.2份交联剂MBA、0.2份引发剂过硫酸钾,加入1-5份乙二醇和3-15份氯化钙防冻剂接着搅拌溶解,乙二醇和氯化钙质量比为1∶3。通 N215min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品。
具体实施方式
下面通过实施例和对比例对本发明作进一步详细说明,但并不因此将本发明保护范围限制在所述的实施例范围之内。本发明中,未注明具体条件者,按照常规条件或制造商建议的条件进行,所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
实施例1
玻璃模板容器中加入20ml蒸馏水,于60℃水浴加热脱氧。冷却至室温后加入单体:α-甲基丙烯酸0.5ml、丙烯酰胺1g、交联剂N , N′-亚甲基双丙烯酰胺0.02g、引发剂过硫酸钾0.02g,按照合成设计要求分别加入乙二醇0.05g ,氯化钙0.15g接着搅拌溶解,加盖。通氮气15min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品。
实施例2
玻璃模板容器中加入20ml蒸馏水,于60℃水浴加热脱氧。冷却至室温后加入单体:α-甲基丙烯酸0.5ml、丙烯酰胺1g、交联剂N , N′-亚甲基双丙烯酰胺0.02g、引发剂过硫酸钾0.02g,按照合成设计要求分别加入乙二醇0.1g ,氯化钙0.3g接着搅拌溶解,加盖。通氮气15min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品。
实施例3
玻璃模板容器中加入20ml蒸馏水,于60℃水浴加热脱氧。冷却至室温后加入单体:α-甲基丙烯酸0.5ml、丙烯酰胺1g、交联剂N , N′-亚甲基双丙烯酰胺0.02g、引发剂过硫酸钾0.02g,按照合成设计要求分别加入乙二醇0.15g ,氯化钙0.45g接着搅拌溶解,加盖。通氮气15min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品。
实施例4
玻璃模板容器中加入20ml蒸馏水,于60℃水浴加热脱氧。冷却至室温后加入单体:α-甲基丙烯酸0.5ml、丙烯酰胺1g、交联剂N , N′-亚甲基双丙烯酰胺0.02g、引发剂过硫酸钾0.02g,按照合成设计要求分别加入乙二醇0.2g ,氯化钙0.6g接着搅拌溶解,加盖。通氮气15min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品。
实施例5
玻璃模板容器中加入20ml蒸馏水,于60℃水浴加热脱氧。冷却至室温后加入单体:α-甲基丙烯酸0.5ml、丙烯酰胺1g、交联剂N , N′-亚甲基双丙烯酰胺0.02g、引发剂过硫酸钾0.02g,按照合成设计要求分别加入乙二醇0.25g ,氯化钙0.75g接着搅拌溶解,加盖。通氮气15min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品,部分产品烘干作溶胀实验。
对比例1
玻璃模板容器中加入20ml蒸馏水,于60℃水浴加热脱氧。冷却至室温后加入单体:α-甲基丙烯酸0.5ml、丙烯酰胺1g、交联剂N , N′-亚甲基双丙烯酰胺0.02g、引发剂过硫酸钾0.02g,加盖。通氮气15min后于60℃水浴中加热反应4h。反应结束,产品用蒸馏水、无水乙醇轮番洗涤,以除去未反应的单体和杂质,最后用布氏漏斗分离得到原位凝胶产品。
将对比例1和实施例1-5作凝固点测试结果见表1。
表1凝固点测试
附图说明
选取实施例5所得水凝胶作为代表,分别测试其不同时间和pH下的溶胀度,结果见图1、图2。
图1是水凝胶时间溶胀曲线图;
图2是pH对水凝胶溶胀的影响趋势图。
上述实验结果表明,乙二醇和氯化钙加入可使P(AM/MAA)水凝胶凝固点降低,加入乙二醇和氯化钙水凝胶的凝固点随着添加量的增加而降低,加入防冻剂的水凝胶具有良好的溶胀性和pH响应性。因而该产品是具备一定抗冻耐低温能力的智能水凝胶。
Claims (7)
1.一种抗冻智能水凝胶,其特征在于,按质量计,包括如下组分:200份蒸馏水,5份α-甲基丙烯酸、10份AM、0.2份交联剂MBA、0.2份引发剂过硫酸钾, 1-5份乙二醇和5-10份氯化钙;合成步骤为:蒸馏水于60℃水浴加热脱氧,在玻璃模板容器中加入各组分单体并混合均匀,充氮气15min后在60℃水浴中加热反应4h,合成的产品进行分离、提纯。
2.根据权利要求1所述的一种抗冻智能水凝胶,其特征在于:所述蒸馏水60℃下加热脱氧,然后冷却至室温。
3.根据权利要求1所述的一种抗冻智能水凝胶,其特征在于:防冻剂为乙二醇和氯化钙组合复配,用量6-15份,乙二醇和氯化钙质量比为1∶3。
4.根据权利要求1所述的一种抗冻智能水凝胶,其特征在于:所述自由基聚合反应温度60℃。
5.根据权利要求1所述的一种抗冻智能水凝胶,其特征在于:所述自由基聚合反应在充氮气后密闭进行。
6.根据权利要求1所述的一种抗冻智能水凝胶,其特征在于:所述自由基聚合反应在定制玻璃模板容器中进行。
7.根据权利要求1所述的一种抗冻智能水凝胶,其特征在于:所述水凝胶用蒸馏水、无水乙醇洗涤,最后用布氏漏斗分离。
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Cited By (2)
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CN111234122A (zh) * | 2020-03-12 | 2020-06-05 | 山东大学 | 一种抗冰水凝胶粘结材料及其制备方法和应用 |
CN113429503A (zh) * | 2021-07-06 | 2021-09-24 | 南京林业大学 | 一种金属离子辅助催化的水凝胶制备方法及其应用 |
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