CN106632915A - 一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法 - Google Patents

一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法 Download PDF

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CN106632915A
CN106632915A CN201610988986.7A CN201610988986A CN106632915A CN 106632915 A CN106632915 A CN 106632915A CN 201610988986 A CN201610988986 A CN 201610988986A CN 106632915 A CN106632915 A CN 106632915A
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张志军
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Abstract

本发明公开了一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，是由以下重量份的原料制成：聚磷酸铵2‑3，凹凸棒土5‑10，硼酸锌1‑2，盐酸溶液15‑20，硫酸锌溶液30‑40，无水乙醇适量，硅烷偶联剂KH‑570 2‑5，纳米氧化铜2‑4，硅烷偶联剂KH‑550 2‑5，壳聚糖2‑3，硝酸铈0.4‑1，丙烯酸5‑10，氮气适量，蒸馏水适量；本发明配合加入的壳聚糖富含氨基，不仅可以提供氨基接枝到凹凸棒土上，参与交联，增强其网络结构的稳定性，同时壳聚糖具有很好的吸附性，可以增加载体的载附量；通过添加聚磷酸铵和硼酸锌，使材料的阻燃抑烟效果好。

Description

一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法
技术领域
本发明涉及一种凹凸棒土载体及其制备，尤其涉及一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法。
背景技术
药物载体释放和靶向系统能够减少药物降解及损失，降低副作用，提高生物利用度，因而对它的研究越来越受到重视。高分子表面活性剂由于其独特的两亲性结构，可以进行自组装，形成各种形式的聚集体，如胶束、微乳液、凝胶、液晶、囊泡等。这些聚集体具有包载药物分子的能力，同时又对膜有良好的渗透性，成为药物载体的重要研究领域。凹凸棒土是一种以凹凸棒石为主要组分的,具有特殊纤维状晶体结构形态的含水富镁铝硅酸盐矿物。由于其优异的吸附性、离子交换、流变性、催化性和可塑性，而被应用于制备药物载体。
朱龙祥在其硕士学位论文《原位聚合制备凹凸棒/聚合物纳米复合材料中的凝胶现象及应用》中，利用凹凸棒土和丙烯酸制备了纳米复合水凝胶，但是其作为药物载体使用，还存在着载附量、抗菌性、缓释性欠佳的问题。
发明内容
基于以上思考，本发明旨在提供一种载附量大、抗菌性好的药物载体用纳米复合水凝胶，及其制备方法。
本发明所要解决的技术问题采用以下的技术方案来实现 ：
一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶，其特征在于，是由以下重量份的原料制成：
聚磷酸铵2-3，凹凸棒土5-10，硼酸锌1-2，盐酸溶液15-20，硫酸锌溶液30-40，无水乙醇适量，硅烷偶联剂KH-570 2-5，纳米氧化铜2-4，硅烷偶联剂KH-550 2-5，壳聚糖2-3，硝酸铈0.4-1，丙烯酸5-10，氮气适量，蒸馏水适量；
所述盐酸溶液浓度为2-6mol/L；硫酸锌溶液为0.5-1mol/L。
所述的一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，由以下步骤制成：
a. 将凹凸棒土在120-160℃下烘烤1-3h，去除其中的有机化合物后，分散于蒸馏水中，再加入盐酸溶液、硫酸锌溶液进行活化和离子交换吸附，再将聚磷酸铵和硼酸锌加入并混合搅拌 20min，使聚磷酸铵和硼酸锌进入凹凸棒土纳米孔道当中，并且表面富含硅羟基，有锌离子吸附；
b. 将步骤a所得凹凸棒纳米棒晶分散到无水乙醇中，加入硅烷偶联剂KH-570、硅烷偶联剂KH-550、壳聚糖，超声分散1-3h后，60-90℃回流20-26h，反应完成后用无水乙醇洗涤2-5次，干燥后，得到碳碳双键接枝和氨基接枝、壳聚糖接枝的凹凸棒纳米棒晶；
c. 将步骤b所得凹凸棒纳米棒晶分散到蒸馏水中，超声分散1-2h后，加入硝酸铈、纳米氧化铜、丙烯酸，氮气保护、磁力搅拌条件下，于50-80℃反应18-25h，用蒸馏水洗去未反应的丙烯酸和聚丙烯酸，即得纳米氧化铜、壳聚糖加强的凹凸棒土/聚丙烯复合凝胶。
所述的一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，步骤b中的干燥条件为30-50℃下真空干燥20-26h。
本发明的有益效果是：用盐酸溶液和硫酸锌溶液处理凹凸棒土，使得凹凸棒土表面富含硅羟基，为下一步的接枝改性做准备，同时吸附的锌离子具有杀菌的作用，使载体能更好的应用在医疗方面；用硅烷偶联剂KH-550和KH-570改性凹凸棒土后，得到氨基和碳碳双键接枝的凹凸棒土；在硝酸铈的催化作用下，丙烯酸在凹凸棒纳米棒晶表面通过氧化还原反应引发聚合，然后与接枝氨基和碳碳双键的凹凸棒土发生交联聚合反应，形成三维网络结构的纳米复合水凝胶；同时，加入的壳聚糖富含氨基，不仅可以提供氨基接枝到凹凸棒土上，参与交联，增强其网络结构的稳定性，同时壳聚糖具有很好的吸附性，可以增加载体的载附量；通过添加聚磷酸铵和硼酸锌，使材料的阻燃抑烟效果好。
具体实施方式
下面结合实施例， 对本发明的具体实施方式作进一步描述。
实施例
一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶，其特征在于，是由以下重量份的原料制成：
聚磷酸铵3，凹凸棒土10，硼酸锌2，盐酸溶液20，硫酸锌溶液40，无水乙醇适量，硅烷偶联剂KH-570 5，纳米氧化铜4，硅烷偶联剂KH-550 5，壳聚糖3，硝酸铈1，丙烯酸10，氮气适量，蒸馏水适量；
所述盐酸溶液浓度为2-6mol/L；硫酸锌溶液为0.5-1mol/L。
所述的一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，由以下步骤制成：
a. 将凹凸棒土在120-160℃下烘烤1-3h，去除其中的有机化合物后，分散于蒸馏水中，再加入盐酸溶液、硫酸锌溶液进行活化和离子交换吸附，再将聚磷酸铵和硼酸锌加入并混合搅拌 20min，使聚磷酸铵和硼酸锌进入凹凸棒土纳米孔道当中，并且表面富含硅羟基，有锌离子吸附；
b. 将步骤a所得凹凸棒纳米棒晶分散到无水乙醇中，加入硅烷偶联剂KH-570、硅烷偶联剂KH-550、壳聚糖，超声分散1-3h后，60-90℃回流20-26h，反应完成后用无水乙醇洗涤2-5次，干燥后，得到碳碳双键接枝和氨基接枝、壳聚糖接枝的凹凸棒纳米棒晶；
c. 将步骤b所得凹凸棒纳米棒晶分散到蒸馏水中，超声分散1-2h后，加入硝酸铈、纳米氧化铜、丙烯酸，氮气保护、磁力搅拌条件下，于50-80℃反应18-25h，用蒸馏水洗去未反应的丙烯酸和聚丙烯酸，即得纳米氧化铜、壳聚糖加强的凹凸棒土/聚丙烯复合凝胶。
所述的一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，步骤b中的干燥条件为30-50℃下真空干燥20-26h。
本发明的技术参数为：在pH值为7.0时，对90.0mg/L的亚甲基蓝溶液的吸附量≥302.0 mg/g。

Claims (3)

1.一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶，其特征在于，是由以下重量份的原料制成：
聚磷酸铵2-3，凹凸棒土5-10，硼酸锌1-2，盐酸溶液15-20，硫酸锌溶液30-40，无水乙醇适量，硅烷偶联剂KH-570 2-5，纳米氧化铜2-4，硅烷偶联剂KH-550 2-5，壳聚糖2-3，硝酸铈0.4-1，丙烯酸5-10，氮气适量，蒸馏水适量；
所述盐酸溶液浓度为2-6mol/L；硫酸锌溶液为0.5-1mol/L。
2.根据权利要求1所述的一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，由以下步骤制成：
a. 将凹凸棒土在120-160℃下烘烤1-3h，去除其中的有机化合物后，分散于蒸馏水中，再加入盐酸溶液、硫酸锌溶液进行活化和离子交换吸附，再将聚磷酸铵和硼酸锌加入并混合搅拌 20min，使聚磷酸铵和硼酸锌进入凹凸棒土纳米孔道当中，并且表面富含硅羟基，有锌离子吸附；
b. 将步骤a所得凹凸棒纳米棒晶分散到无水乙醇中，加入硅烷偶联剂KH-570、硅烷偶联剂KH-550、壳聚糖，超声分散1-3h后，60-90℃回流20-26h，反应完成后用无水乙醇洗涤2-5次，干燥后，得到碳碳双键接枝和氨基接枝、壳聚糖接枝的凹凸棒纳米棒晶；
c. 将步骤b所得凹凸棒纳米棒晶分散到蒸馏水中，超声分散1-2h后，加入硝酸铈、纳米氧化铜、丙烯酸，氮气保护、磁力搅拌条件下，于50-80℃反应18-25h，用蒸馏水洗去未反应的丙烯酸和聚丙烯酸，即得纳米氧化铜、壳聚糖加强的凹凸棒土/聚丙烯复合凝胶。
3.根据权利要求2所述的一种阻燃凹凸棒土/聚丙烯酸纳米复合凝胶及其制备方法，其特征在于，步骤b中的干燥条件为30-50℃下真空干燥20-26h。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113024994A (zh) * 2021-02-08 2021-06-25 厦门大学 一种纳米凹凸棒土/酚醛气凝胶的制备方法及其在制备耐磨汽车轮胎中的应用

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103724569A (zh) * 2013-12-23 2014-04-16 杨立新 一种高分子凹凸棒土复合凝胶及其制备方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103724569A (zh) * 2013-12-23 2014-04-16 杨立新 一种高分子凹凸棒土复合凝胶及其制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
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CN113024994A (zh) * 2021-02-08 2021-06-25 厦门大学 一种纳米凹凸棒土/酚醛气凝胶的制备方法及其在制备耐磨汽车轮胎中的应用
CN113024994B (zh) * 2021-02-08 2021-12-10 厦门大学 一种纳米凹凸棒土/酚醛气凝胶的制备方法及其在制备耐磨汽车轮胎中的应用
US11597809B2 (en) 2021-02-08 2023-03-07 Xiamen University Method for preparing nano attapulgite and phenolic aerogel and method for preparing abrasion-resistant vehicle tire

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Application publication date: 20170510