CN114849655A - 一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法 - Google Patents

一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法 Download PDF

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CN114849655A
CN114849655A CN202210262701.7A CN202210262701A CN114849655A CN 114849655 A CN114849655 A CN 114849655A CN 202210262701 A CN202210262701 A CN 202210262701A CN 114849655 A CN114849655 A CN 114849655A
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王心雨
张辉
谢翔
荣思佳
陈杰
刘盛全
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Anhui Agricultural University AHAU
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Abstract

本发明属于抗菌材料技术领域，具体涉及一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法，制备方法中溶剂采用纯水或弱碱性溶液，交联剂采用环氧氯丙烷，抗菌剂采用表面富含羟基的纳米二氧化钛，具体是以β环糊精或其衍生物为单体，在溶剂中与交联剂及纳米二氧化钛共同作用，反应生成高分子量聚合物，再经透析、洗涤、干燥得到二氧化钛/β‑CD聚合物基微球。本发明制备的水不溶性环糊精聚合物基抗菌微球材料为二氧化钛/β‑CD聚合物基微球，具有成本低，水中稳定、吸附性能、抗菌性能好等优良特性，且该微球的制备方法工艺简单，产品质量高，绿色环保。

Description

一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法
技术领域
本发明属于抗菌材料技术领域，具体涉及一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法。
背景技术
环糊精(Cyclodextrin)是淀粉在没有水分子参与的情况下，经环糊精葡萄糖基转移酶催化降解而得到的一系列环状低聚物的总称，通常含有6～12个D-吡喃葡萄糖单元。其中含有7个葡萄糖单元的β-环糊精(β-CD)，分子空洞适中，生产成本低，可以通过主客体相互作用和一些尺寸和形状相匹配的有机微污染物形成络合物，并兼具生物相溶性、生物可降解性和无污染等特点，在环境治理领域极具前景。
现有技术中的β-CD微球有以下不足：
1)β-CD水溶性较好，在水体污染治理中难以回收再利用；
2)β-CD本身不具备抗菌性能，应用领域受到限制。
有鉴于此，有必要提供一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法。
发明内容
本发明的目的在于克服现有技术中存在的上述问题，提供一种水不溶性环糊精聚合物基抗菌微球材料及其制备方法，通过制备水不溶性β-CD聚合物，实现β-CD基吸附材料在水体治理的应用；通过将二氧化钛等抗菌剂与β-CD聚合物耦合，提高其抗菌性能，拓宽其应用领域。
为实现上述技术目的，达到上述技术效果，本发明是通过以下技术方案实现：
一种水不溶性环糊精聚合物基抗菌微球材料的制备方法，包括如下步骤：
1)使用量筒分别量取纯水、冰醋酸与钛酸四丁酯，将纯水与冰醋酸依次倒入烧杯中并置于磁力搅拌器上，室温搅拌1-3h，使用胶头滴管缓慢滴入钛酸四丁酯，待滴定完成后在室温下继续搅拌6-8h，得到纳米二氧化钛溶胶；将此溶胶置于60℃鼓风干燥箱中干燥12-48h，得到的固体用玛瑙研钵研磨成粉末状的纳米二氧化钛；
2)量取氢氧化钠，倒入烧杯中并加水配制氢氧化钠溶液，加入β-CD粉末，在30-40℃水浴锅中以500rpm搅拌8-16h，再加入环氧氯丙烷，继续搅拌3-5h后，将溶液透析一周，透析产物冷冻干燥得到β-CD聚合物；
3)将步骤2)得到的β-CD聚合物与步骤1)得到的纳米二氧化钛在氢氧化钠溶液中混合，室温下搅拌1-3h，静置4-6min后加入环氧氯丙烷，室温下继续搅拌0.5-2h，置于60℃鼓风干燥箱中干燥12-48h，烘干的固体用玛瑙研钵研磨，水洗醇洗并烘干，得到二氧化钛/β-CD聚合物基微球。
进一步地，步骤1)中，纯水、冰醋酸与钛酸四丁酯的质量比为40-60:8-12:4。
进一步地，步骤1)中，纯水、冰醋酸与钛酸四丁酯的质量比为50:10:4。
进一步地，步骤1)中，钛酸四丁酯在1h内滴完。
进一步地，步骤2)中，氢氧化钠、β-CD粉末、环氧氯丙烷的质量比为10-20:8-12：1。
进一步地，步骤2)中，氢氧化钠、β-CD粉末、环氧氯丙烷的质量比为15:10：1。
进一步地，步骤2)中，在35℃水浴锅中以500rpm搅拌12h。
进一步地，步骤3)中，β-CD聚合物、纳米二氧化钛、环氧氯丙烷的质量比为40-80:0.5-2:1。
进一步地，步骤3)中，β-CD聚合物、纳米二氧化钛、环氧氯丙烷的质量比为60:1:1。
一种水不溶性环糊精聚合物基抗菌微球材料，由上述的制备方法制备得到。
本发明的有益效果是：
1、本发明工艺设计合理，溶剂采用纯水或弱碱性溶液，交联剂采用环氧氯丙烷，抗菌剂采用表面富含羟基的纳米二氧化钛，具体是以β环糊精或其衍生物为单体，在溶剂中与交联剂及纳米二氧化钛共同作用，反应生成高分子量聚合物，再经透析、洗涤、干燥得到二氧化钛/β-CD聚合物基微球。
2、本发明制备的二氧化钛/β-CD聚合物基微球具有成本低，水中稳定、吸附性能、抗菌性能好等优良特性，且该微球的制备方法工艺简单，产品质量高，绿色环保。
当然，实施本发明的任一产品并不一定需要同时达到以上的所有优点。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为实施例中二氧化钛/β-CD聚合物基微球对四环素的吸附降解能力图；
图2为实施例中产品的抗菌效果图；其中：
A-金黄色葡萄球菌光照处理；B-金黄色葡萄球菌避光处理；C-大肠杆菌光照处理；D-大肠杆菌避光处理。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
一种水不溶性环糊精聚合物基抗菌微球材料的制备方法，包括如下步骤：
1)使用量筒分别量取纯水、冰醋酸与钛酸四丁酯，将纯水与冰醋酸依次倒入烧杯中并置于磁力搅拌器上，室温搅拌1-3h，使用胶头滴管缓慢滴入钛酸四丁酯，待滴定完成后在室温下继续搅拌6-8h，得到纳米二氧化钛溶胶；将此溶胶置于60℃鼓风干燥箱中干燥12-48h，得到的固体用玛瑙研钵研磨成粉末状的纳米二氧化钛；
2)量取氢氧化钠，倒入烧杯中并加水配制氢氧化钠溶液，加入β-CD粉末，在30-40℃水浴锅中以500rpm搅拌8-16h，再加入环氧氯丙烷，继续搅拌3-5h后，将溶液透析一周，透析产物冷冻干燥得到β-CD聚合物；
3)将步骤2)得到的β-CD聚合物与步骤1)得到的纳米二氧化钛在氢氧化钠溶液中混合，室温下搅拌1-3h，静置4-6min后加入环氧氯丙烷，室温下继续搅拌0.5-2h，置于60℃鼓风干燥箱中干燥12-48h，烘干的固体用玛瑙研钵研磨，水洗醇洗并烘干，得到二氧化钛/β-CD聚合物基微球。
本发明的具体实施例为：
实施例1
1)采用溶胶凝胶法制备纳米二氧化钛抗菌剂，使用量筒分别量取50份纯水、10份冰醋酸与4份钛酸四丁酯，将纯水与冰醋酸依次倒入烧杯中并置于磁力搅拌器上，室温搅拌2小时，使用胶头滴管在1h内缓慢滴入钛酸四丁酯，待滴定完成后在室温下继续搅拌7小时，得到纳米二氧化钛溶胶。将此溶胶置于60℃鼓风干燥箱中干燥24小时，得到的固体用玛瑙研钵研磨成粉末状纳米二氧化钛。
2)量取15份氢氧化钠溶液，倒入烧杯中配制氢氧化钠溶液，加入10份β-CD粉末，在35℃水浴锅中以500rpm搅拌12h，再加入1份的环氧氯丙烷，继续搅拌4小时后，将溶液透析一周，透析产物冷冻干燥得到β-CD聚合物。
3)将60份制备的β-CD聚合物与1份纳米二氧化钛在氢氧化钠溶液中混合，室温下搅拌2小时，静置5分钟后加入2份环氧氯丙烷，室温下继续搅拌1小时，置于60℃鼓风干燥箱中干燥24小时，烘干的固体用玛瑙研钵研磨，水洗醇洗并烘干，得到二氧化钛/β-CD聚合物基微球。
实施例2
以实施例1制备的二氧化钛/β-CD聚合物基微球为样品，进行相关的性能测试：
如图1所示，制备的微球对水体污染物(以四环素为例)具有良好的吸附降解能力，在自然光照作用下，约半小时就能将水体中的四环素吸附降解完全。
如图2所示，将制备的微球负载在凝胶载体上，进行抗菌实验，结果表明在自然光照下或暗处对大肠杆菌和金黄葡萄球菌均有较好的杀灭作用。图中A：金黄色葡萄球菌光照处理；B:金黄色葡萄球菌避光处理；C：大肠杆菌光照处理；D：大肠杆菌避光处理；a，b，c，d表示所用产品浓度分别为0.1，0.2，0.3和0.4毫克。
以上公开的本发明优选实施例只是利于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。

Claims (10)

1.一种水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于，包括如下步骤：
1)使用量筒分别量取纯水、冰醋酸与钛酸四丁酯，将纯水与冰醋酸依次倒入烧杯中并置于磁力搅拌器上，室温搅拌1-3h，使用胶头滴管缓慢滴入钛酸四丁酯，待滴定完成后在室温下继续搅拌6-8h，得到纳米二氧化钛溶胶；将此溶胶置于60℃鼓风干燥箱中干燥12-48h，得到的固体用玛瑙研钵研磨成粉末状的纳米二氧化钛；
2)量取氢氧化钠，倒入烧杯中并加水配制氢氧化钠溶液，加入β-CD粉末，在30-40℃水浴锅中以500rpm搅拌8-16h，再加入环氧氯丙烷，继续搅拌3-5h后，将溶液透析一周，透析产物冷冻干燥得到β-CD聚合物；
3)将步骤2)得到的β-CD聚合物与步骤1)得到的纳米二氧化钛在氢氧化钠溶液中混合，室温下搅拌1-3h，静置4-6min后加入环氧氯丙烷，室温下继续搅拌0.5-2h，置于60℃鼓风干燥箱中干燥12-48h，烘干的固体用玛瑙研钵研磨，水洗醇洗并烘干，得到二氧化钛/β-CD聚合物基微球。
2.根据权利要求1所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤1)中，纯水、冰醋酸与钛酸四丁酯的质量比为40-60:8-12:4。
3.根据权利要求2所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤1)中，纯水、冰醋酸与钛酸四丁酯的质量比为50:10:4。
4.根据权利要求1所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤1)中，钛酸四丁酯在1h内滴完。
5.根据权利要求1所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤2)中，氢氧化钠、β-CD粉末、环氧氯丙烷的质量比为10-20:8-12：1。
6.根据权利要求5所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤2)中，氢氧化钠、β-CD粉末、环氧氯丙烷的质量比为15:10：1。
7.根据权利要求1所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤2)中，在35℃水浴锅中以500rpm搅拌12h。
8.根据权利要求1所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤3)中，β-CD聚合物、纳米二氧化钛、环氧氯丙烷的质量比为40-80:0.5-2:1。
9.根据权利要求8所述的水不溶性环糊精聚合物基抗菌微球材料的制备方法，其特征在于：步骤3)中，β-CD聚合物、纳米二氧化钛、环氧氯丙烷的质量比为60:1:1。
10.一种水不溶性环糊精聚合物基抗菌微球材料，由权利要求1-9任一项所述的制备方法制备得到。
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