CN101530620A - 一种三磷酸腺苷插层水滑石薄膜及其制备方法 - Google Patents

一种三磷酸腺苷插层水滑石薄膜及其制备方法 Download PDF

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CN101530620A
CN101530620A CN200910080440A CN200910080440A CN101530620A CN 101530620 A CN101530620 A CN 101530620A CN 200910080440 A CN200910080440 A CN 200910080440A CN 200910080440 A CN200910080440 A CN 200910080440A CN 101530620 A CN101530620 A CN 101530620A
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卫敏
倪学云
靳兰
段雪
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Beijing University of Chemical Technology
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Abstract

本发明公开了属于生物－无机复合材料技术领域的一种垂直基底生长的三磷酸腺苷插层水滑石薄膜及其制备方法。本发明采用原位生长法制得水滑石薄膜，然后再加入三磷酸腺苷，具体步骤为：首先使金属铝的表面形成阳极氧化铝层，生成水滑石薄膜；然后将水滑石薄膜浸入到三磷酸腺苷溶液中，于室温下干燥，得到三磷酸腺苷插层水滑石的薄膜。本发明的优点在于：利用原位生长技术，将三磷酸腺苷组装进入水滑石层间，实现三磷酸腺苷的固载化，利用水滑石的层板限域达到研究药物缓释的目的。

Description

一种三磷酸腺苷插层水滑石薄膜及其制备方法
技术领域
本发明属于生物—无机复合材料技术领域，特别涉及一种垂直基底生长的三磷酸腺苷插层水滑石薄膜及其制备方法。
背景技术
层状双羟基复合金属氧化物(LDHs)，是一类阴离子型层状无机功能材料，作为高性能催化材料、吸附材料、分离材料、功能性助剂材料、生物材料和医药材料等应用于国民经济诸多行业。由于LDHs粉体在实际应用中存在的易流失、难回收等问题，LDHs膜的出现引起了人们更广泛的兴趣。前人曾采用溶剂蒸发法，层层组装法和原位生长法等制备了LDHs膜，既便于回收再利用又有利于提高材料的性能。
在文献(1)J.Am.Chem.Soc.，2006，128：4872-4880中，Takayoshi Sasaki等人首先将Co-Al水滑石剥层，然后用层层组装法得到了水滑石层板与阴离子高聚物交替排列的水滑石薄膜，为制备水滑石薄膜提供新方法。
在文献(2)Adv.Mater.，2006，18：3089-3093中，段雪等采用原位合成技术，以经表面阳极氧化后的铝片为基片，利用基片表面上的阳极氧化铝提供水滑石生长所需的铝源，通过滴加氨水调节反应溶液的pH值，使溶液中Ni2+离子与NH3在接近中性条件下生长出疏密可控垂直基片生长的镍铝硝酸根水滑石(NiAl-LDHs)薄膜，并发现该薄膜具有超疏水的性能。
在文献(3)Chem.Mater.，2004，16：3774-3779中，Duk-Young Jung等采用溶剂蒸发技术以单晶硅为基底制备了层板平行于基底方向排列的水滑石薄膜。作者认为水滑石成膜后可明显方便研究水滑石在离子交换反应中形貌以及层间距的变化情况。
三磷酸腺苷可以作为一种注射试剂，临床上现用于心力衰竭、心肌炎、心肌梗塞、脑动脉硬化、冠状动脉硬化、急性脊髓灰质炎、进行性肌萎缩性疾患。在注射过程中要控制该试剂的吸收速度来避免引发头晕、头胀、胸闷及低血压等潜在的危险。将三磷酸腺苷插层水滑石，利用水滑石的层板限域功能可以达到研究药物缓释的目的。
发明内容
本发明目的在于提供一种垂直基底生长的三磷酸腺苷插层水滑石薄膜及其制备方法。三磷酸腺苷(ATP)插层水滑石薄膜为超分子结构，其晶体结构为水滑石材料的晶体结构，其化学式为：
[(M2+)1-x(Al3+)x(OH)2]x+(ATPn-)x/n·mH2O，其中0.2≤x≤0.33，n＝0.5-14，m＝3-6为层间结晶水分子数，M2+为Mg2+、Co2+、Ni2+、Ca2+、Cu2+、Fe2+或Zn2+。
本发明采用原位生长技术，在阳极氧化铝基底上合成了层板垂直于阳极氧化铝基底排列的三磷酸腺苷插层水滑石薄膜材料。其具体制备步骤如下：
a.将铝片分别在无水乙醇和去离子水中超声清洗2～10min，然后放入0.1-0.4M NaOH溶液中处理1～3min，再用去离子水冲洗干净，将清洗后的铝片作为阳极，铅片作为阴极，以1-2M H2SO4溶液作电解液，恒压氧化，工作电压15～25V，氧化电流为1.5～3A，电解时间为0.5～2h，电解温度为室温，使金属铝的表面形成阳极氧化铝层，样品用大量去离子水清洗干净，25～90℃干燥后备用；
b.分别称取二价金属盐和NH4NO3溶解于去离子水中配成反应合成液，二价金属离子浓度为0.1-0.6M，再用质量分数1％-4％的氨水调节反应合成液的pH在5.9～8.5之间，将步骤a制备的阳极氧化铝/铝基片垂直悬吊在上述反应合成液中，在40～130℃温度下反应12～96h，反应结束后用去离子水冲洗3～5遍，于室温下干燥，得到水滑石薄膜；
c.将三磷酸腺苷溶解在水中，浓度1-2g/L，再用质量分数1％-4％的氨水调节pH值在5.9～8.5之间，然后放入步骤b制备的长有水滑石薄膜的铝片，于40～130℃温度下反应12～96h，反应结束后将样品用去离子水冲洗3～5遍，于室温下干燥，得到三磷酸腺苷插层水滑石的薄膜。
木发明的优点在于：利用原位生长技术，将三磷酸腺苷组装进入水滑石层间，实现三磷酸腺苷的固载化以达到研究药物缓释的目的。
具体实施方式
通过下面实施例对本发明予以具体说明。
实施例1
步骤A：将铝片剪切成10cm×10cm的片，于无水乙醇和去离子水中分别超声清洗3min，然后放入0.1M的NaOH溶液中处理2min，再用去离子水冲洗干净，将清洗后的铝片作为阳极，铅片作为阴极，以1M的H2SO4溶液作电解液，恒压氧化，工作电压20V，氧化电流为2A，电解时间为1h，电解温度为室温，使金属铝的表面形成阳极氧化铝层，样品用大量去离子水清洗干净，70℃干燥后备用；
步骤B：分别称取2.960g Zn(NO3)2·6H2O和4.8g NH4NO3溶解于去离子水中配成150mL反应合成液，再用浓度1％的NH3·H2O调节反应合成液的pH为6.5，将步骤A制备的阳极氧化铝/铝基片垂直悬吊在上述反应合成液中，在75℃下反应48h，反应结束后将样品用去离子水冲洗3遍，于室温下干燥，得到水滑石薄膜；
步骤C：称取0.2g三磷酸腺苷溶解于去离子水中配成150ml反应合成液，再用浓度1％的NH3·H2O调节反应合成液的pH为6.5，将步骤B制备的长有水滑石薄膜的铝片垂直悬吊在上述反应合成液中，在75℃下反应48h，反应结束后用去离子水冲洗5遍，于室温下干燥，得到三磷酸腺苷插层水滑石的薄膜。
实施例2
步骤A：按实施例1中步骤A方法得到阳极氧化铝/铝基片；
步骤B：分别称取2.932g Co(NO3)2·6H2O和4.8g NH4NO3溶解于去离子水中配成150ml反应合成液，再用浓度1％的NH3·H2O调节反应合成液的pH为6.5。将阳极氧化铝/铝基片垂直悬吊在上述反应合成液中，在75℃下反应48h，反应结束后用去离子水冲洗，于室温下干燥，得到水滑石薄膜；
步骤C：称取0.15g三磷酸腺苷溶解于去离子水中配成150ml反应合成液，再用浓度1％的NH3·H2O调节反应合成液的pH为6.5，将步骤B制备的长有水滑石薄膜的铝片垂直悬吊在上述反应合成液中，在75℃下反应48h，反应结束后用去离子水冲洗5遍，于室温下干燥，得到三磷酸腺苷插层水滑石的薄膜。
实施例3
步骤A：按实施例1中步骤A方法得到阳极氧化铝/铝基片；
步骤B：分别称取2.908g Ni(NO3)2·6H2O和4.8g NH4NO3溶解于去离子水中配成100ml反应合成液，再用浓度1％的NH3·H2O调节反应合成液的pH为6.5。将阳极氧化铝/铝基片垂直悬吊在上述反应合成液中，在75℃下反应48h，反应结束后用去离子水冲洗，于室温下干燥，得到水滑石薄膜；
步骤C：称取0.15g三磷酸腺苷溶解于去离子水中配成150ml反应合成液，再用浓度1％的NH3·H2O调节反应合成液的pH为6.5，将步骤B制备的长有水滑石薄膜的铝片垂直悬吊在上述反应合成液中，在75℃下反应48h，反应结束后用去离子水冲洗5遍，于室温下干燥，得到三磷酸腺苷插层水滑石的薄膜。

Claims (3)

1.一种三磷酸腺苷插层水滑石薄膜，其特征在于：该薄膜为超分子结构，晶体结构为水滑石材料的晶体结构，其化学式为：
[(M2+)1-x(Al3+)x(OH)2]x+(ATPn-)x/n·mH2O，其中0.2≤x≤0.33，n＝0.5-14，m＝3-6为层间结晶水分子数。
2.根据权利要求1所述三磷酸腺苷插层水滑石薄膜，其特征在于：所述的M2+为Mg2+、Co2+、Ni2+、Ca2+、Cu2+、Fe2+或Zn2+。
3.一种三磷酸腺苷插层水滑石薄膜的制备方法，其特征在于，制备步骤为：
a.将铝片分别在无水乙醇和去离子水中超声清洗2～10min，然后放入0.1-0.4M NaOH溶液中处理1～3min，再用去离子水冲洗干净，将清洗后的铝片作为阳极，铅片作为阴极，以1-2M H2SO4溶液作电解液，恒压氧化，工作电压15～25V，氧化电流为1.5～3A，电解时间为0.5～2h，电解温度为室温，使金属铝的表面形成阳极氧化铝层，样品用大量去离子水清洗干净，25～90℃干燥后备用；
b.分别称取二价金属盐和NH4NO3溶解于去离子水中配成反应合成液，二价金属离子浓度为0.1-0.6M，再用质量分数1％-4％的氨水调节反应合成液的pH在5.9～8.5之间，将步骤a制备的阳极氧化铝/铝基片垂直悬吊在上述反应合成液中，在40～130℃温度下反应12～96h，反应结束后用去离子水冲洗3～5遍，于室温下干燥，得到水滑石薄膜；
c.将三磷酸腺苷溶解在水中，浓度1-2g/L，再用质量分数1％-4％的氨水调节pH值在5.9～8.5之间，然后放入步骤b制备的长有水滑石薄膜的铝片，于40～130℃温度下反应12～96h，反应结束后将样品用去离子水冲洗3～5遍，于室温下干燥，得到三磷酸腺苷插层水滑石的薄膜。
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