CN105106022B - 一种抗菌牙齿生长修复材料的制备方法 - Google Patents
一种抗菌牙齿生长修复材料的制备方法 Download PDFInfo
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Abstract
本发明属于无机非金属材料领域，特别是抗菌牙齿生长修复材料的制备方法，涉及到在缺失牙齿的牙槽里或残缺的牙齿表面生长修复抗菌牙齿材料，主要成分为含银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌。通过水溶性阳离子聚电解质和有机多元酸组成的双元聚电解质复合物的调控作用下，将牙齿生长修复材料成分与可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，采用晶体自然生长的方法，能使银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌等牙齿基体充分吸附反应。该抗菌牙齿生长修复材料的晶粒为纳米级，从而铜和银金属颗粒更为细小和均匀的分布于牙齿生长修复材料中，金属颗粒直径为30‑80nm，能够快速、持久的不断释放出抗菌元素。
Description
技术领域
本发明属于无机非金属材料领域，特别是抗菌牙齿生长修复材料的制备方法，涉及到在缺失牙齿的牙槽里或残缺的牙齿表面生长修复抗菌牙齿材料，主要成分为含银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌。
背景技术
目前，牙科口腔材料的需求量逐年递增，其中钛合金、镍铬合金等牙科口腔材料在生活方面需求量很大，随着人民生活水平的提高，在人造牙齿材料能够保持与天然牙齿一致的色泽十分重要，因此，在钛合金、镍铬合金表面通常需要附着一层牙釉质，牙釉层是覆盖在牙表面的白色半透明的钙化程度最高的坚硬组织，但是人造牙釉层价格十分昂贵，同时钛合金、镍铬合金与人体的相容性有一定差距，易造成人体不适感。因此，寻求在缺失牙齿的牙槽里或残缺的牙齿表面生长修复具有类牙齿材料的抗菌牙齿材料十分必要。抗菌牙齿生长修复材料是通过合成的方法得到一种类牙齿结构的羟基磷灰石、氧化钛和氧化锌合成物。
目前我国现有的牙齿生长修复材料在专利申请号2009801284826中，采用多孔硅酸盐陶瓷坯体，通过烧结获得牙齿修复体。但是该发明材料中不含抗菌元素，起到不杀毒抗菌的作用，同时该专利牙齿生长修复材料的主要成分不是羟基磷灰石与人体的相容性有一定差距，易造成人体不适感。因此，研发一种通过在牙齿生长修复材料基体添加抗菌元素进行抗菌杀毒的牙齿生长修复材料制备方法十分必要。基于上述目的，铜和银金属具有广谱抗菌属性，在由水溶性阳离子聚电解质和有机多元酸组成的双元聚电解质复合物的调控作用下，将牙齿生长修复材料成分与可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终合成抗菌牙齿生长修复材料，主要成分为含银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌。
发明内容
本发明专利的目的是：在于克服上述现有技术不足，提供一种加工工艺稳定、生产成本低廉、无污染排放、可在常规条件下组织生产的一种抗菌牙齿生长修复材料的制备方法，该方法制备的牙齿生长修复材料具有抗菌杀菌效果，较常规牙齿生长修复材料的生物相容性和使用寿命也大幅提升。
本发明提供了一种水热法合成抗菌牙齿生长修复材料的方法 ，其特征在于：水溶性阳离子聚电解质和有机多元酸组成的双元聚电解质复合物的调控作用下，将牙齿生长修复材料成分与可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终合成抗菌牙齿生长修复材料，主要成分为含银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌。该抗菌牙齿生长修复材料的晶粒为纳米级，从而铜和银金属颗粒更为细小和均匀的分布于牙齿生长修复材料中，金属颗粒直径为30-80nm，能够快速、持久的不断释放出抗菌元素。
一种水热法合成抗菌牙齿生长修复材料的制备方法的技术方案：
（1）在由水溶性阳离子聚电解质和有机多元酸组成的双元聚电解质复合物的调控作用下，将纳米棒状氧化锌其长度和直径分别为0.4-1.0μm 和40-80nm；将重量含量为2-5％纳米棒状氧化钛其长度和直径分别为0.4-1.0μm 和40-80nm。
（2）将重量含量为2-5％氧化锌和将重量含量为2-5％的氧化钛分别称取上述两种纳米粉体放入可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，超声分散3小时，然后将上述混合溶液置于36.8℃恒温水浴锅中，恒温水浴加热24-48 小时。
（3）最终在混合液体中结晶形成抗菌牙齿生长修复材料，主要成分为含银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌。该抗菌牙齿生长修复材料的晶粒为纳米级，从而铜和银金属颗粒更为细小和均匀的分布于牙齿生长修复材料中，金属颗粒直径为30-80nm，能够快速、持久的不断释放出抗菌元素。
通过水热合成法生成抗菌牙齿生长修复材料，采用晶体自然生长的方法，能使银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌等牙齿基体充分吸附反应。测试表明所获得的抗菌牙齿生长修复材料具有抗菌杀菌效果，较牙齿涂液和含氟牙膏的抗菌效果和使用寿命大幅提升。
较佳的，所述抗菌牙齿生长修复材料的羟基磷灰石的微观组成单元为直径为30～200nm 的纳米棒，并相互平行紧密堆积形成牙齿状结构。
较佳的，所述可溶性钙盐为四水硝酸钙。
较佳的，所述可溶性硫酸盐为硫酸铜。
较佳的，所述可溶性硝酸盐为硝酸银。
较佳的，所述可溶性磷酸盐选自磷酸二氢钙。
较佳的，所述水溶性聚电解质选自聚丁烯酰胺。
较佳的，所述有机多元酸选自马来酸。
较佳的，所述抗菌牙齿生长修复材料的制备方法包括如下步骤：配制含有水溶性阳离子聚电解质，有机多元酸和尿素的水溶液；接着向制得的水溶液中加入可溶性钙盐、可溶性硫酸盐、可溶性硝酸盐和可溶性磷酸盐，搅拌后制得反应液；将纳米棒状氧化钛和纳米棒状氧化锌放入反应釜中，反应液进行水热反应，水热反应结束后，冷却至室温，取出结晶物，将结晶物在空气中干燥后即可制得抗菌牙齿生长修复材料。
优选的，所述水溶液中，水溶性阳离子聚电解质聚丁烯酰胺的含量为8～120mg/ml，有机多元酸的浓度为10～40mg/ml。
优选的，所述反应液中，可溶性钙盐的浓度为0.1～1mol/L，钙/磷的摩尔比(Ca/P)为1～2.7∶1。
优选的，所述搅拌时间为30～60 分钟。
优选的，所述水热反应的反应温度为80～160℃，反应时间为800～1600小时。
优选的，所述干燥过程为在空气中干燥，干燥温度为20～80℃，干燥时间为1小时。
通过水热法合成抗菌牙齿生长修复材料与天然的牙齿具有相近的力学性能，同时具有抗菌杀菌效果。
该水热法合成抗菌牙齿生长修复材料无需专用设备，在化工厂即可组织生产，本发明投资少，见效快，能快速收回投资成本。
与现有常规抗菌牙齿生长修复材料相比，原位生成的抗菌牙齿生长修复材料的制备方法具有如下优点：
（1）具有强韧性，同时耐磨性和硬度显著提高，这将有利于大批量、小尺寸口腔材料的稳定生产。抗菌牙齿生长修复材料晶粒尺寸细小，分布均匀，组织稳定性高，与人造牙齿基体结合良好。釉层材料的室温韧性、硬度和耐磨性能显著提高。
（2）纳米抗菌釉层组织稳定性好，不会分解有毒气体或有毒溶解物，因为银、铜等物质可以在釉层中以细小的颗粒形式更为均匀和广泛的分布，合成后的纳米硫酸铜和硝酸银粒具有光谱抗菌性，能够快速、持久的不断释放出抗菌元素。
附图说明
下面是结合附图和实施例对本发明的具体实施方案进行详细地说明。
图1为本发明抗菌牙齿生长修复材料试样取点硬度测试示意图；
图2为本发明抗菌牙齿生长修复材料试样与传统牙齿试样硬度比较曲线。
具体实施方式
下面给出本发明的最佳实施例：一种水热法合成抗菌牙齿生长修复材料的制备方法，采用晶体自然生长的方法，通过水热合成法制备抗菌牙齿生长修复材料，首先配制由水溶性阳离子聚电解质和有机多元酸组成的双元聚电解质复合物，将含有40mg/ml聚丁烯酰胺和24wt％马来酸的水溶液。接着向上述溶液加入硫酸铜、硝酸银、四水硝酸钙和磷酸二氢钙，并搅拌45分钟。其中，其中硫酸铜的浓度为0.05mol/L，硝酸银的浓度为0.05mol/L，硝酸钙的浓度为0.14mol/L，钙/磷的摩尔比(Ca/P) 为1.7。随后将反应液倒入水热釜中，将重量含量为3％氧化锌和将重量含量为3％的氧化钛分别称取上述两种纳米粉体放入水热釜中，在90℃反应1000小时，能使银、铜、钙和磷的磷灰石晶体、氧化钛和氧化锌等牙齿基体充分吸附反应。反应结束后，自然冷却至室温。最终取出结晶物，将结晶物在空气中干燥后即可制得具有牙齿结构的抗菌牙齿生长修复材料。经水洗和醇洗，再在40℃下干燥1小时。进行力学性能测试，抗弯强度621MPa、断裂韧性8.15MPa·m1/2、维氏硬度367。并进行抗菌性能测试，抗菌性指标：对大肠杆菌杀菌率大于78.1%，对葡萄球菌的杀菌率大于80.3%，可见，所获得的所获得的抗菌牙齿生长修复材料具有抗菌杀菌效果，较牙齿涂液和含氟牙膏的抗菌效果和使用寿命大幅提升。
Claims (2)
1.一种抗菌牙齿生长修复材料的制备方法，其特征在于，制备方法如下：配制由水溶性阳离子聚电解质和有机多元酸组成的双元聚电解质复合物，具体为含有40mg/mL聚丁烯酰胺和24wt％马来酸的水溶液；接着向上述溶液加入硫酸铜、硝酸银、四水硝酸钙和磷酸二氢钙，并搅拌45分钟，其中，硫酸铜的浓度为0.05mol/L，硝酸银的浓度为0.05mol/L，硝酸钙的浓度为0.14mol/L，钙/磷的摩尔比为1.7；随后将反应液倒入水热釜中，分别称取重量含量为3％的氧化锌和重量含量为3％的氧化钛的纳米粉体放入水热釜中，在90℃反应1000小时；反应结束后，自然冷却至室温，取出结晶物，将结晶物在空气中干燥后即得。
2.如权利要求1所述的一种抗菌牙齿生长修复材料的制备方法，其特征在于，获得的抗菌牙齿生长修复材料的力学性能为：抗弯强度621MPa，断裂韧性8.15MPa·m1/2，维氏硬度367；抗菌性能为：对大肠杆菌杀菌率大于78.1%，对葡萄球菌的杀菌率大于80.3%。
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