CN105147526A - 一种水热法合成纳米抗菌牙釉层的制备方法 - Google Patents
一种水热法合成纳米抗菌牙釉层的制备方法 Download PDFInfo
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Abstract
本发明属于无机非金属材料领域，特别是纳米抗菌牙釉层的制备方法，涉及到在人造牙齿表面附着一层厚度通常为0.2-0.8mm的抗菌牙釉层，主要成分为含银、铜、钙和磷的磷灰石晶体。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，将人造牙齿置入可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终在人造牙齿表面附着一层厚度通常为0.2-0.8mm的抗菌牙釉层。该纳米抗菌牙釉层主要成分为含银、铜、钙和磷的磷灰石晶体。该釉层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釉层中，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，特别是纳米抗菌牙釉层的制备方法，涉及到在人造牙齿表面附着一层厚度通常为0.2-0.8mm的抗菌牙釉层，主要成分为含银、铜、钙和磷的磷灰石晶体。
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，其硬度仅次于金刚石，其厚度通常为0.2-0.8mm，主要成分为含钙和磷的磷灰石晶体组成，人体牙釉层在遭到破坏后无法再生，因此，寻求人工手段获得人工牙釉层十分必要。人工牙釉层是通过合成的方法得到一种类牙釉层结构的羟基磷灰石，用不同种矿物质和化工原料按一定比例配合(部分原料可先制成熔块)经过研磨制成釉浆，施于牙坯体表面，经一定温度煅烧而成。能增加牙制品的力学性能、热稳定性和电介强度，还有美化牙齿、便于刷牙、不被细菌、油渍侵蚀等特点。因此，目前部分人造牙齿材料采用上釉的工艺提高人造牙齿的外在质量。
目前我国现有的牙釉质状羟基磷灰石在专利申请号2010102217096中，采用可溶性钙盐和可溶性磷酸盐通过水热合成法获得具有牙釉质状的羟基磷灰石。但是该发明材料中不含抗菌元素，起到不杀毒抗菌的作用，其它抗菌专利如牙釉质涂液和含氟牙膏，只能起到短期起到杀菌抗菌的作用，因此，研发一种通过在牙釉层基体添加抗菌元素进行抗菌杀毒的牙釉层制备方法十分必要。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，将人造牙齿放入可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终在人造牙齿表面附着一层厚度通常为0.2-0.8mm的纳米抗菌牙釉层，主要成分为含银、铜、钙和磷的磷灰石晶体。
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纳米抗菌牙釉层的制备方法，该方法制备的牙釉层具有抗菌杀菌效果，较常规牙釉层的使用寿命也大幅提升。
本发明提供了一种水热法合成纳米抗菌牙釉层材料的方法，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，将人造牙齿置入可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终在人造牙齿表面附着一层厚度通常为0.2-0.8mm的纳米抗菌牙釉层，主要成分为含银、铜、钙和磷的磷灰石晶体。该釉层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釉层中，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。
本发明是通过以下技术方案：
一种水热法合成纳米抗菌牙釉层的制备方法，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，将人造牙齿放入可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终在人造牙齿表面附着一层厚度通常为0.2-0.8mm的具有牙釉质状羟基磷灰石纳米抗菌牙釉层。
通过水热合成法在人造假牙表面生成纳米抗菌牙釉层材料，采用晶体自然生长的方法，能使纳米抗菌牙釉层与人造牙齿基体充分吸附反应。测试表明所获得的纳米抗菌牙釉层具有抗菌杀菌效果，较牙釉质涂液和含氟牙膏的抗菌效果和使用寿命大幅提升。
较佳的，所述纳米抗菌牙釉层的厚度为0.2～0.8mm；所述具有类牙釉质结构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釉质状结构。
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，所述纳米抗菌牙釉层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；将人造假牙植入反应釜中，反应液进行水热反应，水热反应结束后，冷却至室温，取出人造假牙，将人造假牙并在空气中干燥后即可制得表面附着一层厚度通常为0.2-0.8mm的纳米抗菌牙釉层。
优选的，所述水溶液中，水溶性阳离子聚电解质的含量为8～120mg/ml，尿素的含量为15wt％～25wt％，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。
通过水热法合成纳米抗菌牙釉层与天然的牙釉层具有相近的力学性能，同时具有抗菌杀菌效果。
该水热法合成纳米抗菌牙釉层材料无需专用设备，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。
与现有常规抗菌牙釉层相比，原位生成的纳米抗菌牙釉层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。牙釉层晶粒尺寸细小，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为本发明纳米抗菌牙釉层试样取点硬度测试示意图；
图2为本发明纳米抗菌牙釉层试样与传统牙釉层试样硬度比较曲线。
具体实施方式
下面给出本发明的最佳实施例：一种水热法合成纳米抗菌牙釉层的制备方法，采用晶体自然生长的方法，通过水热合成法在人造假牙表面生成纳米抗菌牙釉层材料，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％尿素的水溶液。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，将人造牙齿放入水热釜中，在90℃反应1000小时，能使纳米抗菌牙釉层与人造牙齿基体充分吸附反应。。反应结束后，自然冷却至室温。最终在人造牙齿表面附着一层厚度通常为0.2-0.8mm的具有牙釉质状羟基磷灰石纳米抗菌牙釉层，经水洗和醇洗，再在40℃下干燥1小时。抗菌性指标：对大肠杆菌杀菌率大于77.2%，对葡萄球菌的杀菌率菌大于80.2%，可见，所获得的所获得的纳米抗菌牙釉层具有抗菌杀菌效果，较牙釉质涂液和含氟牙膏的抗菌效果和使用寿命大幅提升。
Claims (2)
1.一种水热法合成纳米抗菌牙釉层的制备方法，其特征是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，将人造牙齿置入可溶性钙盐、可溶性磷酸盐、硫酸铜与硝酸银盐进行合成，最终在人造牙齿表面附着一层厚度通常为0.2-0.8mm的抗菌牙釉层。
2.根据权利要求1所述的一种水热法合成纳米抗菌牙釉层的制备方法，其特征是该纳米抗菌牙釉层主要成分为含银、铜、钙和磷的磷灰石晶体，该釉层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釉层中，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。
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| CN108946690A (zh) * | 2018-07-02 | 2018-12-07 | 昆明理工大学 | 一种抗菌改性羟基磷灰石材料的制备方法 |
| CN110236716A (zh) * | 2019-06-18 | 2019-09-17 | 上海慧丰牙科技术有限公司 | 一种活动义齿加工工艺 |
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| CN1295041A (zh) * | 1999-11-08 | 2001-05-16 | Aos控股公司 | 抗微生物瓷釉涂层 |
| CN1784975A (zh) * | 2005-12-13 | 2006-06-14 | 四川大学 | 无机纳米抗菌粉体的制备方法 |
| CN101891175A (zh) * | 2010-07-08 | 2010-11-24 | 中国科学院上海硅酸盐研究所 | 牙釉质状羟基磷灰石及其制备方法和应用 |
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| CN1295041A (zh) * | 1999-11-08 | 2001-05-16 | Aos控股公司 | 抗微生物瓷釉涂层 |
| CN1784975A (zh) * | 2005-12-13 | 2006-06-14 | 四川大学 | 无机纳米抗菌粉体的制备方法 |
| CN101891175A (zh) * | 2010-07-08 | 2010-11-24 | 中国科学院上海硅酸盐研究所 | 牙釉质状羟基磷灰石及其制备方法和应用 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946690A (zh) * | 2018-07-02 | 2018-12-07 | 昆明理工大学 | 一种抗菌改性羟基磷灰石材料的制备方法 |
| CN110236716A (zh) * | 2019-06-18 | 2019-09-17 | 上海慧丰牙科技术有限公司 | 一种活动义齿加工工艺 |
| CN110236716B (zh) * | 2019-06-18 | 2021-07-16 | 上海慧丰牙科技术有限公司 | 一种活动义齿加工工艺 |
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