CN113876630A - 一种抗菌抗黏附耐酸防污疏水牙齿保护剂制备方法及应用 - Google Patents
一种抗菌抗黏附耐酸防污疏水牙齿保护剂制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种抗菌抗黏附耐酸防污疏水牙齿保护剂制备方法及应用，该牙齿保护剂包括：光响应抗菌剂、纳米粒子、疏水性改性剂、疏水胶黏剂、无水乙醇溶剂，利用疏水改性剂对纳米粒子疏水改性，并与光响应抗菌剂和疏水胶粘剂通过混合后得到可喷涂光响应抗菌抗黏附耐酸防污超疏水牙齿保护剂，该喷涂剂喷涂在牙齿上固化后形成保护膜具有光响应性、抗菌抗黏附性、耐酸防污性和超疏水性，能够有效防止食物残渣和细菌黏附在牙齿上，在500‑750 nm的LED可见光光源激发下可以进一步提高抗菌性，及时杀灭侥幸黏附于牙齿的细菌，同时达到降解色素美白的效果。本发明方法对生产设备要求不高，生产工艺安全方便，使用简单，实用性强，可以大规模生产和普适于大众。
Description
技术领域
本发明涉及超疏水涂层的制备工艺技术领域，尤其涉及一种抗菌抗黏附耐酸防污疏水牙齿保护剂制备方法及应用。
背景技术
随着社会不断发展进步，生活水平不断提高，牙齿健康问题受到越来越多的人关注，大家不再仅仅满足于牙痛找牙医和简单的刷牙，人们的观念逐渐从治疗牙齿疾病转变为定期牙齿护理。绝大多数的牙齿护理方式都是及时清除牙齿上的残留食物残渣，避免产生口气口臭，防止牙齿变黄变黑，预防细菌在牙齿表面定植生长产酸导致龋病、牙龈炎和牙周炎等。
目前人们主要通过牙刷、牙线和漱口水等进行日常的清洁护理，但是不恰当地使用牙刷牙线等口腔清洁工具实际上是对牙齿做“减法”，不但不能起到清洁作用，反而造成不可逆的牙齿损伤。同时由于生活节奏越来越快，人们很难做到每次进食后及时刷牙并应用牙线和漱口水进行日常的清洁护理，这就导致了残留在牙齿上的食物变成滋养细菌的温床，细菌大量繁殖并产生代谢物，导致口腔疾病例如龋病、牙龈炎和牙周炎等的发生。
为了解决以上问题，本发明研究设计了一款可喷涂光响应抗菌、抗黏附、耐酸和防污的超疏水牙齿保护剂，该保护剂喷涂于牙齿后能够固化成膜，具有光响应抗菌、抗黏附、耐酸防污和超疏水特性，实现牙齿的“加法”保护，有效防止食物残渣和细菌黏附在牙齿上，同时该保护膜还能在500-750 nm波长LED可见光激发下进一步提高抗菌性，及时杀灭侥幸黏附于牙齿的细菌，在500-750 nm波长LED可见光照射下该保护膜还具有降解色素美白的效果。
发明内容
（一）要解决的技术问题
本发明的目的是为了解决上述问题，提供一种抗菌抗黏附耐酸防污疏水牙齿保护剂制备方法及应用，以解决不恰当的牙齿护理对牙齿造成损伤和快节奏生活下食物残渣和细菌黏附牙齿不能及时有效清除，导致龋病和牙龈病高发的问题。
（二）发明内容
为了解决上述技术问题，本发明提出了一种抗菌抗黏附耐酸防污疏水牙齿保护剂，该保护剂各组分按重量份表示为：
0.5~2份光响应抗菌剂；
0.5~2份纳米粒子；
0.1~1份疏水性改性剂；
50-150份疏水胶黏剂；
100~200份无水乙醇溶剂。
所述光响应抗菌剂为碳掺杂氧化锌或碳掺杂二氧化钛或两者混合；
所述纳米粒子为纳米二氧化硅和铜颗粒的混合物；
所述疏水改性剂为十七氟癸基三甲氧基硅烷或十八烷基硫醇或十八烷基三甲氧基硅烷中的一种或多种混合；
所述疏水胶黏剂为聚二甲基硅油或环氧树脂。
优选的，为使牙齿保护膜固化后具有较好的耐磨性，上述的纳米粒子为不同粒径的纳米二氧化硅或铜颗粒混合。
本发明还提供了一种抗菌抗黏附耐酸防污疏水牙齿保护剂的制备方法，包括以下步骤：
步骤1、按配比将纳米粒子和疏水改性剂加入到无水乙醇中疏水改性，得到疏水纳米粒子；
步骤2、将疏水胶黏剂和固化剂按配比搅拌均匀后，加入到含微量己烷的无水乙醇中搅拌分散，得到混合溶液A；
步骤3、按配比将步骤1中所得疏水纳米粒子和光响应抗菌剂加入到步骤2中所得到的混合溶液A中搅拌混匀即得到一种抗菌抗黏附耐酸防污疏水牙齿保护剂。
优选的，步骤1中纳米粒子、疏水改性剂加入到无水乙醇中的顺序为：先将纳米粒子加入到无水乙醇中，再加入疏水改性剂，改性完成后过滤干燥得到疏水纳米粒子。
优选的，所述光响应抗菌剂能够在波长在500-750nm的LED可见光照射下产生活性氧，杀死侥幸黏附在牙齿表面的细菌，同时降解沉着在牙齿表面的色素。
本发明实施例中还提供了一种抗菌抗黏附耐酸防污疏水牙齿保护剂的应用，通过将牙齿保护剂盛装于喷雾瓶中用作喷剂，使用时将其喷涂至牙齿表面以形成保护膜，达到抗菌、抗黏附、耐酸、防污、疏水的目的。
（三）有益效果
1、光响应抗菌剂在LED可见光照射下按需杀菌，不会对口腔组织产生刺激；
2、超疏水性通过物理方式有效防止食物残渣和细菌的黏附、牙齿色素沉着和降低龋齿和牙龈病等口腔疾病发生，避免了耐药菌出现；
3、通过调控不同粒径的疏水纳米二氧化硅和固化剂的配比，使牙齿保护膜固化后具有较好的耐磨性；
4、工艺简单，生物安全性好，操作方法简单，保护效果明显。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中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 为本发明实施例中有牙齿保护剂覆盖的牙齿（左）和普通牙齿（右）的电镜对比图；
图2 为本发明实施例中牙齿保护剂覆盖牙齿后其表面接触角和滚动角示意图；
图3 为本发明实施例中牙齿保护剂覆盖在牙齿上的耐磨性和耐酸腐蚀性的曲线图；
图4 为本发明实施例中覆盖有牙齿保护剂的牙齿在500nm波长的LED可见光源照射一段时间后的抗菌性培养结果对比图；
图5 为本发明实施例中小鼠牙齿抗酸蚀保护对比图；
图6 为本发明实施例中小鼠的相关组织HE染色结果示意图。
具体实施方式
下面结合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做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。以下实施例中所使用的近似性语言可用于定量表述，表明在不改变基本功能的情况下可允许数量有一定的变动。因此，用“大约”、“左右”等语言所修正的数值不限于该准确数值本身，在一些实施例中，“大约”表示允许其修正的数值在正负百分之十(10％)的范围内变化。
实施例1
本发明一种抗菌抗黏附耐酸防污疏水牙齿保护剂，该保护剂各组分按重量份表示为：
0.5~2份光响应抗菌剂；
0.5~2份纳米粒子；
0.1~1份疏水性改性剂；
50-150份疏水胶黏剂；
100~200份无水乙醇溶剂。
具体地，所述光响应抗菌剂为碳掺杂氧化锌或碳掺杂二氧化钛或两者混合；
具体地，所述纳米粒子为纳米二氧化硅或铜颗粒或两者混合；
具体地，所述疏水改性剂为十七氟癸基三甲氧基硅烷或十八烷基硫醇或十八烷基三甲氧基硅烷中的一种或多种混合；
具体地，所述疏水胶黏剂为聚二甲基硅油或环氧树脂。
具体地，所述纳米粒子为不同粒径的纳米二氧化硅或铜颗粒混合。
实施例2
本发明一种抗菌抗黏附耐酸防污疏水牙齿保护剂的制备方法，制备过程包括以下步骤：
步骤1、按配比将纳米粒子和疏水改性剂加入到无水乙醇中疏水改性，得到疏水纳米粒子；
步骤2、将疏水胶黏剂和固化剂按配比搅拌均匀后，加入到含微量己烷的无水乙醇中搅拌分散，得到混合溶液A；
步骤3、按配比将步骤1中所得疏水纳米粒子和光响应抗菌剂加入到步骤2中所得到的混合溶液A中搅拌混匀即得到一种抗菌抗黏附耐酸防污疏水牙齿保护剂。
具体地，所述光响应抗菌剂的激发光源为波长在500-750nm的LED可见光。
实施例3
一种抗菌抗黏附耐酸防污疏水牙齿保护剂的制备方法，制备过程包括以下步骤：
步骤1、将大约2质量份的纳米二氧化硅加入到无水乙醇溶液中，再加入1质量份的十七氟癸基三甲氧基硅烷疏水改性，改性完过滤干燥保存；
步骤2、取大约1质量份的聚二甲基硅氧烷和0.1质量份的固化剂充分混合，加入到10质量份的含微量己烷的无水乙醇中混匀；
步骤3、将步骤1中制得的疏水纳米二氧化硅和0.02质量份的谈掺杂氧化锌加入到步骤2所制得的混合溶液中混匀，得到一种抗菌抗黏附耐酸防污疏水牙齿保护剂。
将按照上述步骤制得的抗菌抗黏附耐酸防污疏水牙齿保护剂盛装于喷雾瓶内，喷涂于小鼠切牙形成牙齿保护膜，通过酸蚀有保护膜保护和无保护膜保护的小鼠牙齿，并且用含菌食物喂养小鼠一段时间后观察牙齿的表面状况，同时将牙齿保护剂通过灌胃的方式灌进小鼠胃里观察小鼠组织反应变化；其结果如图1-6所示。
如图1所示为有牙齿保护剂覆盖的牙齿（左）和普通牙齿（右）的电镜对比图，由图中可以看出，覆盖有牙齿保护剂的牙齿，其表面具备微纳米粗糙结构，有利于实现超疏水，并且相比没有膜保护的牙齿，表面更干净且没有损坏，说明保护膜能够有效地抗包括细菌在内的各种物质黏附，能很好地保护牙齿；
如图2所示为牙齿保护剂覆盖牙齿后其表面接触角和滚动角示意图，由图中可以看出，覆盖有牙齿保护剂的牙齿，水滴在其表面的接触角和滚动角小，表明使用本发明制备的牙齿保护剂后，牙齿具有超疏水性，能有效防止食物残渣和细菌的黏附、牙齿色素沉着和降低龋齿和牙龈病等口腔疾病发生；
如图3所示为牙齿保护剂覆盖牙齿后其耐磨性和耐酸腐蚀性的曲线图，由图中可以看出，通过混合掺入不同粒径的纳米粒子的策略，可以使膜具有较好的耐磨性，同时该保护膜还表现出良好的抗酸蚀性，表明使用本发明制备的牙齿保护剂喷涂在牙齿上形成保护膜后，能够适应口腔复杂的环境；
如图4所示为覆盖有牙齿保护膜的牙齿在500-750nm波长的LED可见光源照射一段时间后的抗菌性培养结果示意图，由图中可以看出，经过500-750nm波长的LED可见光源照射后，覆盖有牙齿保护剂的牙齿，其细菌数量明显少于无保护牙齿组，表明本发明制备的牙齿保护剂能够在LED可见光照射下杀菌，且采用光源照射的杀菌方式不会对口腔组织产生刺激；
图5为小鼠牙齿抗酸蚀保护对比图，左边为牙齿保护膜的牙齿，右边为没有牙齿保护膜的牙齿，通过对比可以看出，没有牙齿保护膜的小鼠牙齿表面有明显的凹陷破坏痕迹，而保护膜牙齿表面的保护膜结构比较完整，表明覆盖有牙齿保护膜的小鼠牙齿能够有效避免因刺激性因素接触而导致的牙齿损伤。
图6为小鼠的相关组织HE染色结果示意图，由图中可以看出，牙齿保护剂灌胃的小鼠和纯水灌胃的小鼠心肝脾肺肾等组织HE染色差别不大，没有发现明显的淤血变性和炎症细胞等，表明本发明制备的牙齿保护剂的生物安全性高，可以作为口腔保健用品进行使用。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (7)
1.一种抗菌抗黏附耐酸防污疏水牙齿保护剂，其特征在于，该保护剂各组分按重量份表示为：
0.5~2份光响应抗菌剂；
0.5~2份纳米粒子；
0.1~1份疏水性改性剂；
50-150份疏水胶黏剂；
100~200份无水乙醇溶剂。
2.根据权利要求1所述的一种抗菌抗黏附耐酸防污疏水牙齿保护剂，其特征在于：
所述光响应抗菌剂为碳掺杂氧化锌或碳掺杂二氧化钛或两者混合；
所述纳米粒子为纳米二氧化硅或铜颗粒或两者混合；
所述疏水改性剂为十七氟癸基三甲氧基硅烷或十八烷基硫醇或十八烷基三甲氧基硅烷中的一种或多种混合；
所述疏水胶黏剂为聚二甲基硅油或环氧树脂。
3.根据权利要求2所述的一种抗菌抗黏附耐酸防污疏水牙齿保护剂，其特征在于，所述纳米粒子为不同粒径的纳米二氧化硅或铜颗粒混合。
4.一种抗菌抗黏附耐酸防污疏水牙齿保护剂的制备方法，其特征在于，包括以下步骤：
步骤1、按配比将纳米粒子和疏水改性剂加入到无水乙醇中疏水改性，得到疏水纳米粒子；
步骤2、将疏水胶黏剂和固化剂按配比搅拌均匀后，加入到含微量己烷的无水乙醇中搅拌分散，得到混合溶液A；
步骤3、按配比将步骤1中所得疏水纳米粒子和光响应抗菌剂加入到步骤2中所得到的混合溶液A中搅拌混匀即得到一种抗菌抗黏附耐酸防污疏水牙齿保护剂。
5.根据权利要求4所述的一种抗菌抗黏附耐酸防污疏水牙齿保护剂的制备方法，其特征在于，步骤1中纳米粒子、疏水改性剂加入到无水乙醇中的顺序为：先将纳米粒子加入到无水乙醇中，再加入疏水改性剂，改性完成后过滤干燥得到疏水纳米粒子。
6.根据权利要求4所述的一种抗菌抗黏附耐酸防污疏水牙齿保护剂的制备方法，其特征在于，所述光响应抗菌剂的激发光源为波长在500-750nm的LED可见光。
7.一种抗菌抗黏附耐酸防污疏水牙齿保护剂的应用，其特征在于，将牙齿保护剂盛装于喷雾瓶中用作喷剂，使用时将其喷涂至牙齿表面以形成保护膜，达到抗菌、抗黏附、耐酸、防污、疏水的目的。
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