CN114775266A - 负载氧化锌的抗菌仿血丝超短纤维及其制备方法和应用 - Google Patents
负载氧化锌的抗菌仿血丝超短纤维及其制备方法和应用 Download PDFInfo
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Abstract
一种负载氧化锌的抗菌仿血丝超短纤维及其制备方法和应用,其中方法包括:将红色颜料与聚酯塑料粒子进行共混,干燥,重新造粒形成纺丝用红色色母粒,再通过熔融纺丝得到仿血丝纤维长丝;向二水醋酸锌的乙醇溶液中缓慢滴加氢氧化锂的乙醇溶液,直至溶液呈现透明状,冷却至室温后得到纳米氧化锌溶胶;将仿血丝纤维长丝先经过碱性溶液处理后,再作为纤维载体浸润在纳米氧化锌溶胶中,取出后经轧水脱水、干燥、切割得到表面负载有纳米氧化锌粒子的抗菌仿血丝短纤维,抗菌仿血丝短纤维在沸水中进行沸水收缩并去除纤维表面油剂,最终得到负载氧化锌的抗菌仿血丝超短纤维。本发明制备方法操作简单、高效,成本低,效用持久。
Description
技术领域
本发明涉及纤维材料领域,具体涉及一种负载氧化锌的抗菌仿血丝超短纤维及其制备方法和应用。
背景技术
口腔医学的发展在一定程度上取决于材料学的发展,以生命科学、信息科学、材料科学为先导的新的科学技术革命,使新的材料层出不穷,也使口腔修复材料的发展日新月异。1936年德国人Walter Bauer首先采用悬浮聚合法制成(PMMA)用于口腔义齿基托修复,PMMA材料具有性能优越,操作简便,生物相容性能良好,易于抛光,色泽美观等优点,经过半个多世纪的发展,逐渐取代了传统的镍络合金基材料,成为临床制作义齿基托最为广泛应用的材料。但是,PMMA材料在常温下是玻璃态,质地较脆,在义齿基托材料服役环境中,口腔咀嚼反复变形和不平衡咀嚼,极易使基托材料产生弹性疲劳和应力,造成PMMA基义齿基托材料的开裂,折断,最终导致修复失败。
此外,PMMA义齿基托长期在口腔中进行佩戴,细菌真菌极易在其表面繁殖,菌斑大量粘附,成为口腔健康隐患,许多研究表明义齿性口炎是佩戴活动义齿后常见并发症状,并且患者长期佩戴的发病率较高,如何能够研发出具有良好抗菌性能和力学性能的塑料基托材料是一个挑战。为了提高PMMA义齿基托的各项性能和服役表现,人们提出了许多方法以提高其机械性能和抗菌活性,但少有人意识到,除了PMMA材料本身的机械性能和抗菌性之外,PMMA义齿材料的仿生美观性也日益受到人们重视,由于真实的口腔环境和牙体组织是布满血丝的浅红色外观,目前常用的方法是在聚合义齿基托材料所用的牙托粉中加入镉红等颜料,但是镉红颜料也仅能提供浅红色的外观效果,无法赋予义齿基托材料仿血丝的外观。义齿基托材料中还有添加红色仿血丝纤维,可以达到媲美真实牙体组织的效果,但针对义齿基托填料用红色仿血丝的相关研究很少。而且现阶段基托树脂抗菌领域无法做到对基托本身力学性能、颜色美观性、抗菌成分长期有效性等各方面地协调发展,并且所添加抗菌成分的生物安全性也有待提高。
发明内容
基于此,本发明提供了一种负载氧化锌的抗菌仿血丝超短纤维及其制备方法和应用,以解决现有技术的基托树脂抗菌领域无法做到对基托本身力学性能、颜色美观性、抗菌成分长期有效性等各方面协调发展,并且所添加抗菌成分的生物安全性不高的技术问题。
为实现上述目的,本发明提供了一种负载氧化锌的抗菌仿血丝超短纤维,其包括纤维载体,以及负载于纤维载体表面的纳米氧化锌粒子,该纤维载体由红色颜料与聚酯塑料共混制备得到。
作为本发明的进一步优选技术方案,所述纤维载体负载纳米氧化锌粒子后形成的负载氧化锌的抗菌仿血丝超短纤维的直径为0.005-0.1mm,长度为0.7-5mm。
根据本发明的另一方面,本发明还提供了一种负载氧化锌的抗菌仿血丝超短纤维的制备方法,包括以下步骤:
1)将红色颜料与聚酯塑料粒子进行共混,干燥,在机械挤出设备上重新造粒形成纺丝用红色色母粒,将红色色母粒通过熔融纺丝得到仿血丝纤维长丝;
2)将二水醋酸锌作为前驱体加入到无水乙醇溶液中,充分搅拌溶解得到二水醋酸锌的乙醇溶液;将一水氢氧化锂加入无水乙醇中,超声溶解得到氢氧化锂的乙醇溶液;再在50-60℃的磁力搅拌下,缓慢向二水醋酸锌的乙醇溶液中滴加氢氧化锂的乙醇溶液,直至溶液呈现透明状,冷却至室温后得到纳米氧化锌溶胶;
3)将步骤1)中得到的仿血丝纤维长丝先通过碱性溶液进行碱处理,之后再作为纤维载体浸润在步骤2)制备的纳米氧化锌溶胶中,取出后依次进行轧水脱水、干燥、切割处理,得到表面负载有纳米氧化锌粒子的抗菌仿血丝短纤维,再将抗菌仿血丝短纤维放入沸水中进行沸水收缩并去除纤维表面油剂,最终得到负载氧化锌的抗菌仿血丝超短纤维。
作为本发明的进一步优选技术方案,步骤1)中的红色颜料为颜料红149和颜料红202中的一种;红色颜料与聚酯塑料粒子的质量比为3-20:80-97。
作为本发明的进一步优选技术方案,步骤1)中红色色母粒的含水率小于50ppm,熔融纺丝的纺丝温度为200-300℃,纺丝牵伸倍率为2-5倍,牵伸辊温度为25-85℃,热定型温度为90-170℃,仿血丝纤维长丝的直径为0.005-0.03mm。
作为本发明的进一步优选技术方案,步骤2)中,二水醋酸锌与一水氢氧化锂的摩尔比例为1:1-1:3。
作为本发明的进一步优选技术方案,步骤3)中,仿血丝纤维长丝先通过浸润于NaOH的碱性溶液中进行碱处理,碱性溶液中NaOH质量浓度为20-60%,浸润时间为10-30分钟,之后再浸润于纳米氧化锌溶胶中10-15分钟;进行轧水脱水的带液率为70-85%;采用热风实现干燥,温度为50-120℃,时间为10-20min。
作为本发明的进一步优选技术方案,步骤3)中,经切割得到的抗菌仿血丝短纤维的长度为1-7.5mm;抗菌仿血丝短纤维进行沸水处理的时间为10min,沸水处理后得到的负载氧化锌的抗菌仿血丝超短纤维的直径为0.005-0.1mm,长度为0.7-5mm。
根据本发明的又一方面,本发明还提供了一种负载氧化锌的抗菌仿血丝超短纤维的应用,将上述负载氧化锌的抗菌仿血丝超短纤维的制备方法得到的抗菌仿血丝超短纤维与聚甲基丙稀酸甲酯复合制备得到义齿基托修复材料。
本发明的负载氧化锌的抗菌仿血丝超短纤维及其制备方法和应用,采用上述技术方案,可以达到如下有益效果:
1)本发明提供的负载氧化锌的抗菌仿血丝超短纤维的制备方法,通过将仿血纤维长丝进行碱处理,使纤维表面富含羟基,有利于后续氧化锌溶胶充分接枝,以及通过溶胶凝胶法原位聚合生成透明的纳米氧化锌溶胶,之后将纳米氧化锌溶胶与碱处理后的仿血丝纤维长丝进行充分浸润、轧水,并在热风环境下进行干燥,以使纤维表面均匀包裹纳米氧化锌溶胶,且在高温干燥条件下,纳米氧化锌溶胶进一步聚合为凝胶,以在纤维表面自然生成纳米氧化锌粒子,且溶胶凝胶转换过程为无色透明,而且对仿血丝纤维的外观无任何影响;
2)本发明提供的负载氧化锌的抗菌仿血丝超短纤维的制备方法,纤维长丝在切割前通过浸润于纳米氧化锌溶胶并干燥之后,纤维弯曲度有明显下降,弹性模量有所提升,可明显改善纤维长丝的切割熔融现象,且延长切割设备使用寿命并明显改善切割后短纤维的分散性;
3)本发明提供的负载氧化锌的抗菌仿血丝超短纤维的制备方法,通过沸水处理使纤维长度能够收缩至1mm以内的长度,且经过沸水后,使得纤维载体上的纤维油剂得到冲洗、稀释,有利于改善负载氧化锌的抗菌仿血丝超短纤维在聚甲基丙稀酸甲酯的粉体中的分散性,可以达到1分钟以内实现单丝完全分散,简化量产中搅拌时间并提升义齿基托树脂中仿血丝纤维的外观表现,使外观更加接近真实口腔中布满血丝的外观;
4)本发明提供的负载氧化锌的抗菌仿血丝超短纤维的制备方法,方法操作简单、高效,成本低,效用持久,应用前景广阔;
5)本发明提供的负载氧化锌的抗菌仿血丝超短纤维的应用,通过本发明制备的提供的负载氧化锌的抗菌仿血丝超短纤维加入聚甲基丙稀酸甲酯的粉体中,可以快速分散,而且制备的义齿基托修复材料具有良好的韧性,由于负载氧化锌的抗菌仿血丝超短纤维在义齿基托修复材料中均匀分散,更加接近人体口腔组织血丝外观,特别是负载于仿血丝纤维表面的纳米氧化锌纳米粒子具有抗菌缓释作用,可有效抑制义齿基托修复材料在口腔环境中的细菌滋生,从而有利于人体健康。
具体实施方式
下面将通过具体实施方式,对本发明做进一步描述。较佳实施例中所引用的如“上”、“下”、“左”、“右”、“中间”及“一”等用语,仅为便于叙述的明了,而非用以限定本发明可实施的范围,其相对关系的改变或调整,在无实质变更技术内容下,当亦视为本发明可实施的范畴。
本发明提供了一种负载氧化锌的抗菌仿血丝超短纤维,其包括仿血丝纤维,仿血丝纤维表面负载有纳米氧化锌溶胶,该仿血丝纤维由红色颜料与聚酯塑料共混制备得到。
优选地,所述负载氧化锌的抗菌仿血丝超短纤维的直径为0.005-0.1mm,长度为0.7-5mm。
为了让本领域技术人员更好地理解并实现本发明的技术方案,以下通过具体实施例对本发明负载氧化锌的抗菌仿血丝超短纤维的制备方法及其应用做进一步地详细说明。
实施例1-4
实施例1-4为四组实例分别采用相同的方法制备负载氧化锌的抗菌仿血丝超短纤维,不同之处在于制备过程中采用了如表1所示的不同工艺参数,具体制备过程如下:
S1、将红色颜料或与聚酯塑料粒子进行共混并充分干燥使含水率小于50ppm,红色颜料与聚酯塑料粒子的质量比为3-20:80-97,再经双螺杆挤出重新造粒,得到纺丝用红色色母粒,将红色色母粒通过熔融纺丝得到仿血丝纤维长丝,其中,熔融纺丝的纺丝温度为200-300℃,纺丝牵伸倍率为2-5倍,牵伸辊温度为25-85℃,热定型温度为90-170℃,得到直径为0.005-0.03mm的仿血丝纤维长丝,通过色彩分析仪测量仿血丝纤维长丝的色度RGB值为R:140-255,G:0-178,B:0-190,所用的红色颜料为颜料149或颜料红202中的一种。
S2、将二水醋酸锌作为前驱体加入到无水乙醇溶液中,充分搅拌溶解得到二水醋酸锌的乙醇溶液;将一水氢氧化锂加入无水乙醇中,超声使其溶解得到氢氧化锂的乙醇溶液;在60℃磁力搅拌下,缓慢向二水醋酸锌的乙醇溶液滴加氢氧化锂的乙醇溶液,直至溶液呈现透明状,冷却至室温后得到纳米氧化锌溶胶溶液,其中,二水醋酸锌与一水氢氧化锂的用量比例为1:1-1:3。
S3、将步骤S1中得到的仿血丝纤维长丝先浸润于NaOH碱性溶液中进行碱处理,碱性溶液中NaOH的质量浓度为20-60%,浸润时间为10-30分钟,之后再将碱处理后的仿血纤维长丝作为纤维载体浸润在步骤S2制备的氧化锌溶胶中,浸润时间为10-15分钟,取出后进行轧水脱水,带液率为80%,之后在热风环境中进行吹风干燥,热风干燥温度为50℃-100℃,时间为10-20min;将干燥后的纤维喂入纤维切断设备中进行切割,切割成长度为1-7.5mm的负载氧化锌的抗菌仿血丝短纤维,再经过沸水处理10min进行沸水收缩并去除纤维表面油剂,最终得长度为0.7-5mm的负载氧化锌的抗菌仿血丝超短纤维。
表1.实施例1-4负载氧化锌的抗菌仿血丝超短纤维制备方法中的工艺参数
对实施例1-4的产物采用光学显微镜投影法测试,测得产物负载氧化锌的抗菌仿血丝超短纤维直径为0.005-0.1mm,长度为0.7-5mm,结合表1根据放入沸水前、后的纤维长度进行计算,得到产物的沸水收缩率为10%-50%;通过观察负载氧化锌的抗菌仿血丝超短纤维的截面,其为圆形、中空圆形、椭圆形或葫芦形。
实施例5
负载氧化锌的抗菌仿血丝超短纤维的应用
将0.2g实施例1制得的负载氧化锌的抗菌仿血丝超短纤维与10g聚甲基丙稀酸甲酯进行混合,然后再加入6.5ml甲基丙烯酸溶液并进行充分搅拌,待溶液呈现胶团状后放入模具中进行热压,制备得到义齿基托样条。
按《中华人民共和国医药行业标准YY0270-2003》中的相关规定将义齿基托样条尺寸设计为64mm*10mm*3mm,数量为5个,进行三点弯曲试验,跨距为50mm,使加荷杆从零开始均匀加荷,加载速度为5mm/min,直至义齿基托样条断裂,得到的5个义齿基托样条的弯曲模量为2587MPa±113MPa,弯曲强度为98MPa±21Mpa,表明具有良好的韧性,相比纯的或添加其他填料的聚甲基丙稀酸甲酯材料的义齿基托,机械性能有明显提升;采用接触震荡法对制得的5个义齿基托样条进行抗菌性测试,测试结果为:对大肠杆菌的抗菌率>92%,对变形链球菌的抗菌率>73%,能很好地满足了口腔医学抗菌要求。
虽然以上描述了本发明的具体实施方式,但是本领域熟练技术人员应当理解,这些仅是举例说明,可以对本实施方式做出多种变更或修改,而不背离本发明的原理和实质,本发明的保护范围仅由所附权利要求书限定。
Claims (9)
1.一种负载氧化锌的抗菌仿血丝超短纤维,其特征在于,包括纤维载体,以及负载于纤维载体表面的纳米氧化锌粒子,该纤维载体由红色颜料与聚酯塑料共混制备得到。
2.根据权利要求1所述的负载氧化锌的抗菌仿血丝超短纤维,其特征在于,所述纤维载体负载纳米氧化锌粒子后形成的负载氧化锌的抗菌仿血丝超短纤维的直径为0.005-0.1mm,长度为0.7-5mm。
3.一种权利要求1或2所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法,其特征在于,包括以下步骤:
1)将红色颜料与聚酯塑料粒子进行共混,干燥,在机械挤出设备上重新造粒形成纺丝用红色色母粒,将红色色母粒通过熔融纺丝得到仿血丝纤维长丝;
2)将二水醋酸锌作为前驱体加入到无水乙醇溶液中,充分搅拌溶解得到二水醋酸锌的乙醇溶液;将一水氢氧化锂加入无水乙醇中,超声溶解得到氢氧化锂的乙醇溶液;再在50-60℃的磁力搅拌下,缓慢向二水醋酸锌的乙醇溶液中滴加氢氧化锂的乙醇溶液,直至溶液呈现透明状,冷却至室温后得到纳米氧化锌溶胶;
3)将步骤1)中得到的仿血丝纤维长丝先通过碱性溶液进行碱处理,之后再作为纤维载体浸润在步骤2)制备的纳米氧化锌溶胶中,取出后依次进行轧水脱水、干燥、切割处理,得到表面负载有纳米氧化锌粒子的抗菌仿血丝短纤维,再将抗菌仿血丝短纤维放入沸水中进行沸水收缩并去除纤维表面油剂,最终得到负载氧化锌的抗菌仿血丝超短纤维。
4.根据权利要求3所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法,其特征在于,步骤1)中的红色颜料为颜料红149和颜料红202中的一种;红色颜料与聚酯塑料粒子的质量比为3-20:80-97。
5.根据权利要求3所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法,其特征在于,步骤1)中红色色母粒的含水率小于50ppm,熔融纺丝的纺丝温度为200-300℃,纺丝牵伸倍率为2-5倍,牵伸辊温度为25-85℃,热定型温度为90-170℃,仿血丝纤维长丝的直径为0.005-0.03mm。
6.根据权利要求3所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法,其特征在于,步骤2)中,二水醋酸锌与一水氢氧化锂的摩尔比例为1:1-1:3。
7.根据权利要求3所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法,其特征在于,步骤3)中,仿血丝纤维长丝先通过浸润于NaOH的碱性溶液中进行碱处理,碱性溶液中NaOH质量浓度为20-60%,浸润时间为10-30分钟,之后再浸润于纳米氧化锌溶胶中10-15分钟;进行轧水脱水的带液率为70-85%;采用热风实现干燥,温度为50-120℃,时间为10-20min。
8.根据权利要求3所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法,其特征在于,步骤3)中,经切割得到的抗菌仿血丝短纤维的长度为1-7.5mm;抗菌仿血丝短纤维进行沸水处理的时间为10min,沸水处理后得到的负载氧化锌的抗菌仿血丝超短纤维的直径为0.005-0.1mm,长度为0.7-5mm。
9.一种负载氧化锌的抗菌仿血丝超短纤维的应用,其特征在于,所述应用中,将权利要求3-8任一项所述的负载氧化锌的抗菌仿血丝超短纤维的制备方法得到的抗菌仿血丝超短纤维与聚甲基丙稀酸甲酯复合制备得到义齿基托修复材料。
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