CN113527748A - 一种聚醚醚酮表面改性方法及改性得到的聚醚醚酮及其应用 - Google Patents
一种聚醚醚酮表面改性方法及改性得到的聚醚醚酮及其应用 Download PDFInfo
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- CN113527748A CN113527748A CN202110783516.8A CN202110783516A CN113527748A CN 113527748 A CN113527748 A CN 113527748A CN 202110783516 A CN202110783516 A CN 202110783516A CN 113527748 A CN113527748 A CN 113527748A
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Abstract
本发明提供一种聚醚醚酮表面改性方法及改性得到的聚醚醚酮及其应用,所述改性方法包括以下步骤:(1)将聚醚醚酮进行表面预处理,形成表面微纳米结构;(2)使用多巴胺碱性溶液对步骤(1)表面预处理后的聚醚醚酮进行表面功能化,而后将其在生物相容性聚合物溶液中浸泡,在聚醚醚酮表面形成聚合物粘结层;(3)将步骤(2)得到的具有粘结层的聚醚醚酮与功能化生物活性纳米材料复合,完成对聚醚醚酮的表面改性。本发明的方法条件温和、容易控制、成本低效率高并且可以在复杂的植入体表面改性,改性后的PEEK具有良好的骨诱导性能和骨整合性能。
Description
技术领域
本发明属于生物材料领域,涉及一种聚醚醚酮表面改性方法及改性得到的聚醚醚酮及其应用。
背景技术
聚醚醚酮(PEEK)是一种半结晶性的高分子,结晶度在30-35%之间,玻璃化转化温度为143°,PEEK具有与人工骨相匹配的弹性模量、稳定的物理化学性质、良好的生物相容性、热稳定性和射线可透过性等优点,可以避免传统金属植入材料(钛,钛合金,不锈钢)带来的应力屏蔽而造成的骨吸收,离子析出和摩擦带来的炎症,以及需要二次手术和对检测带来的各种困难。同时PEEK具有良好的热塑性,可以通过注塑或者3D打印等制作需要的骨形状,因此被认为是下一代骨植入材料。但是PEEK同样也存在例如生物惰性,表明接触的骨组织无法与其形成化学键合,容易导致植入体松动。PEEK的骨整合能力差,一些研究表明,光滑的PEEK骨接触和周围的矿化区域较少,软骨和纤维组织包裹较多。这样的缺点也限制了PEEK在临床上的进一步使用,因此也有一些针对PEEK的这些缺点进行改性的方法。
通常的情况下,在PEEK内部增加生物活性物质,例如羟基磷灰石(HA)粉体、磷酸三钙、生物活性陶瓷,但是这种添加其他材料到PEEK块体的内部,第二相的添加会影响PEEK的整体力学性能。因此需要开发针对PEEK表面改性而不影响其整体力学性能的方法。刘宣勇等人公开了一种PEEK表面改性的方法(CN104497344A),采用离子注入的方法,可以在材料表面注入一些生物活性金属,例如钙、锌、镁等金属,也可以是银、铜等金属,可以使其表面具有抗菌性能。但是其不能在复杂的表面进行,例如卷曲的内孔和3D打印的复杂形状,缺乏与人体骨组织成分HA的活性,需要离子注入设备提高成本和制作时间。
因此,在本领域,期望开发一种条件温和、容易控制、成本低效率高并且可以在复杂的植入体表面改性(3D打印的骨植入内表面),且能够提高骨组织的生长速率、促进骨整合的改性方法,本发明改性得到的聚醚醚酮可以作为潜在的骨植入性材料,为PEEK向人工骨应用提供设计思路。
发明内容
针对现有技术的不足,本发明的目的在于提供一种聚醚醚酮(PEEK)表面改性方法及改性得到的聚醚醚酮及其应用。本发明的方法条件温和、容易控制、成本低效率高并且可以在复杂的植入体表面改性,特别适合3D打印的骨植入内表面,改性后的PEEK具有良好的骨诱导性能和骨整合性能。
为达到此发明目的,本发明采用以下技术方案:
一方面,本发明提供一种聚醚醚酮表面改性方法,所述改性方法包括以下步骤:
(1)将聚醚醚酮进行表面预处理,形成表面微纳米结构;
(2)使用多巴胺碱性溶液对步骤(1)表面预处理后的聚醚醚酮进行表面功能化,而后将其在生物相容性聚合物溶液中浸泡,在聚醚醚酮表面形成聚合物粘结层;
(3)将步骤(2)得到的具有粘结层的聚醚醚酮与功能化生物活性纳米材料复合,完成对聚醚醚酮的表面改性。
本发明中,通过预处理在聚醚醚酮表面形成微纳米结构,从而有利于细胞的粘附和骨整合,而后通过多巴胺表面功能化以及生物相容性聚合物在其表面形成粘结层,从而使得能够有效的吸附功能化的生物活性纳米材料,得到表面改性的聚醚醚酮,功能化的生物活性纳米材料可以进一步有效的提高成骨分化能力,促进新骨的形成。
本发明首先在医用PEEK表面形成微纳米结构的粘结层或过渡层,然后再在上面沉积或自主装具有良好生物活性的涂层,通过连续的沉积或生长,可在医疗材料或器械表面具有良好生物活性的涂层,该方法对医疗器械具有普适性,并且具有成分可调、厚度可变、快速制备等优点。
经过本发明方法改性的材料表面能够促进细胞成骨方向分化,增加细胞粘附和分化,促进骨整合性能。
优选地,步骤(1)所述表面预处理的方式为利用浓硫酸进行磺化处理、利用ICP等离子刻蚀进行处理或通过喷砂处理。相比较于离子注入等改性方式,利用硫酸刻蚀,ICP等离子体刻蚀或者喷砂处理的方式可以快速地在PEEK表面形成微纳米结构,从而有利于细胞的粘附和骨整合性能。
步骤(2)所述多巴胺碱性溶液为多巴胺的Tris-HCl溶液,其pH=8.5。
优选地,步骤(2)所述多巴胺碱性溶液的浓度为0.5~50mg/mL,例如0.8mg/mL、1mg/mL、5mg/mL、8mg/mL、10mg/mL、20mg/mL、30mg/mL、40mg/mL或50mg/mL。
优选地,步骤(2)所述使用多巴胺碱性溶液对步骤(1)表面预处理后的聚醚醚酮进行表面功能化的方法为:将步骤(1)表面预处理后的聚醚醚酮浸泡在多巴胺碱性溶液中1~48h(例如2h、4h、6h、8h、10h、12h、15h、18h、20h、24h、28h、30h、33h、35h、38h、40h、44h、46h或48h)。
优选地,步骤(2)所述生物相容性聚合物为蚕丝蛋白、海藻酸钠或硫酸软骨素。
优选地,步骤(2)所述生物相容性聚合物溶液的浓度为0.5~100mg/mL,例如0.8mg/mL、1mg/mL、5mg/mL、8mg/mL、10mg/mL、20mg/mL、30mg/mL、40mg/mL、50mg/mL、60mg/mL、70mg/mL、80mg/mL、90mg/mL或99mg/mL。
优选地,步骤(2)所述生物相容性聚合物溶液的溶剂为乙醇。
优选地,步骤(2)所述在生物相容性聚合物溶液中浸泡的时间为1~48h,例如2h、4h、6h、8h、10h、12h、15h、18h、20h、24h、28h、30h、33h、35h、38h、40h、44h、46h或48h。
在本发明中,PDA及生物聚合物(蚕丝蛋白,硫酸软骨素等)可以均匀的在其表面形成粘结层,该粘结层可以有效吸附功能化的无极纳米颗粒,实现不同的功能,不仅是在平面可以改性,对于复杂的结构,比如3D打印的PEEK植入物内孔也可以均匀形成功能化涂层。
优选地,步骤(3)所述功能化生物活性纳米材料为陶瓷材料或金属氧化物材料或生物蛋白中的任意一种或至少两种的组合。
优选地,所述陶瓷材料为羟基磷灰石(HA)和/或磷酸三钙(TCP)。
优选地,所述金属氧化物材料为ZnO和/或MgO。
优选地,步骤(3)所述复合为将步骤(2)得到的具有粘结层的聚醚醚酮浸没在功能化生物活性纳米材料溶液中反应1~48h,例如2h、4h、6h、8h、10h、12h、15h、18h、20h、24h、28h、30h、33h、35h、38h、40h、44h、46h或48h。
优选地,所述功能化生物活性纳米材料溶液中溶剂为乙醇。
优选地,所述功能化生物活性纳米材料溶液的浓度为0.1~100mg/mL,例如0.3mg/mL、1mg/mL、5mg/mL、8mg/mL、10mg/mL、20mg/mL、30mg/mL、40mg/mL、50mg/mL、60mg/mL、70mg/mL、80mg/mL、90mg/mL或99mg/mL。
在本发明中,表面功能化生物活性纳米材料,可以根据需要调整成分和比例,HA可以促进成骨,ZnO,MgO具有抗菌和促进骨生成的作用,表面功能化生物活性纳米材料也可以是其中几种的复合涂层。该表面功能化涂层可以进一步有效的提高成骨分化能力,促进新骨的形成。
另一方面,本发明提供一种通过如上所述改性方法得到的表面改性的聚醚醚酮。
另一方面,本发明提供了如上所述的表面改性的聚醚醚酮在骨植入材料制备中的应用。
相对于现有技术,本发明具有以下有益效果:
本发明的改性方法条件温和、容易控制、成本低效率高并且可以在复杂的植入体表面改性,改性后的PEEK具有良好的骨诱导性能和骨整合性能。
附图说明
图1为实施例1改性得到的聚醚醚酮的SEM图,其中标尺为5μm。
图2为实施例2改性得到的聚醚醚酮的SEM图,其中标尺为20μm。
图3为实施例5改性得到的聚醚醚酮的SEM图,其中标尺为200μm。
图4为实施例6改性得到的聚醚醚酮的SEM图,其中标尺为1mm。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。本领域技术人员应该明了,所述实施例仅仅是帮助理解本发明,不应视为对本发明的具体限制。
实施例1
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个平面的PEEK,使用硫酸磺化反应5min,使用去离子水冲洗表面,去除残余的硫酸,使用2mg/mL的PDA(其为多巴胺的Tris-HCl溶液,其pH=8.5,下同)聚合24h,得到PDA改性的PEEK,将改性后的PEEK浸没在2mg/mL蚕丝蛋白溶液(溶剂为乙醇,下同)中,反应12h,干燥后将其浸没在2mg/mL的HA溶液(其溶剂为乙醇,下同)中,反应2h后干燥,得到HA改性的PEEK。
利用扫描电镜(Tescan,Mira3)对得到的PEEK进行表征,得到如图1所示结果,由图1可以看出,表面由疏松的层状的结构组成。
实施例2
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个平面的PEEK,使用ICP刻蚀10min,使用去离子水冲洗表面,,使用2mg/mL的PDA聚合24h,得到PDA改性的PEEK,将改性后的PEEK浸没在2mg/mL蚕丝蛋白溶液中,反应2h,干燥后将其浸没在2mg/mL的HA溶液中,反应2h后干燥,得到HA改性的PEEK。
利用扫描电镜(Tescan Mira3)对得到的PEEK进行表征,得到如图2所示结果,由图2可以看出,表面由一层复合涂层构成。
实施例3
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个平面的PEEK,使用喷砂处理10min,使用去离子水冲洗表面,去除残余的硫酸,使用2mg/mL的PDA聚合24h,得到PDA改性的PEEK,将改性后的PEEK浸没在2mg/mL蚕丝蛋白溶液中,反应12h,干燥后将其浸没在2mg/mL的HA溶液中,反应12h后干燥,得到HA改性的PEEK。
实施例4
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个3D打印的PEEK支架,使用硫酸磺化反应5min,使用去离子水冲洗表面,去除残余的硫酸,使用2mg/mL的PDA聚合24h,得到PDA改性的PEEK,将改性后的PEEK浸没在2mg/mL蚕丝蛋白溶液中,反应24h,干燥后将其浸没在2mg/mL的HA溶液中,反应2h后干燥,得到HA改性的PEEK。
实施例5
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个3D打印的PEEK支架,使用硫酸磺化反应5min,使用去离子水冲洗表面,去除残余的硫酸,使用2mg/mL的PDA聚合24h,得到PDA改性的PEEK,将改性后的PEEK浸没在2mg/mL硫酸软骨素溶液中,反应12h,干燥后将其浸没在2mg/mL的HA溶液中,反应12h后干燥,得到HA改性的PEEK。
利用扫描电镜(Tescan,Mira3)对得到的PEEK进行表征,得到如图3所示结果,由图3可以看出,表面有一层厚厚的涂层,EDX能谱可以看到Ca、P是均匀分布在支架表面。
实施例6
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个3D打印的PEEK支架,使用硫酸磺化反应5min,使用去离子水冲洗表面,去除残余的硫酸,使用2mg/mL的PDA聚合24h,得到PDA改性的PEEK,将改性后的PEEK浸没在3mg/mL海藻酸钠溶液中,反应12h,干燥后将其浸没在2mg/mL的HA溶液中,反应12h后干燥,得到HA改性的PEEK。
利用扫描电镜对得到的PEEK进行表征,得到如图4所示结果,由图4可以看出,表面由一层厚的涂层组成。
实施例7
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个3D打印的PEEK支架,使用硫酸磺化反应40min,使用去离子水冲洗表面,去除残余的硫酸,使用50mg/mL的PDA聚合48h,得到PDA改性的PEEK,将改性后的PEEK浸没在100mg/mL蚕丝蛋白溶液中,反应20h,干燥后将其浸没在100mg/mL的磷酸三钙TCP溶液中,反应48h后干燥,得到TCP改性的PEEK。
实施例8
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个3D打印的PEEK支架,使用硫酸磺化反应30min,使用去离子水冲洗表面,去除残余的硫酸,使用10mg/mL的PDA聚合3h,得到PDA改性的PEEK,将改性后的PEEK浸没在60mg/mL蚕丝蛋白溶液中,反应10h,干燥后将其浸没在40mg/mL的ZnO溶液中,反应12h后干燥,得到ZnO改性的PEEK。
实施例9
本实施例提供一种聚醚醚酮表面改性方法,所述方法包括以下步骤:
取一个3D打印的PEEK支架,使用硫酸磺化反应10min,使用去离子水冲洗表面,去除残余的硫酸,使用2mg/mL的PDA聚合5h,得到PDA改性的PEEK,将改性后的PEEK浸没在5mg/mL蚕丝蛋白溶液中,反应1h,干燥后将其浸没在10mg/mL的MgO溶液中,反应1h后干燥,得到MgO改性的PEEK。
实施例1-9得到的改性聚醚醚酮由于有Ca、P的存在,使得其成骨诱导作用较好。
申请人声明,本发明通过上述实施例来说明本发明的工艺方法,但本发明并不局限于上述工艺步骤,即不意味着本发明必须依赖上述工艺步骤才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明所选用原料的等效替换及辅助成分的添加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。
Claims (10)
1.一种聚醚醚酮表面改性方法,其特征在于,所述改性方法包括以下步骤:
(1)将聚醚醚酮进行表面预处理,形成表面微纳米结构;
(2)使用多巴胺碱性溶液对步骤(1)表面预处理后的聚醚醚酮进行表面功能化,而后将其在生物相容性聚合物溶液中浸泡,在聚醚醚酮表面形成聚合物粘结层;
(3)将步骤(2)得到的具有粘结层的聚醚醚酮与功能化生物活性纳米材料复合,完成对聚醚醚酮的表面改性。
2.根据权利要求1所述的聚醚醚酮表面改性方法,其特征在于,步骤(1)所述表面预处理的方式为利用浓硫酸进行磺化处理、利用ICP等离子刻蚀进行处理或通过喷砂处理。
3.根据权利要求1或2所述的聚醚醚酮表面改性方法,其特征在于,步骤(2)所述多巴胺碱性溶液为多巴胺的Tris-HCl溶液,其pH=8.5;
优选地,步骤(2)所述多巴胺碱性溶液的浓度为0.5~50mg/mL;
优选地,步骤(2)所述使用多巴胺碱性溶液对步骤(1)表面预处理后的聚醚醚酮进行表面功能化的方法为:将步骤(1)表面预处理后的聚醚醚酮浸泡在多巴胺碱性溶液中1~48h。
4.根据权利要求1-3中任一项所述的聚醚醚酮表面改性方法,其特征在于,步骤(2)所述生物相容性聚合物为蚕丝蛋白、海藻酸钠或硫酸软骨素。
5.根据权利要求1-4中任一项所述的聚醚醚酮表面改性方法,其特征在于,步骤(2)所述生物相容性聚合物溶液的浓度为0.5~100mg/mL;
优选地,步骤(2)所述生物相容性聚合物溶液的溶剂为乙醇;
优选地,步骤(2)所述在生物相容性聚合物溶液中浸泡的时间为1~48h。
6.根据权利要求1-5中任一项所述的聚醚醚酮表面改性方法,其特征在于,步骤(3)所述功能化生物活性纳米材料为陶瓷材料或金属氧化物材料或生物蛋白中的任意一种或至少两种的组合。
7.根据权利要求6所述的聚醚醚酮表面改性方法,其特征在于,所述陶瓷材料为羟基磷灰石和/或磷酸三钙;
优选地,所述金属氧化物材料为ZnO和/或MgO。
8.根据权利要求1-7中任一项所述的聚醚醚酮表面改性方法,其特征在于,步骤(3)所述复合为将步骤(2)得到的具有粘结层的聚醚醚酮浸没在功能化生物活性纳米材料溶液中反应1~48h;
优选地,所述功能化生物活性纳米材料溶液中溶剂为乙醇;
优选地,所述功能化生物活性纳米材料溶液的浓度为0.1~100mg/mL。
9.一种通过如权利要求1-8中任一项所述聚醚醚酮表面改性方法得到的表面改性的聚醚醚酮。
10.根据权利要求9所述的表面改性的聚醚醚酮在骨植入材料制备中的应用。
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