CN114712564A - 一种组织修复用可降解纳米短纤维材料及其制备方法 - Google Patents
一种组织修复用可降解纳米短纤维材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种组织修复用可降解纳米短纤维材料及其制备方法,属于组织修复材料领域,包括纳米短纤维和亲水性基础材料,所述纳米短纤维保持结晶形态均匀分散于亲水性基础材料中,所述纳米短纤维为聚酯材料,所述聚酯材料为聚乙交酯或聚丙交酯。本方案利用水溶性基础材料和纳米短纤维之间的溶解性差异,将纳米短纤维均匀分散在水溶性基础材料中,形成二级网络结构,保持了两种材料各自的优点,并将缺点互补,得到了力学性能优异、生物相容性好,生物可降解性好、对血管等组织的损伤小的优点,可以在人体组织内保持较好的拉伸强度和断裂伸长率,又可以大幅度的提高材料的拉伸强度,特别适用于较小面积或深层缺损的组织修复。
Description
技术领域
本发明涉及组织修复材料技术领域,具体为一种组织修复用可降解纳米短纤维材料及其制备方法。
背景技术
人体内的各种组织、器官都有可能发生异常或损伤,目前主要依靠组织、器官的移植来恢复其功能,在此过程中需要大量的生物材料来支持组织、器官的正常工作,如支架、结扎夹等,具有良好生物相容性和生物可降解性的材料由于可以随着细胞的进一步增殖和分化以及材料的降解、吸收,最终形成新的功能组织,达到修复缺损组织的目的,因而在市场中的需求也越来越大。
采用单组份的高分子原料制备成的组织修复材料断裂伸长率较高,柔韧性好,对血管等组织的损伤小,但是也存在以下不足,如降解速度较慢,拉伸强度差,脱落需1-2个月,完全吸收则需6个月以上,而临床上血管及其他管状组织闭合时间仅为1-2周,组织修复材料长期在人体中存在潜在风险,此外血管或其他组织仍可能出现受损、出血等现象,不利于患者的康复;而采用两种材料简单的接枝或共聚,其组成比例、链段分布、分子量等不易稳定控制,材料的力学性能和生物可降解性很难同时符合要求,因而不能充分满足组织修复材料的临床需求,故提出一种组织修复用可降解纳米短纤维材料及其制备方法。
发明内容
(一)解决的技术问题
1.要解决的技术问题
针对现有技术中存在的问题,本发明的目的在于提供一种组织修复用可降解纳米短纤维材料及其制备方法,解决上述的问题。
(二)技术方案
为实现上述目的,本发明提供如下技术方案:
一种组织修复用可降解纳米短纤维材料,包括纳米短纤维和亲水性基础材料,所述纳米短纤维保持结晶形态均匀分散于亲水性基础材料中,所述纳米短纤维为聚酯材料,所述聚酯材料为聚乙交酯或聚丙交酯,所述亲水性基础材料为胶原、明胶、透明质酸、壳聚糖、丝素、纤维素和淀粉中的任一种或任两种。
优选的,所述纳米短纤维为高结晶性纳米短纤维,其中当纳米短纤维为聚乙交酯时,其结晶度为80~90%,取向因子为0.90~0.95;当纳米短纤维为聚丙交酯时,其结晶度为70~80%,取向因子为0.65~0.75。
优选的,所述纳米短纤维的直径为300~500nm,长度为50~100μm。
优选的,所述纳米短纤维的堆叠密度为0.02~0.06g/cm3。
本发明要解决的另一技术问题是提供一种组织修复用可降解纳米短纤维材料的制备方法,包括以下步骤:
①将聚酯材料在100℃下真空干燥24h,在氮气保护下,置于纺丝装置螺杆中熔融,在电压8~30KV下,以恒定速度挤出喷丝,漩涡冷却液槽接收后得到直径6~10μm的聚酯纤维束;所述聚酯材料为聚乙交酯或聚丙交酯;
②在氮气保护下,将步骤①所得聚酯纤维束经过两次热拉伸,每次拉伸倍数为5~8倍,得到直径300~500nm的纳米纤维;
当步骤①所得聚酯纤维束的材料为聚乙交酯时两次热拉伸的温度分别为180℃和160℃;当步骤①所得聚酯纤维束的材料为聚丙交酯时两次热拉伸的温度分别为150℃和130℃;
③将步骤②所得纳米纤维置于-100℃以下的液氮中深冷2~3小时,经过高速粉碎机粉碎后过筛,得到长度为50~100μm的纳米短纤维;
④用溶剂将亲水性基础材料配置成质量浓度为10~20%溶液,向其中加入步骤③所得的纳米短纤维,搅拌分散均匀,得到混合液;
⑤步骤④得到的混合液加入模具中冷冻成型,然后置于冷冻干燥机中冷冻干燥除去溶剂,得到组织修复用可降解纳米短纤维材料。
优选的,所述溶剂为水或醋酸。
(三)有益效果
与现有技术相比,本发明提供了一种组织修复用可降解纳米短纤维材料及其制备方法,具备以下有益效果:
(1)本方案利用水溶性基础材料和纳米短纤维之间的溶解性差异,将纳米短纤维均匀分散在水溶性基础材料中,形成二级网络结构,保持了两种材料各自的优点,并将缺点互补,得到了力学性能优异、生物相容性好,生物可降解性好、对血管等组织的损伤小的优点,可以在人体组织内保持较好的拉伸强度和断裂伸长率,又可以大幅度的提高材料的拉伸强度,特别适用于较小面积或深层缺损的组织修复。
(2)在降解过程中,由于纳米短纤维的聚酯材料如聚乙交酯或聚丙交酯的水解比较快,一般在30天后会在结扎夹的内部形成区域酸性环境,加速基础材料的降解,将基础材料的吸收时间由原来的180天大幅缩短为90天,并且无异物不良反应的产生。
(3)当临床应用遇到组织液或者血液时,亲水性基础材料亲水变软,聚酯材料疏水保持不变,形成软硬段储能结构,在保留其亲水性和生物相容性好的特点下,显著增强其拉伸强度、径向支撑力和回弹性等力学性能,该材料适用于组织补片、防粘连、止血等组织修复和再生领域。
具体实施方式
下面将结合本发明的实施例,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。
实施例一:
一种组织修复用可降解纳米短纤维材料,包括纳米短纤维和亲水性基础材料,纳米短纤维保持结晶形态均匀分散于亲水性基础材料中,纳米短纤维为聚酯材料,聚酯材料为聚乙交酯或聚丙交酯,亲水性基础材料为胶原、明胶、透明质酸、壳聚糖、丝素、纤维素和淀粉中的任一种或任两种。
进一步的,纳米短纤维为高结晶性纳米短纤维,其中当纳米短纤维为聚乙交酯时,其结晶度为80%,取向因子为0.90;当纳米短纤维为聚丙交酯时,其结晶度为70%,取向因子为0.65。
进一步的,纳米短纤维的直径为300nm,长度为50μm。
进一步的,纳米短纤维的堆叠密度为0.02g/cm3。
一种组织修复用可降解纳米短纤维材料的制备方法,包括以下步骤:
①将聚酯材料在100℃下真空干燥24h,在氮气保护下,置于纺丝装置螺杆中熔融,在电压8KV下,以恒定速度挤出喷丝,漩涡冷却液槽接收后得到直径6μm的聚酯纤维束;聚酯材料为聚乙交酯或聚丙交酯;
②在氮气保护下,将步骤①所得聚酯纤维束经过两次热拉伸,每次拉伸倍数为5倍,得到直径300nm的纳米纤维;
当步骤①所得聚酯纤维束的材料为聚乙交酯时两次热拉伸的温度分别为180℃和160℃;当步骤①所得聚酯纤维束的材料为聚丙交酯时两次热拉伸的温度分别为150℃和130℃;
③将步骤②所得纳米纤维置于-100℃以下的液氮中深冷2小时,经过高速粉碎机粉碎后过筛,得到长度为50μm的纳米短纤维;
④用溶剂将亲水性基础材料配置成质量浓度为10%溶液,向其中加入步骤③所得的纳米短纤维,搅拌分散均匀,得到混合液;
⑤步骤④得到的混合液加入模具中冷冻成型,然后置于冷冻干燥机中冷冻干燥除去溶剂,得到组织修复用可降解纳米短纤维材料。
进一步的,溶剂为水或醋酸。
实施例二:
一种组织修复用可降解纳米短纤维材料,包括纳米短纤维和亲水性基础材料,纳米短纤维保持结晶形态均匀分散于亲水性基础材料中,纳米短纤维为聚酯材料,聚酯材料为聚乙交酯或聚丙交酯,亲水性基础材料为胶原、明胶、透明质酸、壳聚糖、丝素、纤维素和淀粉中的任一种或任两种。
进一步的,纳米短纤维为高结晶性纳米短纤维,其中当纳米短纤维为聚乙交酯时,其结晶度为85%,取向因子为0.93;当纳米短纤维为聚丙交酯时,其结晶度为75%,取向因子为0.70。
进一步的,纳米短纤维的直径为400nm,长度为75μm。
进一步的,纳米短纤维的堆叠密度为0.04g/cm3。
一种组织修复用可降解纳米短纤维材料的制备方法,包括以下步骤:
①将聚酯材料在100℃下真空干燥24h,在氮气保护下,置于纺丝装置螺杆中熔融,在电压19KV下,以恒定速度挤出喷丝,漩涡冷却液槽接收后得到直径8μm的聚酯纤维束;聚酯材料为聚乙交酯或聚丙交酯;
②在氮气保护下,将步骤①所得聚酯纤维束经过两次热拉伸,每次拉伸倍数为6.5倍,得到直径400nm的纳米纤维;
当步骤①所得聚酯纤维束的材料为聚乙交酯时两次热拉伸的温度分别为180℃和160℃;当步骤①所得聚酯纤维束的材料为聚丙交酯时两次热拉伸的温度分别为150℃和130℃;
③将步骤②所得纳米纤维置于-100℃以下的液氮中深冷2.5小时,经过高速粉碎机粉碎后过筛,得到长度为75μm的纳米短纤维;
④用溶剂将亲水性基础材料配置成质量浓度为15%溶液,向其中加入步骤③所得的纳米短纤维,搅拌分散均匀,得到混合液;
⑤步骤④得到的混合液加入模具中冷冻成型,然后置于冷冻干燥机中冷冻干燥除去溶剂,得到组织修复用可降解纳米短纤维材料。
进一步的,溶剂为水或醋酸。
实施例三:
一种组织修复用可降解纳米短纤维材料,包括纳米短纤维和亲水性基础材料,纳米短纤维保持结晶形态均匀分散于亲水性基础材料中,纳米短纤维为聚酯材料,聚酯材料为聚乙交酯或聚丙交酯,亲水性基础材料为胶原、明胶、透明质酸、壳聚糖、丝素、纤维素和淀粉中的任一种或任两种。
进一步的,纳米短纤维为高结晶性纳米短纤维,其中当纳米短纤维为聚乙交酯时,其结晶度为90%,取向因子为0.95;当纳米短纤维为聚丙交酯时,其结晶度为80%,取向因子为0.75。
进一步的,纳米短纤维的直径为500nm,长度为100μm。
进一步的,纳米短纤维的堆叠密度为0.06g/cm3。
一种组织修复用可降解纳米短纤维材料的制备方法,包括以下步骤:
①将聚酯材料在100℃下真空干燥24h,在氮气保护下,置于纺丝装置螺杆中熔融,在电压30KV下,以恒定速度挤出喷丝,漩涡冷却液槽接收后得到直径10μm的聚酯纤维束;聚酯材料为聚乙交酯或聚丙交酯;
②在氮气保护下,将步骤①所得聚酯纤维束经过两次热拉伸,每次拉伸倍数为8倍,得到直径500nm的纳米纤维;
当步骤①所得聚酯纤维束的材料为聚乙交酯时两次热拉伸的温度分别为180℃和160℃;当步骤①所得聚酯纤维束的材料为聚丙交酯时两次热拉伸的温度分别为150℃和130℃;
③将步骤②所得纳米纤维置于-100℃以下的液氮中深冷3小时,经过高速粉碎机粉碎后过筛,得到长度为100μm的纳米短纤维;
④用溶剂将亲水性基础材料配置成质量浓度为20%溶液,向其中加入步骤③所得的纳米短纤维,搅拌分散均匀,得到混合液;
⑤步骤④得到的混合液加入模具中冷冻成型,然后置于冷冻干燥机中冷冻干燥除去溶剂,得到组织修复用可降解纳米短纤维材料。
进一步的,溶剂为水或醋酸。
以上所述,仅为本发明较佳的具体实施方式;但本发明的保护范围并不局限于此。任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其改进构思加以等同替换或改变,都应涵盖在本发明的保护范围内。
Claims (7)
1.一种组织修复用可降解纳米短纤维材料,其特征在于:包括纳米短纤维和亲水性基础材料,所述纳米短纤维保持结晶形态均匀分散于亲水性基础材料中,所述纳米短纤维为聚酯材料,所述聚酯材料为聚乙交酯或聚丙交酯,所述亲水性基础材料为胶原、明胶、透明质酸、壳聚糖、丝素、纤维素和淀粉中的任一种或任两种。
2.根据权利要求1所述的一种组织修复用可降解纳米短纤维材料,其特征在于:所述纳米短纤维为高结晶性纳米短纤维,其中当纳米短纤维为聚乙交酯时,其结晶度为80~90%,取向因子为0.90~0.95;当纳米短纤维为聚丙交酯时,其结晶度为70~80%,取向因子为0.65~0.75。
3.根据权利要求1所述的一种组织修复用可降解纳米短纤维材料,其特征在于:所述纳米短纤维的直径为300~500nm,长度为50~100μm。
4.根据权利要求1所述的一种组织修复用可降解纳米短纤维材料,其特征在于:所述纳米短纤维的堆叠密度为0.02~0.06g/cm3。
5.根据权利要求1所述的一种组织修复用可降解纳米短纤维材料,其特征在于:所述纳米短纤维和在组织修复用可降解纳米短纤维材料中的占比为25~30%。
6.一种组织修复用可降解纳米短纤维材料的制备方法,其特征在于,包括以下步骤:
①将聚酯材料在100℃下真空干燥24h,在氮气保护下,置于纺丝装置螺杆中熔融,在电压8~30KV下,以恒定速度挤出喷丝,漩涡冷却液槽接收后得到直径6~10μm的聚酯纤维束;所述聚酯材料为聚乙交酯或聚丙交酯;
②在氮气保护下,将步骤①所得聚酯纤维束经过两次热拉伸,每次拉伸倍数为5~8倍,得到直径300~500nm的纳米纤维;
当步骤①所得聚酯纤维束的材料为聚乙交酯时两次热拉伸的温度分别为180℃和160℃;当步骤①所得聚酯纤维束的材料为聚丙交酯时两次热拉伸的温度分别为150℃和130℃;
③将步骤②所得纳米纤维置于-100℃以下的液氮中深冷2~3小时,经过高速粉碎机粉碎后过筛,得到长度为50~100μm的纳米短纤维;
④用溶剂将亲水性基础材料配置成质量浓度为10~20%溶液,向其中加入步骤③所得的纳米短纤维,搅拌分散均匀,得到混合液;
⑤步骤④得到的混合液加入模具中冷冻成型,然后置于冷冻干燥机中冷冻干燥除去溶剂,得到组织修复用可降解纳米短纤维材料。
7.根据权利要求6所述的一种组织修复用可降解纳米短纤维材料的制备方法,其特征在于:所述溶剂为水或醋酸。
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