CN105749339B - 一种尼龙纳米纤维三维交联大孔支架及其制备方法 - Google Patents
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Abstract
本发明涉及一种尼龙纳米纤维三维交联大孔支架及其制备方法，它采用在一定条件下静电纺丝纳米尼龙纤维膜，并将纤维膜在水中高速剪切成短纤维，分样后，加入一定大小的晶体碳酸钙颗粒作为致孔剂，经冷冻干燥成型，用稀盐酸去除碳酸钙致孔剂，水洗后用聚丙烯酸溶液交联，再经水洗、冷冻和冷冻干燥得到尼龙纳米纤维三维交联大孔支架。该支架具有大孔，适于细胞和组织的长入。尼龙纤维经聚丙烯酸交联后，纤维之间有较好的结合力，支架整体有较好的弹性和整体结构稳定性，可用于组织和器官的修复。
Description
技术领域
本发明涉及一种尼龙纳米纤维三维交联大孔支架及其制备方法，属于生物医用材料技术领域。
背景技术
尼龙是分子主链上含有重复酰胺基团-[NHCO]-的热塑性树脂总称，它具有良好力学性能、耐热性、耐磨损性、耐化学药品性和自润滑性，且摩擦系数低，有一定的阻燃性，易于加工，适于用玻璃纤维和其它填料填充增强改性，在工业中有广泛的应用。尼龙目前在生物材料领域也有广泛的应用，可被制成各种形状的支架材料用于骨、皮肤和心脏等器官和组织的修复（Suman Das 等，2003，Rapid Prototyping Journal, 9（1）:43-49）。在支架中，尼龙一般都制成实心结构，较少制成多孔网络状的纤维支架，使细胞、血管和神经等难以在支架内部生长。工业中可将尼龙纺丝成各种尺度的纤维，但由于尼龙纤维之间无结合力，将尼龙纤维制成三维多孔网络状的纤维支架是非常困难的。
发明内容
本发明的主要设想是采用静电纺丝的方法制备纳米尼龙薄膜，将尼龙薄膜在水中高速剪切成短纤维，得到尼龙纳米纤维的悬浮液，将悬浮分样后，加入一定大小的晶体碳酸钙致孔剂，经冷冻干燥成型，用稀盐酸去除碳酸钙致孔剂，水洗后用聚丙烯酸溶液交联，再经水洗、冷冻和冷冻干燥得到尼龙纳米纤维三维交联大孔支架。
本发明中尼龙纳米纤维三维交联大孔支架的制备方法具体如下所述。
(1)静电纺丝纳米尼龙纤维膜，配制一定浓度的尼龙溶液，溶剂为甲酸和水混合物，通以一定的纺丝电压静电纺丝形成纳米尼龙纤维膜。
(2)称取一定量的纳米尼龙纤维膜，加入到定量的水中，在水中高速剪切成短纤维。
(3)分样至称量瓶中，加入平均粒度在200～500μm之间的晶体碳酸钙致孔剂，在-18℃下冷冻成型并冻干。
(4)冻干后的样品用稀盐酸去除碳酸钙致孔剂，水洗后再用10%的聚丙烯酸溶液交联。
(5)交联后的支架经水洗，-18℃下冷冻成型，冷冻干燥可获得尼龙纳米纤维三维交联大孔支架。
本发明制得的尼龙纳米纤维三维交联大孔支架为白色圆盘，其形状和高度可在分样中采用不同的容器和分样体积调节。尼龙纳米纤维的直径可通过改变静电纺丝的工艺条件调节，支架具有大孔结构，尼龙纤维经聚丙烯酸交联后，纤维之间有较好的结合力，支架整体有较好的弹性和整体结构稳定性，可用于组织和器官的修复。该制备工艺简单，相比于单纯的静电纺丝法，该法可容易地制备三维结构的支架。
具体实施方式
下面结合具体实施例，对本发明内容作进一步的说明，但本发明的实现方式并不局限于此。
实施例1：分别取9ml的甲酸和1ml的水，混合均匀，称取1.0g尼龙6，搅拌溶解，静置2小时。将尼龙6溶液加入到注射器中，通以15kV的电压纺丝，收集在接地的铝箔上，可获得尼龙纤维平均直径80nm的薄膜。称取0.5g纳米尼龙纤维膜，在100ml水中高速剪切成短纤维，分样至称量瓶中，加入平均粒度为200μm的碳酸钙颗粒，高度与分样的液面相同，在-18℃下冷冻成型，在冻干机中冻干。冻干后的样品用稀盐酸去除碳酸钙致孔剂，水洗后再把样品浸泡在10%的聚丙烯酸溶液中交联，时间为2小时，取出交联支架，水洗，-18℃下冷冻，在冻干机中再次冻干可获得尼龙6纳米纤维三维交联大孔支架。
实施例2：分别取8ml的甲酸和2ml的水，混合均匀，称取2.0g尼龙66，搅拌溶解，静置2小时。将尼龙66溶液加入到注射器中，通以20kV的电压纺丝，收集在接地的铝箔上，可获得尼龙纤维平均直径150nm的薄膜。称取2.0g纳米尼龙66纤维膜，在100ml水中高速剪切成短纤维，分样至称量瓶中，加入平均粒度为500μm的碳酸钙颗粒，高度与分样的液面相同，在-18℃下冷冻成型，在冻干机中冻干。冻干后的样品用稀盐酸去除碳酸钙致孔剂，水洗后再把样品浸泡在10%的聚丙烯酸溶液中交联，时间为2小时，取出交联支架，水洗，-18℃下冷冻，在冻干机中再次冻干可获得尼龙66纳米纤维三维交联大孔支架。
Claims (6)
1.一种尼龙纳米纤维三维交联大孔支架，其特征在于在一定条件下静电纺丝纳米纤维尼龙膜，将纳米尼龙纤维膜在水中高速剪切成短纤维，分样后，加入具有一定粒度的晶体碳酸钙致孔剂，经冷冻干燥成型，用稀盐酸去除碳酸钙致孔剂，水洗后用聚丙烯酸溶液交联，再经水洗、冷冻和冷冻干燥得到尼龙纳米纤维三维交联大孔支架。
2.根据权利要求1所述的尼龙纳米纤维三维交联大孔支架，其特征在于所使用的尼龙为尼龙6或尼龙66。
3.根据权利要求1所述的尼龙纳米纤维三维交联大孔支架，其特征在于静电纺丝纳米纤维膜时，尼龙浓度为10.0%（w/v）或20.0%（w/v），溶剂为甲酸和水的混合物，体积比为90:10或80:20，纺丝电压为15kV或20kV。
4.根据权利要求1所述的尼龙纳米纤维三维交联大孔支架，其特征在于纳米尼龙纤维在水中高速剪切时的浓度为0.5%（w/v）或2%（w/v）。
5.根据权利要求1所述的尼龙纳米纤维三维交联大孔支架，其特征在于使用的碳酸钙致孔剂的粒度范围在200～500μm之间。
6.根据权利要求1所述的尼龙纳米纤维三维交联大孔支架，其特征在于使用的交联剂为10%的聚丙烯酸溶液。
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| CN1887365A (zh) * | 2006-08-01 | 2007-01-03 | 四川大学 | 具有多孔结构的生物材料膜及其制备方法 |
| CN104815355A (zh) * | 2015-04-16 | 2015-08-05 | 四川大学 | 表面具有纳米纤维多孔结构的羟基磷灰石/聚酰胺复合生物材料及其制备方法 |
| CN105107022A (zh) * | 2015-09-21 | 2015-12-02 | 东华大学 | 一种在湿态下具有压缩弹性的纳米纤维多孔支架的制备方法 |
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| CN1887365A (zh) * | 2006-08-01 | 2007-01-03 | 四川大学 | 具有多孔结构的生物材料膜及其制备方法 |
| CN104815355A (zh) * | 2015-04-16 | 2015-08-05 | 四川大学 | 表面具有纳米纤维多孔结构的羟基磷灰石/聚酰胺复合生物材料及其制备方法 |
| CN105107022A (zh) * | 2015-09-21 | 2015-12-02 | 东华大学 | 一种在湿态下具有压缩弹性的纳米纤维多孔支架的制备方法 |
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