CN108755137A - 一种抗凝血的纺织基人造血管材料及其制备方法 - Google Patents

一种抗凝血的纺织基人造血管材料及其制备方法 Download PDF

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CN108755137A
CN108755137A CN201810575419.8A CN201810575419A CN108755137A CN 108755137 A CN108755137 A CN 108755137A CN 201810575419 A CN201810575419 A CN 201810575419A CN 108755137 A CN108755137 A CN 108755137A
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anticoagulant
blood vessel
artificial blood
preparation
vessel material
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陈莹
王鸿达
张勤
黄丽君
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Beijing Institute Fashion Technology
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Abstract

本发明涉及一种抗凝血的纺织基人造血管材料及其制备方法，其特征在于在聚酯织物表面聚合具有抗凝血性的聚吡咯(polypyrrole,PPy)涂层，该涂层为微纳结构使其具有良好的疏水性能，进而提高抗凝血效果。同时，涂层内还可掺杂一些低表面能物质，进一步提高抗凝血效果。制备时，首先对聚酯材料进行碱减量或等离子体前处理，然后采用化学聚合或电化学聚合工艺将吡咯单体涂覆到前处理过的材料表面。本发明所提供的人造血管材料具有，抗凝血效果好，制备工艺简单、成本低、安全可靠的优点。

Description

一种抗凝血的纺织基人造血管材料及其制备方法
技术领域
本发明属于人造血管材料技术领域，特别是涉及一种聚吡咯改性聚酯织物的抗凝血纺织基人造血管材料。
背景技术
心血管疾病正日益威胁着人类的健康，而血管移植是解决血管疾病的有效方法。纺织基人造血管具有成型方式简单、织品力学性能优良等优点，特别是涤纶(PET)机织血管在大口径人造血管中已有很好的应用。但直径小于6mm的PET机织小口径人造血管易形成血栓或内膜异常增生从而导致移植后远期通畅率低，尚不能满足临床应用需求，内膜增生和血栓的形成是人造血管材料与人体组织、血液的界面相互作用的结果，如人造血管材料血液和细胞不相容、顺应性的不匹配和人造血管内壁与人体血管壁表面结构的不匹配等，都会引起移植区域血液成分、血流动力学参数的扰动及变化。
由于其优良的机械力学性能和应用于大中口径人造血管时较好的生物稳定性，PET仍是该领域受到高度关注的材料之一。若再能提高涤纶和PTT等聚酯材料的血液相容性，便有望使聚酯材料成功应用于小口径人造血管中。
优异的抗凝血性和诱导内皮化能力成为心血管材料表面生物功能化的双重要求，也是进一步发展与应用的关键。根据ISO的标准定义血液相容性涵盖了凝血系统、血栓激活系统和免疫系统等，而良好的血液相容性是指材料与血液接触后不引起血小板粘附激活，不引发凝血、溶血，不引发免疫激活，使血液保持正常的流动态并体现正常生理功能。血液相容性的影响因素繁多，除血液固有成分外，材料表面界面特征起着决定性作用。目前，材料表面界面特征优化及改性已成为提高其血液相容性的重要途径。抗凝血高分子生物材料的表面设计包括微相分离结构、亲(疏)水性表面、负电荷表面、生物活性分子化表面、内皮细胞化表面、两性离子化表面等。如：公开号为US 2015/0352265 A1的专利利用聚乙烯吡咯烷酮在中空纤维膜的表面进行改性，然后涂覆季胺盐和肝素混合物。公开号为WO 2011/007196 A1提供了一种利用纳米粒子涂层增加抗凝血性能的方法，可有效防止脆断等力学现象。中国专利(申请号201610547453.5)公开了一种磺化聚丙烯无纺布抗凝血材料的制备方法。中国专利(申请号201510948201.9)涉及一种壳聚糖复合N-二苯亚甲基-氨基-甘氨酸苄酯抗凝血材料的制备方法，属于抗凝血材料制备领域。然而至今仅有少量肝素相关产品在临床上得到运用，而内皮细胞生长的相关研究仍然是较为复杂和长久的课题，因此亟需开发针对提高抗凝血性能的PET表面改性新材料。
发明内容
为克服上述不足，本发明提供一种聚吡咯改性聚酯的人造血管材料及其制备方法。所述血管材料具有抗凝血性能，能同时满足外用或体内植入的组织器官修复材料所需求的良好抗凝血性、生物相容性等多方面性能要求。
本发明的技术方案如下：
一种抗凝血的纺织基人造血管材料，其特征在于在聚酯织物表面聚合具有抗凝血性的聚吡咯(polypyrrole,PPy)涂层；PPy是一种具有优良电化学活性和生物相容性的导电高分子，能够支持细胞的粘附、迁移、增殖以及改善细胞与材料界面的相互作用，聚酯织物上聚合具有抗凝血性的PPy，可改变织物与血液的界面相互作用，提高其抗凝血性。
进一步的，所述PPy涂层为微纳结构，包括颗粒、膜、纳米线等不同形式；该涂层最大接触角为122°，具有良好的疏水性能，进一步提高抗凝血效果。微纳结构可通过不同的溶剂如乙醇与水、乙腈与水混合液等，软硬模板如磺酸盐型阴离子表面活性剂蒽醌-2-磺酸钠盐(AQS)等，还原氧化石墨烯等制备；
进一步的，所述PPy涂层含有低表面能掺杂剂，所述掺杂剂包括含氟化合物、烷烃类化合物(十二烷基苯磺酸、十二烷基磺酸等)；通过低表面能掺杂剂的使用可进一步提高疏水效果，进一步提高抗凝血性能。
进一步的，所述聚酯织物包括PET(涤纶)、PTT(聚对苯二甲酸丙二醇酯)；
本方案PPy的加入使得各种材料的抗凝血程度得到提高，血液在PPy复合聚酯材料表面血液的凝固时间延长；PPy复合聚酯材料不易粘连血小板；
本发明还提供了纺织基人造血管材料的制备方法，具体方案如下：
一种抗凝血的纺织基人造血管材料制备方法，首先对聚酯材料进行碱减量或等离子体等前处理，然后采用化学聚合或电化学聚合工艺将吡咯单体涂覆到前处理过的材料表面。
所述碱减量工艺如下：将大块交织物试样除杂烘干后剪裁成小块，然后将其与NaOH溶液、促进剂溶液按一定比例混合后放入染色小样机中处理，然后拿出织物小样，冲洗干净烘干。
进一步的，所述促进剂为1127溶液(十二烷基二甲基苄基氯化铵)
进一步的，所述NaOH溶液浓度为20～40g/L、促进剂溶液浓度为0.5～1g/L；所述NaOH溶液与促进剂溶液浴比为1∶50～1∶30
所述聚合工艺，其特征在于在乙醇、水的混合溶液中原位聚合。以一定比例配制乙醇与水的混合溶液，倒入烧杯，然后加入吡咯，搅拌均匀后将处理过的织物放入，同时加入氧化剂，在低温条件下反应。反应结束后拿出织物冲洗干净，放入烘箱烘干。
所述聚合工艺，其特征在于在乙腈、水的混合溶液中原位聚合。在溶剂中加入吡咯，搅拌均匀后降温，将前处理过的织物放入，称取氧化剂倒入，搅拌均匀，低温条件下反应。反应结束后拿出织物冲洗干净，放入烘箱烘干。
所述聚合工艺，其特征在于在吡咯水溶液中加入一定质量的表面活性剂如十六烷基三甲基溴化铵(CTAB)、甲基橙、木质素磺酸钠、蒽醌-2-磺酸钠盐(AQS)等充当软模板，再将前处理后的织物放入，冰水浴反应一定时间。再缓慢向混合液中滴加氧化剂冰水浴反应一段时间。反应结束后取出清洗烘干。
本制备方法具有：工艺简单、成本低、安全可靠的优点。
附图说明
图1为PPy改性聚酯材料的电镜照片；
图2为PPy改性PET/PTT织物的接触角；
图3为PPy改性PET/PTT织物对血小板的粘附效果。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
一种抗凝血的纺织基人造血管材料，其特征在于在聚酯织物表面聚合具有抗凝血性的聚吡咯涂层；所述PPy涂层可为微纳结构，包括颗粒、膜、纳米线等不同形式；所述PPy涂层还可含有低表面能掺杂剂，所述掺杂剂包括含氟化合物、烷烃类化合物(十二烷基苯磺酸、十二烷基磺酸等)。
一种抗凝血的纺织基人造血管材料制备方法，首先对聚酯材料进行碱减量或等离子体等前处理，然后采用聚合工艺将吡咯单体涂覆到前处理过的材料表面。
其中，改变NaOH浓度、碱处理时间、碱处理温度及促进剂浓度等条件均能对PET和PTT进行碱减量，同时使得纤维在碱减量后断裂强力满足实验要求。
抗凝血性能测量：将各种处理样的织物放入100ml的烧杯的底部中心，在37℃恒温水浴下保温5min后，用注射器向织物上滴下0.25ml抗凝全血，保温处理10min后，向血液中注入0.02mol/L的氯化钙水溶液0.2ml，开始计时，摇晃烧杯l min，使当中的血液和氯化钙溶液可以充分混合，盖好烧杯，在5、15、30、45min时，将各烧杯取出并加入50ml的蒸馏水，摇晃烧杯10min，取上清液，用分光光度计在λmax波长处测量各组样品的吸光度，每个吸光度测量3次，并取其平均值。利用扫描电镜观察不同条件下的材料对血小板粘附性能的影响。
减量率计算方法：
式中：W0为碱减量处理前的重量(g)；W1为碱减量处理后的重量(g)。
抗凝血程度计算方法：
BCI(抗凝血程度)＝(Is/Iw)×100％
Is：血液、氯化钙溶液与样品接触一定时间后的吸光度值；
Iw：血液与50ml蒸馏水混合后液体的吸光度值。
下面通过一些具体实施例来进行介绍
实施例1
将一大块PET/PTT交织物试样除杂后烘干，然后裁剪成10cm*8cm大的小块。配制40g/L NaOH、1g/L1227溶液，按照1:50的浴比，将织物小样和溶液放入染色小样机中，90℃温度条件下处理20min，然后拿出织物小样，冲洗干净后烘干。
在乙醇水的混合溶液中聚合。按照浴比，计算出聚合实验中所需溶液的体积，以乙醇与水的体积比为2:8的比例来配制溶液，倒入烧杯，然后加入吡咯，吡咯的浓度为0.6mol/L，搅拌均匀后降温至0～5℃将处理过的织物小样放入烧杯中，同时加入20ml的FeCl3溶液，浓度为0.3mol/L，在0～5℃条件下反应4h。反应结束后拿出织物冲洗干净，放入烘箱70℃烘干。然后做抗凝血性能测试。
实施例2
将一大块PET/PTT交织物试样除杂后烘干，然后裁剪成10cm*8cm大的小块。配制40g/L NaOH、1g/L1227溶液，按照1:50的浴比，将织物小样和溶液放入染色小样机中，90℃温度条件下处理20min，然后拿出织物小样，冲洗干净后烘干。
在乙腈水的混合溶液中聚合。按照浴比，计算出聚合实验中所需溶液的体积，以乙腈与水的体积比为1:9的比例来配制溶液，倒入烧杯，然后加入吡咯，吡咯的浓度为0.6mol/L，搅拌均匀后降温至0～5℃，将织物小样放入烧杯中，称取10g过硫酸铵(APS)，用25ml的水溶解后倒入烧杯中，搅拌均匀，在0～5℃条件下反应4h。反应结束后拿出织物冲洗干净，放入烘箱70℃烘干。然后做抗凝血性能测试。
实施例3
将一大块PET/PTT交织物试样除杂后烘干，然后裁剪成10cm*8cm大的小块。配制40g/L NaOH、1g/L1227溶液，按照1:50的浴比，将织物小样和溶液放入染色小样机中，90℃温度条件下处理20min，然后拿出织物小样，冲洗干净后烘干。
在十六烷基三甲基溴化铵(CTAB)模板中进行聚合。按照浴比，计算出所需溶液的体积，首先确定CTAB与吡咯的摩尔比为1:2，称取11g CTAB溶于200ml的蒸馏水中，倒入烧杯，再加入4.2ml的Py(吡咯)，搅拌均匀后降温至0～5℃，称取20g APS并用25ml的蒸馏水溶解，将织物小样放入烧杯中，再将APS倒入烧杯后搅拌均匀，在0～5℃条件下反应4h，反应结束后拿出织物冲洗干净，70℃烘干。改变CTAB和Py的用量，分别控制CTAB/Py的摩尔比为1:2,1:5,1:10，重复上述实验步骤。然后做抗凝血性能测试。
实例结果如下：
聚合聚吡咯后的电镜照片如图1所示(实施例1)，在聚酯材料的表面可看到有微纳米颗粒构成的聚吡咯镀层。该镀层使得改性后的聚酯材料最大接触角为122°，具有良好的疏水性能，如图2所示。
在凝血测试中，如表1～表4所示，聚吡咯的加入对抗凝血性能有很大的提高，上述三种聚合方法所得到的聚吡咯改性PET/PTT材料都比未改性的聚酯材料抗凝血性能提高，在乙腈溶液中聚合得到的织物的抗凝血值最高，抗凝血性最好。扫描电镜观察如图3所示，聚吡咯改性PET/PTT材料的表面粘连较少的血小板细胞，由此说明聚吡咯涂覆在PET/PTT材料表面能减少材料表面血小板的粘附。
表1. 5min时不同织物样品的吸光度值及抗凝血程度
表2. 15min时不同织物样品的吸光度值及抗凝血程度
表3. 30min时不同织物样品的吸光度值及抗凝血程度
表4. 45min时不同织物样品的吸光度值及抗凝血程度

Claims (10)

1.一种抗凝血的纺织基人造血管材料，其特征在于，在聚酯织物表面聚合具有抗凝血性的PPy涂层。
2.根据权利要求1所述的一种抗凝血的纺织基人造血管材料，其特征在于，所述聚酯织物包括PET或PTT。
3.根据权利要求1或2所述的一种抗凝血的纺织基人造血管材料，其特征在于，所述涂层为颗粒、膜或纳米线形的纳微结构。
4.根据权利要求1或2所述的一种抗凝血的纺织基人造血管材料，其特征在于，所述涂层还含有低表面能掺杂剂，所述掺杂剂包括含氟化合物、烷烃类化合物。
5.一种抗凝血的纺织基人造血管材料制备方法，其特征在于，首先对聚酯材料进行碱减量或等离子体前处理，然后采用聚合工艺将吡咯单体涂覆到前处理过的材料表面。
6.根据权利要求5所述的一种抗凝血的纺织基人造血管材料制备方法，其特征在于，所述碱减量工艺如下：将大块交织物试样除杂烘干后剪裁成小块，然后将其与NaOH溶液、促进剂溶液按一定比例混合后放入染色小样机中处理，然后拿出织物小样，冲洗干净烘干。
7.根据权利要求6所述的一种抗凝血的纺织基人造血管材料制备方法，其特征在于，所述促进剂为十二烷基二甲基苄基氯化铵；所述NaOH溶液浓度为20～40g/L、促进剂溶液浓度为0.5～1g/L；所述NaOH溶液与促进剂溶液浴比为1∶50～1∶30。
8.根据权利要求5所述的一种抗凝血的纺织基人造血管材料制备方法，其特征在于，所述聚合工艺，在乙醇/乙腈与水的混合溶液中原位聚合；以一定比例配制乙醇/乙腈与水的混合溶液，倒入烧杯，然后加入吡咯，搅拌均匀后将处理过的织物放入，同时加入氧化剂，在低温条件下反应，反应结束后拿出织物冲洗干净，放入烘箱烘干。
9.根据权利要求5所述的一种抗凝血的纺织基人造血管材料制备方法，其特征在于，所述聚合工艺，在吡咯水溶液中加入一定质量的表面活性剂充当软模板，再将前处理后的织物放入，冰水浴反应一定时间，再缓慢向混合液中滴加氧化剂冰水浴反应一段时间，反应结束后取出清洗烘干。
10.根据权利要求9所述的一种抗凝血的纺织基人造血管材料制备方法，其特征在于，所述表面活性剂为十六烷基三甲基溴化铵(CTAB)、甲基橙、木质素磺酸钠或蒽醌-2-磺酸钠盐(AQS)等。
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