CN115177777A - 一种压电促愈型创面修复辅助材料的制备方法 - Google Patents
一种压电促愈型创面修复辅助材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种压电促愈型创面修复辅助材料的制备方法，其方法是首先通过静电纺丝法制备聚偏氟乙烯、聚（偏氟乙烯‑三氟乙烯）或聚（偏氟乙烯‑四氟乙烯）静电纺丝微钠纤维膜作为压电层，然后将其通过具有自粘功能的导电粘合材料粘附于导电粘合材料的一面，该二层结构共同构成压电促愈型创面修复辅助材料，该整体可以粘附于现有多种类型的创面治疗材料上，其作用是与现有的多种类型创面修复材料/敷料共同使用，通过压电层产生的压电效应提供电刺激，通过导电粘合材料传导到创面四周达到对创面的电刺激治疗作用，以加快创面愈合速度和提高创面修复效果。该方法制备的压电促愈型创面修复辅助材料可联合各类型伤口敷料进行应用。
Description
技术领域
本发明涉及一种压电促愈型创面修复辅助材料的制备方法，属于材料领域。
背景技术
在各种外伤中，皮肤的损伤最为常见，严重的皮肤损伤、慢性皮肤创伤若不能得到有效治疗，不仅会使皮肤丧失原有功能，还会引起整个身体一系列复杂的病理、生理变化，包括水、电解质和酸碱平衡失调、休克、感染以及败血症等，造成人员伤亡。为了重建皮肤的屏障功能，有必要使用适当的创面敷料作为受损皮肤的临时替代品，结合一些新兴护理技术进行治疗，如电刺激等。随着医学、材料学等领域的研究进展，伤口敷料及新兴治疗手段都在不断的进步发展。长期以来，如何快速、精确、安全、有效地治疗皮肤创伤、加快愈合时间、提高愈合质量是创伤愈合领域的研究热点。
研究发现，使用伤口敷料和一些辅助治疗手段有助于伤口愈合。如用封闭敷料保持干净且湿润的伤口环境，有助于加速再上皮化和改变炎症环境，以利于更好的愈合；电刺激已被证明是有益于伤口愈合的。创伤敷料与护理能够对伤口的愈合起到正面的促进作用。现代创面敷料其成分有活性细胞、天然细胞外基质、天然高分子及其衍生物、合成聚合物等，现代敷料还具有多种多样的结构特征，包括膜、水胶体、水凝胶、泡沫、纤维毡、液体敷料、复合结构等。
生理微电流对人体的作用影响已有多年的研宄历史，生理微电流普遍存在于人体组织。未受损的人体皮肤具有内源性电位和10-60 mV的经皮电流电位。在皮肤受伤后，电流流经伤口路径会产生横向电场，这被称为“受伤电流”，损伤电流被认为是伤口启动修复的重要因素。当上皮细胞因损伤而分解时，电位差异就会消失，这种电位的丧失是启动细胞迁移和再上皮化的最早的刺激信号，包括人的角质形成细胞在内的许多上皮细胞都具有检测电场并进行定向迁移的能力。许多研究都表明电刺激是促进伤口愈合的有效治疗手段。2002年，美国食品和药物管理局批准电刺激设备在临床上用于治疗某些慢性伤口（例如，糖尿病、淤血和动脉溃疡等）。目前，已有许多临床研究报告了电刺激对于伤口愈合的积极结果，并在临床实践中用于加速伤口闭合。因此，目前许多学者主张将电刺激疗法与标准伤口护理结合使用。
目前，电刺激治疗需要专用设备，临床上的电刺激设备具有使用不便，需要专人操作等缺陷，能够产生电刺激的敷料具有更广泛的应用场景，能够满足更多的应用需求。压电材料是指受到压力作用时会在两端面间出现电压的晶体材料，其原理是具有压电性的晶体对称性较低，当受到外力作用发生形变时，晶胞中正负离子的相对位移使正负电荷中心不再重合，导致晶体发生宏观极化，而晶体表面电荷面密度等于极化强度在表面法向上的投影，所以压电材料受压力作用形变时两端面会出现异号电荷。压电材料在受力形变过程中能够产生电信号，且安全、便捷，能够在不需外接电源情况下实现对伤口的电刺激治疗。压电材料分为无机压电材料，如压电陶瓷，与有机压电材料，又称压电聚合物。如聚偏氟乙烯家族，是发现最早的，已经被证实了的铁电压电聚合物之一。对高分子材料来说，其成型工艺对其性能以及应用有较大影响。如果用作生物材料，要求材料安全无毒、具有较好的生物相容性外，对材料的结构也有一定的要求。静电纺丝是一种特殊的纤维制造工艺，聚合物溶液或熔体在强电场中进行喷射纺丝，在电场作用下，针头处的液滴会由球形变为圆锥形（即“泰勒锥”），并从圆锥尖端延展得到纤维细丝。这种方式可以生产出微米级、纳米级直径的聚合物细丝。
将压电材料与现有敷料相结合，能够发挥二者的优势达到双重促愈的效果，现有普通伤口敷料能够有效覆盖创面，为伤口愈合创造一个适宜愈合环境，压电材料在上层能够对伤口起到一个电刺激的疗效，也避免了压电材料作为一种较为惰性的材料与伤口直接接触不能创造良好伤口愈合环境的弊端。为了保证压电材料产生的电信号能够更好的传导到伤口处及伤口四周，并且需要无创地将压电材料附加到现有伤口敷料上，使用具有粘附性能的导电水凝胶将压电层与现有普通敷料相结合，压电层与导电粘合材料共同作为一种压电促愈型创面修复辅助材料。使用时当下层普通敷料是湿性的或具有一定导电效果时，对添加的压电促愈型创面修复辅助材料面积大小可以无特殊大小及形态要求；当下层普通敷料是无导电效果时，添加的压电促愈型创面修复辅助材料面积略大于下层普通敷料，上层敷料附件可直接无创粘附到正常皮肤上，对伤口四周产生电刺激效果。
发明内容
1.一种压电促愈型创面修复辅助材料的制备方法，其特征是：
（1）静电纺丝液的配制：量取30~45体积份的丙酮与55~70体积份的N,N-二甲基甲酰胺混合成100体积份的溶剂，将质量浓度为8%~25%的聚偏氟乙烯聚合物溶于上述混合溶剂中，随后以聚合物干重记，加入其质量分数为0%~15%的季铵盐，0%~0.5%的纳米粒子，搅拌均匀，备用；
（2）静电纺丝微纳纤维膜压电层的制备：纺丝液使用前经超声除泡0~60 min；将除泡后的溶液装入静电纺丝用注射器中，接上导电针头，并将注射器装入推注器中，设置推注速度为0.5~1 ml/h，将高压电源连接至导电针头上；在接受滚筒上包裹一层铝箔纸，将负压电源连接至接收滚筒，打开滚筒开关，设置转速为100~1000 rpm。随后，打开负压，调节负压为-1~2 kV；打开高压电源，调节电压至15~30 kV，设置纺丝时间为2~12h。纺丝结束后，关闭高压、负压电源，使用接地安全棒去除残留静电，关闭其它开关，取下铝箔纸，将其置于真空干燥箱中干燥或通风橱中自然风干；
（3）促愈型创面治疗附件材料的制备：将制备得到的静电纺丝微纳纤维膜压电层粘附到导电粘附材料上，获得压电促愈型创面修复辅助材料。
2.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的聚偏氟乙烯聚合物是指聚偏氟乙烯、聚（偏氟乙烯-三氟乙烯）、聚（偏氟乙烯-四氟乙烯）。
3.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的季铵盐只是四丁基氯化铵、甲基三乙基氯化铵、双十二烷基二甲基氯化铵、双十八烷基二甲基氯化铵。
4. 根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的纳米粒子是指石墨烯、氧化石墨烯、碳纳米管、纳米四氧化三铁、纳米钛酸钡、纳米二氧化钛、纳米二氧化硅等碳纳米材料、金属纳米材料及金属氧化物纳米材料。
5. 根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的导电粘合材料是指细胞毒性合格的导电粘合水凝胶、导电粘合剂和导电粘合膜等具有导电和自粘功能的材料。
6. 根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其特征在于该方法制备的压电促愈型创面修复辅助材料可联合各类型伤口敷料用于创伤修复。
本发明具有以下优点：
（1）制备得到的压电层——聚偏氟乙烯聚合物静电纺丝微钠纤维膜具有良好的压电性能，体外实验证实其产生的电刺激能够促进细胞迁移、增殖，以SD大鼠全层皮肤缺损模型考察其促进伤口修复的能力，证实添加和不添加压电层的敷料处理后的伤口具有不同的愈合速率，添加压电层的敷料在大鼠日常活动中产生的电刺激能够明显促进伤口愈合；
（2）制备得到的压电层——聚偏氟乙烯聚合物静电纺丝微钠纤维膜具有良好的生物相容性，细胞毒性实验表明其细胞毒性符合体表使用要求，细胞可以在材料上良好的粘附生长；
（3）制备得到的压电层——聚偏氟乙烯聚合物静电纺丝微钠纤维膜对皮肤无致敏反应，使用中可以与皮肤直接接触；
（4）制备得到的压电促愈型创面修复辅助材料解决了现有电刺激疗法需要单独依靠额外设备来使用的缺陷，扩大了电刺激疗法在伤口修复领域的应用范围及应用方式；
（5）制备得到的压电促愈型创面修复辅助材料具有自粘性能，能够与现有的大部分敷料如藻酸盐敷料、脱细胞真皮基质敷料、水凝胶敷料等等结合使用，不影响下层敷料的功效发挥；
（6）制备得到的压电促愈型创面修复辅助材料能发挥电刺激疗法的功效，将电刺激疗法与普通敷料相结合，与现有敷料达成双重协同促愈作用；
（7）制备得到的压电促愈型创面修复辅助材料可随意裁剪，可以适应任何形状及大小的伤口及伤口敷料；
（8）该制备方法操作简单，易于实施，对环境要求不苛刻，对操作人员友好；
（9）制备得到的压电促愈型创面修复辅助材料可以作为广泛适用型的附件运用到现有的各种常规敷料上，从而提高现有各种常规敷料的促愈功能，适用范围广。
具体实施方式
下面通过实施例对本发明进行具体的描述，有必要在此指出的是本实施例只用于对本发明进行进一步说明，而不能理解为对本发明保护范围的限制，该领域的技术熟练人员可以根据上述发明的内容作出一些非本质的改进和调整。
实施例1
（1）聚偏氟乙烯静电纺丝液的配制：称取3.24 g聚偏氟乙烯溶于20 ml N,N-二甲基甲酰胺——丙酮混合溶剂中，N,N-二甲基甲酰胺与丙酮的体积比为7:3，随后加入0.3g双十二烷基二甲基氯化铵和0.01 g 纳米四氧化三铁，室温下搅拌过夜；
（2）聚偏氟乙烯静电纺丝膜的制备：将纺丝液超声除泡后，转移至静电纺丝注射器中，接上导电针头，并将注射器装入推注器中，设置推注速度为1 ml/h，将高压电源连接至导电针头上；在接受滚筒上包裹一层铝箔纸，将负压电源连接至接收滚筒，打开滚筒开关，设置转速为500 rpm。随后，调节负压为-1kV；打开高压电源，调节高压至18 kV，设置纺丝时间为3 h。纺丝结束后，关闭高压、负压电源，使用接地安全棒去除残留静电，关闭其它开关，取下铝箔纸，将其置于通风橱中自然风干；
（3）压电促愈型创面修复辅助材料的制备：将制备得到的聚偏氟乙烯静电纺丝膜裁剪成10cm宽的正方形直接粘附到同样大小的基于多巴胺和碳纳米管的导电粘附水凝胶上，获得压电促愈型创面修复辅助材料。
实施例2
（1）聚（偏氟乙烯-三氟乙烯）静电纺丝液的配制：量取27 mlN,N-二甲基甲酰胺和23 ml丙酮混合后，称取5.4g聚偏氟乙烯溶于混合溶剂中，随后加入0.4g四丁基氯化铵，搅拌混合均匀；
（2）聚偏氟乙烯静电纺丝膜的制备：将纺丝液超声除泡后，转移至静电纺丝注射器中，接上导电针头，并将注射器装入推注器中，设置推注速度为0.6 ml/h，将高压电源连接至导电针头上；在接受滚筒上包裹一层铝箔纸，将负压电源连接至接收滚筒，打开滚筒开关，设置转速为800 rpm。随后，调节负压为-1kV；打开高压电源，调节高压至25kV，设置纺丝时间为5 h；同时开启5台静电纺丝机，纺丝结束后，关闭高压、负压电源，使用接地安全棒去除残留静电，关闭其它开关，取下铝箔纸，将其置于通风橱中自然风干；
（3）压电促愈型创面修复辅助材料的制备：将制备得到的聚（偏氟乙烯-三氟乙烯）静电纺丝膜裁剪成若干15 cm的圆片直接粘附到同样大小的基于多巴胺和还原的氧化石墨烯的导电粘附水凝胶上，获得压电促愈型创面修复辅助材料。
实施例3
（1）聚偏氟乙烯——聚（偏氟乙烯-三氟乙烯）静电纺丝液的配制：量取6 ml N,N-二甲基甲酰胺和4 ml丙酮混合后，称取0.6g聚偏氟乙烯和0.6g聚（偏氟乙烯-三氟乙烯）溶于混合溶剂中，随后加入0.004g氧化石墨烯，搅拌混合均匀；
（2）聚偏氟乙烯——聚（偏氟乙烯-三氟乙烯）静电纺丝膜的制备：将纺丝液超声除泡后，转移至静电纺丝注射器中，接上导电针头，并将注射器装入推注器中，设置推注速度为0.8 ml/h，将高压电源连接至导电针头上；在接受滚筒上包裹一层铝箔纸，将负压电源连接至接收滚筒，打开滚筒开关，设置转速为1000 rpm。随后，调节负压为-2kV；打开高压电源，调节高压至28kV，设置纺丝时间为4 h；纺丝结束后，关闭高压、负压电源，使用接地安全棒去除残留静电，关闭其它开关，取下铝箔纸，将其置于通风橱中自然风干；
（3）压电促愈型创面修复辅助材料的制备：将制备得到的聚偏氟乙烯——聚（偏氟乙烯-三氟乙烯）静电纺丝膜裁剪成15× 6 cm的矩形片，通过导电粘合剂粘附到市售的脱细胞猪真皮基质敷料上。
Claims (6)
1.一种压电促愈型创面修复辅助材料的制备方法，其特征是：
（1）静电纺丝液的配制：量取30~45体积份的丙酮与55~70体积份的N,N-二甲基甲酰胺混合成100体积份的溶剂，将质量浓度为8%~25%的聚偏氟乙烯聚合物溶于上述混合溶剂中，随后以聚合物干重记，加入其质量分数为0%~15%的季铵盐，0%~0.5%的纳米粒子，搅拌均匀，备用；
（2）静电纺丝微纳纤维膜压电层的制备：纺丝液使用前经超声除泡0~60 min；将除泡后的溶液装入静电纺丝用注射器中，接上导电针头，并将注射器装入推注器中，设置推注速度为0.5~1 ml/h，将高压电源连接至导电针头上；在接受滚筒上包裹一层铝箔纸，将负压电源连接至接收滚筒，打开滚筒开关，设置转速为100~1000 rpm；随后，打开负压，调节负压为-1~2 kV；打开高压电源，调节电压至15~30 kV，设置纺丝时间为2~12h；纺丝结束后，关闭高压、负压电源，使用接地安全棒去除残留静电，关闭其它开关，取下铝箔纸，将其置于真空干燥箱中干燥或通风橱中自然风干；
（3）促愈型创面治疗附件材料的制备：将制备得到的静电纺丝微纳纤维膜压电层粘附到导电粘附材料上，获得压电促愈型创面修复辅助材料。
2.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的聚偏氟乙烯聚合物是指聚偏氟乙烯、聚（偏氟乙烯-三氟乙烯）、聚（偏氟乙烯-四氟乙烯）。
3.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的季铵盐只是四丁基氯化铵、甲基三乙基氯化铵、双十二烷基二甲基氯化铵、双十八烷基二甲基氯化铵等季铵盐。
4.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的纳米粒子是指石墨烯、氧化石墨烯、碳纳米管、纳米四氧化三铁、纳米钛酸钡、纳米二氧化钛、纳米二氧化硅等碳纳米材料、金属纳米材料及金属氧化物纳米材料。
5.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其中所述的导电粘合材料是指细胞毒性合格的导电粘合水凝胶、导电粘合剂和导电粘合膜等具有导电和自粘功能的材料。
6.根据权利要求1所述的一种压电促愈型创面修复辅助材料的制备方法，其特征在于该方法制备的压电促愈型创面修复辅助材料可联合各类型伤口敷料用于创伤修复。
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| CN118059241A (zh) * | 2024-04-24 | 2024-05-24 | 吉林大学 | 一种用于伤口愈合的压电复合膜及其制备方法和应用 |
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