CN111621974A - 可生物降解的冷湿敷绷带的制备方法及其用途 - Google Patents
可生物降解的冷湿敷绷带的制备方法及其用途 Download PDFInfo
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Abstract
本发明公开了一种可生物降解的冷湿敷绷带的制备方法及其用途，该制备方法包括冷湿敷剂的制备及冷湿敷绷带的制备。本发明还公开了一种冷湿敷绷带所用棉纱布的制备方法，包括配置10‑12％质量浓度的NaOH溶液，向NaOH溶液中加入四甲基哌啶酮，20‑25℃下将布样置于NaOH溶液中浸渍15‑20min，加入苯氨基丙酸，将反应容器置于70‑72℃水浴反应3‑4h，反应结束后，调节温度为50‑60℃，加入环氧氯丙烷交联反应60‑90min，交联反应结束后，洗涤、烘干，即得样品。采用本发明提供的制备方法制得的冷湿敷绷带具有冷湿敷剂含量高、作用时间长、柔性好、透气性好、力学强度高的优点。
Description
技术领域
本发明属于医药技术领域，具体涉及可生物降解的冷湿敷绷带的制备方法及其用途。
背景技术
棉纱布是一种有很长应用历史的传统性用敷料，因为它对创而的愈合无明显作用，故又称惰性敷料。作为治疗过程中经常使用的种用纺织品，它能包裹和保护伤口，促进其愈合。棉纱布质地柔软，价格低廉，来源广泛，生产加工过程比较简单，可重复使用。由于棉纤维具有吸湿、柔软且不过敏等性质，传统的医用纱布多以中、粗特纯棉纱平纹织成，织物结构疏松，经练漂、脱脂及严格高温高压消毒，具有吸湿和散湿性能优良、耐热性和耐碱性较好等特点，至今仍在各种类型的创伤治疗中广泛应用。棉纱布的吸湿性是由于其织物结构中所形成的毛细空间。根据湿性愈合理论，在湿润的环境下，细胞分裂速度更快，有利于酶活性的发挥，更有利于伤口愈合。
医用敷料主要是一些软填料、纱布、绷带及类似产品。纤维素纤维为原料的医用敷料在医疗卫生行业的应用已经有很长的历史。以纤维素材料为基础材料制作高吸水材料应用于医用敷料、日用品、农业、工业和林业园艺用保水材料，具有安全可靠、可降解、环保无污染的优点。纱布的原料一般采用棉纱，即棉纱布。尽管目前新技术和新材料在不断涌现，传统的棉纱布仍然是伤口护理中使用的主要的材料。以棉纱为原料制备的纱布是医院中用量最多的外科材料，是纺织材料在医用领域应用最多的产品之一，是医疗过程中经常使用的一种医用敷料。由于棉纱布质地柔软，价格低廉，来源广泛，所以在医用敷料中大量应用。
现有技术如授权公告号为CN 103536961 B的中国发明专利，公开了一种医用冷湿敷绷带及其生产方法。该医用冷湿敷绷带由冷湿敷剂与载带所述冷湿敷剂的织物组成的，所述的冷湿敷剂由冰片、樟脑、薄荷脑及其衍生物、N,2,3-三甲基-2-异丙基丁酰胺、植物精油、甘油、乙醇、增稠剂、增溶剂与防腐剂组成。该发明的医用冷湿敷绷带常温保存，携带方便、使用方便、安全，一次性冷敷时间长达2hr以上；该发明的冷湿敷绷带具有加压包扎固定的功能；对无创急性损伤、闭合骨折手术前48hr的冷湿敷，具有消肿、止痛、止血的良好效果，止痛效果优于冰袋。
发明内容
本发明的目的在于提供一种冷湿敷剂含量高、作用时间长、柔性好、透气性好、力学强度高的可生物降解的冷湿敷绷带的制备方法及其用途。
本发明为实现上述目的所采取的技术方案为：
提供一种医用棉纱布的制备方法，包括以下步骤：
S1、配置10-12％质量浓度的NaOH溶液；
S2、向NaOH溶液中加入四甲基哌啶酮，20-25℃下将布样置于NaOH溶液中浸渍15-20min；
S3、加入苯氨基丙酸，将反应容器置于70-72℃水浴反应3-4h；
S4、反应结束后，调节温度为50-60℃，加入环氧氯丙烷交联反应60-90min；
S5、交联反应结束后，将布样取出，浸入无水乙醇与水(体积比为4:1)的混合溶液中，并用乙酸调节溶液的pH至中性；
S6、取出将中和完毕的布样，挤压出材料中多余的液体，用无水乙醇与水(体积比为4:1)的混合溶液重复洗涤2-3次；
S7、将清洗完的布样置于65-70℃烘干，即得样品。利用苯氨基丙酸对医用棉纺织布改性，在特定比例范围内，四甲基哌啶酮可以与NaOH协同促进纤维素上反应的活性中心的形成，促进苯氨基丙酸与棉纱布上的羟基发生酰化反应，提高取代度，引入亲水基团氨基、羧基，增强吸水性和保水性，从而能够促进对冷湿敷剂的吸收和作用时间，同时由于引入的苯环结构的空间位阻作用，抑制纤维之间的摩擦和缠结，能够保持绷带较好的柔性，增加透气性。
优选地，上述苯氨基丙酸与NaOH的摩尔比为5:4-6。
优选地，上述四甲基哌啶酮与NaOH的摩尔比为1:8-10。
优选地，上述苯氨基丙酸与布样的质量比为3-5:4。
优选地，上述步骤S4中用环氧氯丙烷进行交联时加入硫辛酰胺。优选地，上述硫锌酰胺与环氧氯丙烷的质量比为1:3.2-4.1。用环氧氯丙烷进行交联时应过程中，存在许多副反应，比如，环氧氯丙烷可能只和纤维素的一个羟基反应，或者环氧氯丙烷完全水解等。硫辛酰胺能够促进环氧氯丙烷与棉纱布纤维素的交联，提高交联度，同时促进纤维素表面裂纹和孔洞的形成，增强毛细效应，促进液体储存在这些孔洞和沟槽内，增加纤维吸湿性和保湿性，从而促进对冷湿敷剂的吸附并增加作用时间，且具有良好的透气性、力学强度。
提供一种医用棉纱布，采用上述一种医用棉纱布的制备方法进行制备。
提供一种可生物降解的冷湿敷绷带的制备方法，包括以下步骤：
冷湿敷剂的制备：将0.1-5重量份冰片、0.1-5重量份樟脑、0.1-5重量份薄荷脑、0.1-5重量份N,2,3-三甲基-2-异丙基丁酰胺、0.1-5重量份植物精油、0.5-15重量份甘油、10-30重量份乙醇、0.05-0.1重量份增稠剂、0.1-1重量份增溶剂、0.01-0.1重量份防腐剂混合均匀，补加水至总量为100重量份，得到冷湿敷剂；
冷湿敷绷带的制备：将按照上述一种医用棉纱布的制备方法制得的棉纱布置于含有上述冷湿敷剂的不锈钢容器中浸泡5-30min后，装入铝箔包装袋中，封口，得到上述冷湿敷绷带。
提供上述一种可生物降解的冷湿敷绷带的制备方法在制备具有消肿止痛功能的医用绷带中的用途。
本发明由于采用了四甲基哌啶酮与NaOH协同促进苯氨基丙酸对医用棉纱布改性，并采用了硫辛酰胺促进环氧氯丙烷与棉纱布纤维素的交联，因而具有如下有益效果：
1)能够促进苯氨基丙酸与棉纱布上的羟基发生酰化反应，提高取代度，引入亲水基团氨基、羧基，增强吸水性和保水性，从而能够促进对冷湿敷剂的吸收和作用时间，同时由于引入的苯环结构的空间位阻作用，抑制纤维之间的摩擦和缠结，能够保持绷带较好的柔性，增加透气性。；
2)能够促进环氧氯丙烷与棉纱布纤维素的交联，提高交联度，同时促进纤维素表面裂纹和孔洞的形成，增强毛细效应，促进液体储存在这些孔洞和沟槽内，增加纤维吸湿性和保湿性，从而促进对冷湿敷剂的吸附并增加作用时间，且具有良好的透气性、力学强度。
因此，本发明是一种冷湿敷剂含量高、作用时间长、柔性好、透气性好、力学强度高的可生物降解的冷湿敷绷带的制备方法及其用途。
附图说明
图1为本发明试验例1中红外光谱图；
图2为本发明试验例1中取代度的测定结果；
图3为本发明试验例2中溶胀系数的测定结果；
图4为本发明试验例2中扫描电镜图；
图5为本发明试验例3中吸液率和保湿率的测定结果；
图6为本发明试验例3中透气性的测定结果；
图7为本发明试验例3中抗弯刚度的测定结果；
图8为本发明试验例3中断裂强度和断裂伸长率的测定结果；
图9为本发明试验例4中冷湿敷剂的含量及剩余量的测定结果。
具体实施方式
以下结合具体实施方式和附图对本发明的技术方案作进一步详细描述：
实施例1：
一种医用棉纱布的制备方法，包括以下步骤：
S1、配置10％质量浓度的NaOH溶液。
S2、向10g 10％(m/m)NaOH溶液中加入0.466g四甲基哌啶酮，20℃下将4g布样置于NaOH溶液中浸渍15min。
S3、加入4.96g苯氨基丙酸，将反应容器置于70℃水浴反应3h。
S4、反应结束后，调节温度为60℃，加入0.2g环氧氯丙烷溶液交联反应70min；
S5、交联反应结束后，将布样取出。
一种可生物降解的冷湿敷绷带的制备方法，包括以下步骤：
冷湿敷剂的制备：将2g冰片、2g樟脑、3g薄荷脑、2g N,2,3-三甲基-2-异丙基丁酰胺、4g植物精油、8g甘油、20g乙醇、0.05g增稠剂、0.4g增溶剂、0.02g防腐剂混合均匀，补加水至总量为100g，得到冷湿敷剂；
冷湿敷绷带的制备：将上述制备的5g医用棉纱布置于含有上述冷湿敷剂的不锈钢容器中浸泡10min后，得到冷湿敷绷带。
实施例2：
步骤S2中未添加四甲基哌啶酮，其余部分和实施例1完全一致。
实施例3：
步骤S3中未添加苯氨基丙酸，其余部分和实施例1完全一致。
实施例4：
步骤S2中未添加四甲基哌啶酮，步骤S3中未添加苯氨基丙酸，其余部分和实施例1完全一致。
实施例5：
步骤S2中四甲基哌啶酮添加量为0.368g，其余部分和实施例1完全一致。
实施例6：
步骤S2中四甲基哌啶酮添加量为0.475g，其余部分和实施例1完全一致。
实施例7：
步骤S4中用环氧氯丙烷进行交联时加入0.07g硫辛酰胺，其余部分和实施例1完全一致。
实施例8：
步骤S4中用环氧氯丙烷进行交联时加入0.07g硫辛酰胺，其余部分和实施例4完全一致。
试验例1：
分别取实施例1-8部分步骤S3改性后的医用棉纱布浸入无水乙醇与水(体积比为4:1)的混合溶液中，并用乙酸调节溶液的pH至中性；取出将中和完毕的布样，挤压出材料中多余的液体，用无水乙醇与水(体积比为4:1)的混合溶液重复洗涤3次；将清洗完的布样置于70℃烘干，得样品。
红外光谱分析：将实施例1、实施例4制得的上述样品直接在傅立叶红外光谱仪上扫描测试完成，分析改性医用棉纱布发生改性反应的特征。红外光谱图见图1。
取代度的测定：剪取质量约为0.50g的上述样品，置于250mL锥形瓶中，加入2mol/LH2SO4溶液100mL，浸泡3h以上，使其充分酸化。用蒸馏水反复的冲洗布样，确保样品完全清洗干净。后用0.l0mol/L NaOH标准溶液50mL浸泡3h以上，并对溶液微热，使反应充分，滴入2滴酚酞试剂，再立即用0.05mol/L标准H2SO4溶液反滴至酚酞指示剂的红色刚退去。取代度计算如下：
A＝(BC-DE)/F；
DS＝162A/(1000-164A)；
式中，A是1mg改性棉纱布消耗的酸的物质的量；B为加入NaOH溶液的体积，mL；C指NaOH的摩尔浓度，mol/L；D是滴定过量的NaOH所需H2SO4的体积，mL；E是H2SO4的摩尔浓度，mol/L；F为改性棉纱布的质量，g；162是纤维素中的失水葡萄糖单元的摩尔质量；164代表每引入一个羧基则失水葡萄糖单元净增的分子质量。取代度的测定结果见图2。
由图1可以看出，与实施例4相比，实施例1的红外光谱图中增加了1586cm-1处-COOH的伸缩振动特征吸收峰，1687cm-1处酰胺键的C＝O的伸缩振动特征吸收峰，1610cm-1、1517cm-1、1464cm-1处苯环的骨架C＝C的伸缩振动特征吸收峰，1377cm-1、911cm-1处-OH的弯曲振动特征吸收峰，说明苯氨基丙酸成功与棉纱布上的羟基发生酰化反应，引入了亲水基团氨基、羧基及苯环结构。
由图2可以看出，实施例1中苯氨基丙酸的取代度明显大于实施例2、实施例3、实施例4、实施例5、实施例6，实施例7的取代度明显大于实施例8，这说明，当四甲基哌啶酮与NaOH的摩尔比在1:8-10的范围内，四甲基哌啶酮可以与NaOH协同促进纤维素上反应的活性中心的形成，促进苯氨基丙酸与棉纱布上的羟基发生酰化反应，提高取代度。
试验例2
交联程度的测定：通过纤维溶胀系数测定棉纱布的交联程度。称量绝对干重样品m0后放入安倍瓶内，然后将安培瓶放入装有20℃的蒸馏水的烧杯中，使纤维充分润湿溶胀，加入1g/L的润湿渗透剂，延长润湿时间至16h，确保纤维充分润湿溶胀。离心排水后立即称重m1，烘干后称重m2，溶胀系数n的计算如下式：
n＝(m1-m2)/m0。
溶胀系数的测定结果见图3。
扫描电镜分析：分别取实施例4、实施例8制得干净的的新型医用棉纱布中间的纱线制作试样，经过真空镀金处理，在TM3000台式扫描电子显微镜观测试样的表面形貌。扫描电镜图见图4。
由图3可以看出，实施例7、实施例8制得的医用棉纱布的溶胀系数明显高于实施例1、实施例2、实施例3、实施例4、实施例5、实施例6，由图4可以看出，实施例8中纤维素表面裂纹和孔洞明显多于实施例4，这说明，硫辛酰胺能够促进环氧氯丙烷与棉纱布纤维素的交联，提高交联度，同时促进纤维素表面裂纹和孔洞的形成。
试验例3：
吸水性能测试：参照国际上常用的测试创面用敷料吸湿性的方法，采用吸湿称重法测试医用棉纱布的吸液性能，具体操作为：裁制5cm×5cm棉纱布，准确称出其干重W0，放入100mL去离子水中，吸液30min，取出棉纱布，自然平展地垂直悬挂30s后，立刻称量棉纱布重量W1，棉纱布的吸液率Q计算如下式：
Q＝(W1-W0)/W0
式中：Q—棉纱布的吸液率，％；W0—棉纱布吸液前的质量，g；W1—棉纱布吸液后的质量，g。
保湿性能测试：分别取干燥的一定质量的医用棉纱布，加入质量分数10％的水，置于硅胶干燥器中，放在20℃恒温培养箱中，每隔一段时间称量各个样品质量，记录。保湿率(％)计算公式如下：
保湿率＝(Mn-M0)/M0
式中：Mn-放置后样品质量(g)；
M0-放置前样品质量(g)。
吸液率和保湿率的测定结果见图5。
透气性能测试：在锥形瓶中加入200mL左右的蒸馏水，并将样品剪切成瓶口大小Dm，然后用双面胶把样品粘在瓶口，使锥形瓶内的蒸馏水只能通过样品扩散出去。透气性的测定结果见图6。
刚柔性能测试：
纱布作为医用敷料，柔软性是评价纱布质量的一项重要指标，纱布的柔软性能较差时，与患者伤口接触，会有较强的异物感，甚至会对伤口形成二次伤害。纱布的柔软性通常用抗弯刚度表示，抗弯刚度越小越柔软；反之，抗弯刚度越大，纱布的硬挺度越大，柔软性越差。参照标准GB/T18318.1-2009，将试样分经纬向裁制成2.5cm×25cm的纱布条，放在硬度仪测试平台上，将滑尺压在所测试样上，保证试样头端、测试平台边缘、滑尺端三端平齐。启动测试，测试仪器自动显示伸出长度L，记录数据并求出平均弯曲长度C，纱布的刚度G计算如式：
G＝m×C3×10-3
式中：G—单位宽度的抗弯刚度，mN·cm；
m—试样的单位面积质量，g/m2；
C—试样的平均弯曲长度，cm。
抗弯刚度的测定结果见图7。
力学性能测试：采用电子织物强力机对医用棉纱布进行经向拉伸断裂性能测试，隔距长度为120mm，拉伸速度为50mm/min。断裂强度和断裂伸长率的测定结果见图8。
由图5、图6、图7可以看出，实施例1制备的医用棉纱布的吸液率、保湿率、透气性明显高于实施例2、实施例3、实施例4、实施例5、实施例6，实施例7的明显高于实施例8，且实施例1、实施例2、实施例3、实施例4、实施例5、实施例6，实施例7、实施例8的抗弯刚度无明显差别，这说明，当四甲基哌啶酮与NaOH的摩尔比在1:8-10的范围内，四甲基哌啶酮可以与NaOH协同促进纤维素上反应的活性中心的形成，提高苯氨基丙酸取代度，增强吸水性和保水性，同时由于引入的苯环结构的空间位阻作用，抑制纤维之间的摩擦和缠结，能够保持绷带较好的柔性，增加透气性。
由图5、图6、图7、图8可以看出，实施例7制备的医用棉纱布的吸液率、保湿率、透气性、断裂强度、断裂伸长率明显高于实施例1，实施例8明显高于实施例4，这说明，硫辛酰胺能够促进环氧氯丙烷与棉纱布纤维素的交联，提高交联度，同时促进纤维素表面裂纹和孔洞的形成，增强毛细效应，促进液体储存在这些孔洞和沟槽内，增加纤维吸湿性和保湿性，且具有良好的透气性、力学强度。
试验例4：
冷湿敷剂含量及作用时间的测定：
将上述实施例中制备的冷湿敷绷带称重，记为w1，将称重后的样品置于自然环境下72h，再次称重，记为w2，将样品放入恒温干燥箱中烘干，烘干后称重，记为w0。以冷湿敷剂的剩余量表示作用时间。冷湿敷剂的含量N1(g/g)及剩余量N2(g/g)的计算公式如下：
N1＝(w1-w0)/w0
N2＝(w2-w0)/w0
冷湿敷剂的含量及剩余量的测定结果见图9。
由图9可以看出，实施例1制备的冷湿敷绷带中冷湿敷剂的含量及剩余量明显高于实施例2、实施例3、实施例4、实施例5、实施例6，实施例7的明显高于实施例8，这说明，当四甲基哌啶酮与NaOH的摩尔比在1:8-10的范围内，四甲基哌啶酮可以与NaOH协同促进纤维素上反应的活性中心的形成，提高苯氨基丙酸取代度，增强吸水性和保水性，从而能够促进对冷湿敷剂的吸收和作用时间。
由图9可以看出，实施例7制备的冷湿敷绷带中冷湿敷剂的含量及剩余量明显高于实施例1，实施例8明显高于实施例4，这说明，硫辛酰胺能够促进环氧氯丙烷与棉纱布纤维素的交联，提高交联度，同时促进纤维素表面裂纹和孔洞的形成，增强毛细效应，促进液体储存在这些孔洞和沟槽内，增加纤维吸湿性和保湿性，从而促进对冷湿敷剂的吸附并增加作用时间。
上述实施例中的常规技术为本领域技术人员所知晓的现有技术，故在此不再详细赘述。
以上实施方式仅用于说明本发明，而并非对本发明的限制，本领域的普通技术人员，在不脱离本发明的精神和范围的情况下，还可以做出各种变化和变型。因此，所有等同的技术方案也属于本发明的范畴，本发明的专利保护范围应由权利要求限定。
Claims (8)
1.一种医用棉纱布的制备方法，其特征在于，包括以下步骤：
S1、配置10-12％质量浓度的NaOH溶液；
S2、向NaOH溶液中加入四甲基哌啶酮，20-25℃下将布样置于NaOH溶液中浸渍15-20min；
S3、加入苯氨基丙酸，将反应容器置于70-72℃水浴反应3-4h；
S4、反应结束后，调节温度为50-60℃，加入环氧氯丙烷交联反应60-90min；
S5、交联反应结束后，将布样取出，浸入无水乙醇与水的混合溶液中，并用乙酸调节溶液的pH至中性；
S6、取出将中和完毕的布样，挤压出材料中多余的液体，用无水乙醇与水的混合溶液重复洗涤2-3次；
S7、将清洗完的布样置于65-70℃烘干，即得样品。
2.根据权利要求1所述的制备方法，其特征在于：所述苯氨基丙酸与NaOH的摩尔比为5:4-6。
3.根据权利要求1所述的制备方法，其特征在于：所述四甲基哌啶酮与NaOH的摩尔比为1:8-10。
4.根据权利要求1所述的制备方法，其特征在于：所述苯氨基丙酸与布样的质量比为3-5:4。
5.根据权利要求1所述的制备方法，其特征在于：所述步骤S4中用环氧氯丙烷进行交联时加入硫辛酰胺。
6.一种医用棉纱布，其特征在于：采用权利要求1-5任一项中所述的制备方法进行制备。
7.一种可生物降解的冷湿敷绷带的制备方法，其特征在于，包括以下步骤：
1)冷湿敷剂的制备：将0.1-5重量份冰片、0.1-5重量份樟脑、0.1-5重量份薄荷脑、0.1-5重量份N,2,3-三甲基-2-异丙基丁酰胺、0.1-5重量份植物精油、0.5-15重量份甘油、10-30重量份乙醇、0.05-0.1重量份增稠剂、0.1-1重量份增溶剂、0.01-0.1重量份防腐剂混合均匀，补加水至总量为100重量份，得到冷湿敷剂；
2)冷湿敷绷带的制备：将按照权利要求1-5任一项中所述的制备方法制得的棉纱布置于含有所述冷湿敷剂的不锈钢容器中浸泡5-30min后，优选地，浸泡10min，装入铝箔包装袋中，封口，得到所述冷湿敷绷带。
8.权利要求7所述的一种可生物降解的冷湿敷绷带的制备方法在制备具有消肿止痛功能的医用绷带中的用途。
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| CN1151895A (zh) * | 1996-08-02 | 1997-06-18 | 高景星 | 人体相容性抗菌消炎止血敷料及其制备方法 |
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| CN104721875A (zh) * | 2015-03-18 | 2015-06-24 | 华南理工大学 | 一种亲水型硅橡胶医用敷料及其制备方法 |
| CN106758214A (zh) * | 2017-01-11 | 2017-05-31 | 东华大学 | 具有表面分子刷结构的亲水拒油自清洁棉织物的制备方法 |
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- 2020-05-06 CN CN202010371359.5A patent/CN111621974A/zh not_active Withdrawn
- 2020-05-06 CN CN202110333006.0A patent/CN113047030A/zh not_active Withdrawn
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| CN1151895A (zh) * | 1996-08-02 | 1997-06-18 | 高景星 | 人体相容性抗菌消炎止血敷料及其制备方法 |
| US6211308B1 (en) * | 1998-08-20 | 2001-04-03 | Henkel Corporation | Method for coating a textile |
| CN1609336A (zh) * | 2003-10-21 | 2005-04-27 | 北京服装学院 | 抗病毒纤维及其制造方法和用途 |
| CN1970876A (zh) * | 2006-12-01 | 2007-05-30 | 陕西师范大学 | 一种制备具有亲水或疏水性纤维的方法 |
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| CN104721875A (zh) * | 2015-03-18 | 2015-06-24 | 华南理工大学 | 一种亲水型硅橡胶医用敷料及其制备方法 |
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