CN108096626A - 促愈合止血无纺布的制备方法 - Google Patents
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Abstract
本发明涉及无纺布技术领域，尤其是一种促愈合止血无纺布的制备方法；所述制备方法包括以下步骤：(1)将质量分数为2wt％的壳聚糖乙醇溶液和30％的聚丙烯酸去离子水溶液按比例混合，得到壳聚糖、聚丙烯酸混合溶液，然后向该混合溶液中加入三七粉、紫珠草提取物和小蓟提取物的混合物，超声波震荡形成静电纺丝悬浮液；(2)将静电纺丝溶液以的2‑4ml/h流速通过静电纺丝装置注射泵的22号钝性针头，静电纺丝纤维收集旋转圆轴上，转速为550‑650r/min，从圆轴上取下膜片，真空干燥48h后，即得；本发明医用无纺布的制备方法，工艺简单，制备而成的医用无纺布可止血抗菌防粘结。
Description
技术领域
本发明涉及无纺布技术领域，尤其是一种促愈合止血无纺布的制备方法。
背景技术
壳聚糖是甲壳质的脱乙酰产物，是一种多糖物质，其化学名为β(1-4)-2-氨基-2-脱氧-D-葡聚糖。据文献报道，壳聚糖对神经损伤修复及骨关节损伤修复有一定促进作用，并可能有止血作用。壳聚糖具有天然抑菌、止血、消炎、促进伤口愈合、减小伤口疤痕以及生物相溶性好的特点，目前已有技术将壳聚糖湿法纺丝成纤维，再织成壳聚糖纤维无纺布，用于伤口愈合材料。但是，采用这种方法制成的壳聚糖纤维无纺布敷在伤口上时，只能少量的吸收伤口流出液，并不能保证伤口周围湿润，伤口愈合后易与皮肤粘连，使用不方便。因此需要研发一种即可以吸收伤口流出液，并且溶解具有一定黏稠度，能粘在伤口上的壳聚糖纤维无纺布。
发明内容
本发明要解决的技术问题是：克服现有技术中的不足，提供一种促愈合止血无纺布的制备方法，采用该方法制得的无纺布具有使用方便、使用后不会发生黏连的有益效果。
为解决上述技术问题，本发明采用的技术方案如下：
一种促愈合止血无纺布的制备方法，所述制备方法包括以下步骤：
(1)将质量分数为2wt％的壳聚糖乙醇溶液和30％的聚丙烯酸去离子水溶液按比例混合，得到壳聚糖、聚丙烯酸混合溶液，然后向该混合溶液中加入三七粉、紫珠草提取物和小蓟提取物的混合物，超声波震荡形成静电纺丝悬浮液；
(2)将静电纺丝溶液以的2-4ml/h流速通过静电纺丝装置注射泵的22号钝性针头，静电纺丝纤维收集旋转圆轴上，转速为550-650r/min，从圆轴上取下膜片，真空干燥48h后，即得。
优选的，所述壳聚糖、聚丙烯酸混合溶液中壳聚糖与聚丙烯酸的质量比3:7。
优选的，所述三七粉、紫珠草和小蓟的质量比为10:1.5-2:1。
优选的，所述三七粉、紫珠草和小蓟的质量比为10:1.8:1。
优选的，所述壳聚糖为改性壳聚糖，所述改性壳聚糖采用以下方法制得：壳聚糖采用稀盐酸酸化，将乳糖酸溶液与活化的N,N′-二环丙基碳二亚胺的混合溶液滴加到酸化的壳聚糖中，反应100h，得到混合物，将混合物进行过滤，得滤液，再将滤液经过截留分子质量为10000～15000的透析袋透析5天，得到袋内截留溶液，然后将袋内截留溶液置于温度为40℃下真空干燥，得到改性的壳聚糖。
优选的，所述酸化的壳聚糖与乳糖酸溶液的体积比为1:6，所述的酸化的壳聚糖与活化的N,N′-二环丙基碳二亚胺的体积比为1:5。
优选的，所述稀盐酸的质量分数为5％。
优选的，所述小蓟提取物采用以下方法制得：将小蓟洗净干燥粉碎后于乙二醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:1.5-5。
优选的，所述紫珠草提取物采用以下方法制得：将紫珠草洗净干燥粉碎后于乙醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:2-5。
采用本发明的技术方案的有益效果是：
1、本发明医用无纺布的制备方法，工艺简单，制备而成的医用无纺布可止血抗菌防粘结。
2、本发明中采用的三七粉、紫珠草提取物和小蓟提取物均为中草药，伤者使用本发明中的无纺布，不会有任何毒副作用，同时采用本发明技术方案制得的无纺布用作创伤材料或敷料，具有止血、活血化瘀、消肿定痛等功能，并且所用材料可以在体内降解，细胞亲和性好，可促进坏组织康复，而制备方法过程简单，工艺条件方便控制。
具体实施方式
下面结合具体实施方式对本发明作进一步说明。
实施例1
一种促愈合止血无纺布的制备方法，包括以下步骤：
(1)将质量分数为2wt％的壳聚糖乙醇溶液和30％的聚丙烯酸去离子水溶液按比例混合，得到壳聚糖、聚丙烯酸混合溶液，其中壳聚糖、聚丙烯酸混合溶液中壳聚糖与聚丙烯酸的质量比3:7；然后向该混合溶液中加入三七粉、紫珠草提取物和小蓟提取物的混合物，三七粉、紫珠草和小蓟的质量比为10:1.5:1，超声波震荡形成静电纺丝悬浮液；
其中，小蓟提取物采用以下方法制得：将小蓟洗净干燥粉碎后于乙二醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:1.5；
其中，紫珠草提取物采用以下方法制得：将紫珠草洗净干燥粉碎后于乙醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:2；
本实施例中壳聚糖为改性壳聚糖，改性壳聚糖采用以下方法制得：壳聚糖采用质量分数为5％的稀盐酸酸化，将乳糖酸溶液与活化的N,N′-二环丙基碳二亚胺的混合溶液滴加到酸化的壳聚糖中，反应100h，得到混合物，将混合物进行过滤，得滤液，再将滤液经过截留分子质量为10000～15000的透析袋透析5天，得到袋内截留溶液，然后将袋内截留溶液置于温度为40℃下真空干燥，得到改性的壳聚糖；酸化的壳聚糖与乳糖酸溶液的体积比为1:6，所述的酸化的壳聚糖与活化的N,N′-二环丙基碳二亚胺的体积比为1:5；
(2)将静电纺丝溶液以的2-4ml/h流速通过静电纺丝装置注射泵的22号钝性针头，静电纺丝纤维收集旋转圆轴上，转速为550r/min，从圆轴上取下膜片，真空干燥48h后，即得。
实施例2
一种促愈合止血无纺布的制备方法，包括以下步骤：
(1)将质量分数为2wt％的壳聚糖乙醇溶液和30％的聚丙烯酸去离子水溶液按比例混合，得到壳聚糖、聚丙烯酸混合溶液，其中壳聚糖、聚丙烯酸混合溶液中壳聚糖与聚丙烯酸的质量比3:7；然后向该混合溶液中加入三七粉、紫珠草提取物和小蓟提取物的混合物，三七粉、紫珠草和小蓟的质量比为10:1.8:1；超声波震荡形成静电纺丝悬浮液；
其中，小蓟提取物采用以下方法制得：将小蓟洗净干燥粉碎后于乙二醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:3；
其中，紫珠草提取物采用以下方法制得：将紫珠草洗净干燥粉碎后于乙醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:3；
本实施例中壳聚糖为改性壳聚糖，改性壳聚糖采用以下方法制得：壳聚糖采用质量分数为5％的稀盐酸酸化，将乳糖酸溶液与活化的N,N′-二环丙基碳二亚胺的混合溶液滴加到酸化的壳聚糖中，反应100h，得到混合物，将混合物进行过滤，得滤液，再将滤液经过截留分子质量为10000～15000的透析袋透析5天，得到袋内截留溶液，然后将袋内截留溶液置于温度为40℃下真空干燥，得到改性的壳聚糖；酸化的壳聚糖与乳糖酸溶液的体积比为1:6，所述的酸化的壳聚糖与活化的N,N′-二环丙基碳二亚胺的体积比为1:5；
(2)将静电纺丝溶液以的2-4ml/h流速通过静电纺丝装置注射泵的22号钝性针头，静电纺丝纤维收集旋转圆轴上，转速为600r/min，从圆轴上取下膜片，真空干燥48h后，即得。
实施例3
一种促愈合止血无纺布的制备方法，包括以下步骤：
(1)将质量分数为2wt％的壳聚糖乙醇溶液和30％的聚丙烯酸去离子水溶液按比例混合，得到壳聚糖、聚丙烯酸混合溶液，其中壳聚糖、聚丙烯酸混合溶液中壳聚糖与聚丙烯酸的质量比3:7；然后向该混合溶液中加入三七粉、紫珠草提取物和小蓟提取物的混合物，三七粉、紫珠草和小蓟的质量比为10:2:1，超声波震荡形成静电纺丝悬浮液；
其中，小蓟提取物采用以下方法制得：将小蓟洗净干燥粉碎后于乙二醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:5；
其中，紫珠草提取物采用以下方法制得：将紫珠草洗净干燥粉碎后于乙醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:5；
本实施例中壳聚糖为改性壳聚糖，改性壳聚糖采用以下方法制得：壳聚糖采用质量分数为5％的稀盐酸酸化，将乳糖酸溶液与活化的N,N′-二环丙基碳二亚胺的混合溶液滴加到酸化的壳聚糖中，反应100h，得到混合物，将混合物进行过滤，得滤液，再将滤液经过截留分子质量为10000～15000的透析袋透析5天，得到袋内截留溶液，然后将袋内截留溶液置于温度为40℃下真空干燥，得到改性的壳聚糖；酸化的壳聚糖与乳糖酸溶液的体积比为1:6，所述的酸化的壳聚糖与活化的N,N′-二环丙基碳二亚胺的体积比为1:5；
(2)将静电纺丝溶液以的2-4ml/h流速通过静电纺丝装置注射泵的22号钝性针头，静电纺丝纤维收集旋转圆轴上，转速为650r/min，从圆轴上取下膜片，真空干燥48h后，即得。
实验验证：
吸水性：本文所公开的促愈合止血无纺布，它的功能是其中的药物成分能够粘附到开放性伤口形成物理屏障来止血并立即吸收血液中的水份，具有良好的水溶性和生物相容性。
用吸水性能实验来测试本发明的无纺布对伤口液体模拟溶液(溶液A)的吸收能力，表示为每克无纺布吸收水的质量(克水/克无纺布)。溶液A含有142微摩尔每升的氯化钠和2.5微摩尔氯化钙。用这种溶液来模仿血清和外伤液体。
该测试装置包括250ml烧杯中的200ml溶液A，溶液放在搅拌电热板上，加热到37±1℃并保持这个温度。称取一定量的无纺布放入溶液A中。浸泡到预定的时间，取出无纺布，称量无纺布，浸泡前后的质量差就是颗粒所吸收的溶液的质量。实验结果是，无纺布具有较强的吸收能力。
止血能力：在正常的血压下，止血剂应阻止液体的流动。通常使用的是70毫米汞柱的压力或952毫米水柱的压力。这样一种阻止液体流动的测试以本发明一个实施例中2的样品为对象。在该测试中，将含有模拟体液溶液A的保持垂直的1000mm或1米中空柱子，柱子底部设置有活塞，该柱子用于模仿人体的血管出血时的压力，将柱子的溶液A的出口埋入实施例1中止血剂中，打开柱子底部的活塞，溶液A从无纺布上流过，如果柱子底部被止血剂封住，溶液A不再向下流动，则证明本实施例2制备的止血剂止血效果好。试验结果是，溶液A不再向下流动。
综上所述：
1、本发明医用无纺布的制备方法，工艺简单，制备而成的医用无纺布可止血抗菌防粘结。
2、本发明中采用的三七粉、紫珠草提取物和小蓟提取物均为中草药，伤者使用本发明中的无纺布，不会有任何毒副作用，同时采用本发明技术方案制得的无纺布用作创伤材料或敷料，具有止血、活血化瘀、消肿定痛等功能，并且所用材料可以在体内降解，细胞亲和性好，可促进坏组织康复，而制备方法过程简单，工艺条件方便控制。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (9)
1.一种促愈合止血无纺布的制备方法，其特征在于，所述制备方法包括以下步骤：
(1)将质量分数为2wt％的壳聚糖乙醇溶液和30％的聚丙烯酸去离子水溶液按比例混合，得到壳聚糖、聚丙烯酸混合溶液，然后向该混合溶液中加入三七粉、紫珠草提取物和小蓟提取物的混合物，超声波震荡形成静电纺丝悬浮液；
(2)将静电纺丝溶液以的2-4ml/h流速通过静电纺丝装置注射泵的22号钝性针头，静电纺丝纤维收集旋转圆轴上，转速为550-650r/min，从圆轴上取下膜片，真空干燥48h后，即得。
2.根据权利要求1所述的促愈合止血无纺布的制备方法，其特征在于：所述壳聚糖、聚丙烯酸混合溶液中壳聚糖与聚丙烯酸的质量比3:7。
3.根据权利要求1所述的促愈合止血无纺布的制备方法，其特征在于：所述三七粉、紫珠草和小蓟的质量比为10:1.5-2:1。
4.根据权利要求3所述的促愈合止血无纺布的制备方法，其特征在于：所述三七粉、紫珠草和小蓟的质量比为10:1.8:1。
5.根据权利要求1所述的促愈合止血无纺布的制备方法，其特征在于：所述壳聚糖为改性壳聚糖，所述改性壳聚糖采用以下方法制得：壳聚糖采用稀盐酸酸化，将乳糖酸溶液与活化的N,N′-二环丙基碳二亚胺的混合溶液滴加到酸化的壳聚糖中，反应100h，得到混合物，将混合物进行过滤，得滤液，再将滤液经过截留分子质量为10000～15000的透析袋透析5天，得到袋内截留溶液，然后将袋内截留溶液置于温度为40℃下真空干燥，得到改性的壳聚糖。
6.根据权利要求5所述的促愈合止血无纺布的制备方法，其特征在于：所述酸化的壳聚糖与乳糖酸溶液的体积比为1:6，所述的酸化的壳聚糖与活化的N,N′-二环丙基碳二亚胺的体积比为1:5。
7.根据权利要求5所述的促愈合止血无纺布的制备方法，其特征在于：所述稀盐酸的质量分数为5％。
8.根据权利要求1所述的促愈合止血无纺布的制备方法，其特征在于：所述小蓟提取物采用以下方法制得：将小蓟洗净干燥粉碎后于乙二醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:1.5-5。
9.根据权利要求1所述的促愈合止血无纺布的制备方法，其特征在于：所述紫珠草提取物采用以下方法制得：将紫珠草洗净干燥粉碎后于乙醇和乙酸乙酯的混合溶剂回流24h后浓缩得到小蓟提取物，其中乙二醇与乙酸乙酯的体积比为1:2-5。
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