CN105734985B - 一种微胶囊复合衬垫材料的制备方法 - Google Patents
一种微胶囊复合衬垫材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种微胶囊复合衬垫材料的制备方法，包括（1）在室温条件下，先将芯材溶液、壁材和乳化剂加入到反应介质中搅拌乳化，再加入交联剂和过量盐酸并搅拌，减压抽滤得到微胶囊；（2）另取芯材溶液加入到海藻酸钠溶液中搅拌，然后加入步骤（1）得到的微胶囊、远红外纳米陶瓷粉、分散剂和粘合剂搅拌使之混合均匀，得到微胶囊复合整理剂；(3)将步骤(2)中制备的微胶囊复合整理剂通过涂覆、浸渍或浸轧复合在非织造布上，然后表面喷洒氯化钙溶液，烘干得到微胶囊复合衬垫材料。该方法简单易行，工艺条件温和；所得复合衬垫材料可重复利用性强，易于更换，有效物质释放持久，成本低廉，具有广阔的市场前景。
Description
技术领域
本发明属于功能性织物的制备领域，具体是一种微胶囊复合衬垫材料的制备方法。
背景技术
现代人快速的生活节奏，不太合理的饮食习惯以及运动的缺乏很容易导致身体局部的肥胖，严重影响形体的美观。为取得更好的减肥效果，很多人在加强锻炼的基础上在身体特定部位涂抹或敷贴减肥药物膏剂或药包等来强化瘦身效果。而且天然植物提取物的引入大大地提高了药物减肥的安全性，使得药物减肥更为安全可靠，为更多消费者所青睐。这种方式虽然可以使药物更有效地作用于特定部位，但由于涂抹，敷贴等施药形式本身的局限性，难免会出现使用不便，药效持续时间较短，贴剂等制剂还存在着影响肢体活动的问题，另外，当敷贴剂与皮肤在较长时间内紧密粘着时还容易引起过敏反应。这些不足的存在，影响了此类药物的适用范围和经济前景。
微胶囊技术是一种利用天然或合成高分子有机物将液体或粉体包裹起来制成直径在1～1000μm之间的微小颗粒的技术。微胶囊的囊芯物质可以通过囊壁上的细小孔隙缓慢地释放出来，不但具有良好的持续释放能力，还可以通过涂层整理技术与纺织品相结合，在不影响穿着使用的前提下实现药物、香精等物质的持续释放，达到治疗，保健等多种功能。
由于微胶囊是通过壁材高分子在芯材液滴表面交联沉积实现药物包覆的，目前作为微胶囊囊壁材料所使用的高分子材料多为水溶性材料，难以在同样是水溶性的药物表面交联沉积实现包覆。选用油溶性壁材，通过油相分离法虽然可以制备装载水溶性药物微胶囊，但制备出微胶囊的粒径较大，颗粒之间粘连较多，机械强度较低，而且制备过程中会不可避免地大量使用二氯甲烷、甲苯等毒性较强的有机溶剂，去除不彻底会对人体健康造成一定的危害。通过复乳液聚合法虽然可以制备粒径较小，具有一定机械强度的微胶囊，制备过程中不需要过多使用毒性较强的有机溶剂，但复乳液的制备需经过两次乳化操作，工艺较为复杂且仍然存在着被包覆在微胶囊内部的有机溶剂不易去除的问题，不太适合规模化生产。而油溶性药物的包覆工艺则相对简单，可用于包覆的水溶性高分子壁材物质种类也比较多，生产过程中以水为主要的反应介质，成本相对较低，较适合规模化生产。
申请号为201310331825.7的发明专利公开了一种纳米火麻油微胶囊及其微胶囊织物的制备方法和所制备的产品。该发明专利以聚乳酸为囊壁材料制作的火麻油微胶囊，可以用于织物的浸轧整理，可以实现药物的持久稳定释放，不影响肢体活动，还可以保持使用过程中的相对舒适。但可重复利用性较差，所载微胶囊中药物一旦释放完全，载药服装、织物就失去了本来的保健功能，只能通过整体更换的方式来保证用药的连续性，成本较高，不利于织物载体的最大限度利用。
发明内容
针对现有技术的不足，本发明拟解决的技术问题是，提供一种微胶囊复合衬垫材料的制备方法。该方法简单易行，工艺条件温和；所得复合衬垫材料可重复利用性强，易于更换，有效物质释放持久，成本低廉，具有广阔的市场前景。
本发明解决所述技术问题的技术方案是，提供微胶囊复合衬垫材料的制备方法，其特征在于由以下步骤组成：
(1)微胶囊的制备：在室温条件下，先将芯材溶液、壁材和乳化剂均匀混合，而后加入到反应介质中搅拌乳化5-25min，得到乳化分散体系；向乳化分散体系中加入交联剂和过量盐酸并搅拌，在40℃-60℃条件下反应60-90min，得到微胶囊分散液；减压抽滤微胶囊分散液，依次以石油醚、无水乙醇和蒸馏水洗涤除去未反应物质，得到微胶囊；
所述芯材溶液和壁材的质量比为20-30:1，乳化剂的质量为芯材溶液和壁材总质量的4％-20％，交联剂的质量为壁材质量的2.5-5倍；
所述芯材溶液为水溶性天然植物提取物；所述壁材为聚乙烯醇、聚乙二醇、海藻酸钠或壳聚糖中的至少一种；所述乳化剂为司盘-80、司盘-60、OP-10或吐温-80中的至少一种；所述反应介质为正庚烷、正己烷或石油醚中的至少一种；所述交联剂为甲醛或戊二醛的至少一种；
(2)微胶囊复合整理剂的制备：在室温条件下，另取芯材溶液加入到海藻酸钠溶液中搅拌2-5min，然后加入步骤(1)得到的微胶囊、远红外纳米陶瓷粉、分散剂和粘合剂，搅拌3-5min使之初步分散，再高速搅拌10-20min，使之混合均匀，得到微胶囊复合整理剂；
芯材溶液的质量为海藻酸钠溶液总质量的2％-20％，微胶囊的质量为海藻酸钠溶液质量的2％-20％，远红外纳米陶瓷粉的质量为海藻酸钠溶液质量的1％-10％，粘合剂的质量为海藻酸钠溶液质量的0.5％-5％，分散剂的质量为海藻酸钠溶液质量的1％-5％；
所述粘合剂为水性聚氨酯粘合剂或水性聚丙烯酸酯粘合剂中的至少一种；所述分散剂是十二烷基硫酸钠、OP-10或吐温-80中的至少一种；
(3)微胶囊复合衬垫材料的制备：将步骤(2)中制备的微胶囊复合整理剂通过涂覆、浸渍或浸轧工艺复合在非织造布上，然后对非织造布具有微胶囊复合整理剂的表面喷洒质量分数为10％-20％的氯化钙溶液，静置10-20分钟后，最后将非织造布在40℃-60℃下烘干10-30min，得到微胶囊复合衬垫材料。
与现有技术相比，本发明有益效果在于：
1.该复合衬垫材料具有轻薄、柔软的特点，可以根据需要任意裁剪，易于与各类塑形内衣，保健带等通过沿缝、粘贴等方式相结合，易于更换；其既可以作为单独的服装内衬，也可作为部分保健带，保健服中药包的替代品使用，拓展了此类药物的应用领域。
2.海藻酸钠和芯材溶液的组合保证使用初期药物的释放浓度，而后以微胶囊内所载药物作为海藻酸钠中药物的补充，可以大幅度延长药物的释放时间，保证药物的长效稳定释放。
3.海藻酸钠具有温和，亲肤的特性，可以减少过敏反应的发生。远红外纳米陶瓷粉能够促进人体血液循环，可以与药物中加入的吸收促进剂共同作用，强化药物的使用效果。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整的描述，显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明提供了一种微胶囊复合衬垫材料的制备方法，其特征在于由以下步骤组成：
(1)微胶囊的制备：在室温条件下，先将芯材溶液、壁材和乳化剂均匀混合，而后加入到反应介质中搅拌乳化5-25min，转速为500-1500rpm，得到乳化分散体系；向乳化分散体系中加入交联剂和过量盐酸并搅拌，转速为500-1500rpm，在40℃-60℃条件下反应60-90min，使交联剂与壁材发生交联反应，得到微胶囊分散液；减压抽滤微胶囊分散液，依次以石油醚、无水乙醇和蒸馏水洗涤除去未反应物质，得到微胶囊；
所述芯材溶液和壁材的质量比为20-30:1，乳化剂的质量为芯材溶液和壁材总质量的4％-20％，交联剂的质量为壁材质量的2.5-5倍；
所述芯材溶液为水溶性天然植物提取物，具体为山茶提取物、三叶草花提取物或可可花提取物中的至少一种；所述壁材为聚乙烯醇、聚乙二醇、海藻酸钠或壳聚糖中的至少一种；所述乳化剂为司盘-80、司盘-60、OP-10或吐温-80中的至少一种；所述反应介质为正庚烷、正己烷或石油醚中的至少一种；所述交联剂为甲醛或戊二醛的至少一种；盐酸的作用是使得体系呈强酸性；
(2)微胶囊复合整理剂的制备：在室温条件下，另取芯材溶液加入到海藻酸钠溶液中搅拌2-5min，然后加入步骤(1)得到的微胶囊、远红外纳米陶瓷粉、分散剂和粘合剂，搅拌3-5min使之初步分散，再高速搅拌10-20min，使之混合均匀，得到微胶囊复合整理剂；
芯材溶液的质量为海藻酸钠溶液总质量的2％-20％，微胶囊的质量为海藻酸钠溶液质量的2％-20％，远红外纳米陶瓷粉的质量为海藻酸钠溶液质量的1％-10％，粘合剂的质量为海藻酸钠溶液质量的0.5％-5％，分散剂的质量为海藻酸钠溶液质量的1％-5％；
所述粘合剂为水性聚氨酯粘合剂或水性聚丙烯酸酯粘合剂中的至少一种；所述分散剂是十二烷基硫酸钠、OP-10或吐温-80中的至少一种；
(3)微胶囊复合衬垫材料的制备：将步骤(2)中制备的微胶囊复合整理剂通过涂覆、浸渍或浸轧工艺复合在非织造布上，然后对非织造布具有微胶囊复合整理剂的表面喷洒质量分数为10％-20％的氯化钙溶液，静置10-20分钟后，最后将非织造布在40℃-60℃下烘干10-30min，得到微胶囊复合衬垫材料。
实施例1
(1)微胶囊制备：将芯材液体(由山茶提取物、三叶草花提取物、可可花提取物以质量比1:1:1的比例混合制成)与质量分数5％的聚乙烯醇溶液以质量比1:1的比例混合均匀制成混合液。取该混合液8g加入盛有60ml正庚烷的锥形瓶中，并加入0.16g乳化剂span-80，在60℃，搅拌速度1500rpm的条件下，乳化5min，制成乳化液。保持1500rpm搅拌速度，向前述乳化液中加入盐酸酸化的25％戊二醛溶液(pH＝2)3.5mL。保持1500rpm搅拌转速反应60min后可得微胶囊分散液。减压抽滤前述微胶囊分散液，将滤出物经石油醚、无水乙醇和蒸馏水充分洗涤后冷冻干燥即可得到微胶囊。
(2)取质量分数如下：步骤(1)的微胶囊20％、远红外纳米陶瓷粉3％、芯材液体(由山茶提取物，三叶草花提取物，可可花提取物以质量比1:1:1的比例混合制成)20％、水性聚丙烯酸酯粘合剂5％、2％分散剂吐温-80、余量为海藻酸钠溶液。在室温条件下，先将芯材液体加入海藻酸钠溶液中，搅拌5min，然后加入分散剂、水性聚丙烯酸酯粘合剂、微胶囊和远红外纳米陶瓷粉，高速剪切分散20min制成均一稳定的微胶囊复合整理剂。
(3)将涤纶非织造布在上述微胶囊复合整理剂中一浸一轧后取出，其中非织造布带液率为80％。在非织造布具有微胶囊复合整理剂的表面喷涂质量分数为10％氯化钙溶液，静置15min使海藻酸钠大分子充分交联，再经过60℃烘干10min，即可得到微胶囊复合衬垫材料。
实施例2
(1)微胶囊制备：将芯材液体(由山茶提取物、可可花提取物以质量比2:1的比例混合制成)与质量分数5％的聚乙烯醇溶液以质量比1:1的比例混合均匀制成混合液。取该混合液8g加入盛有60ml石油醚的锥形瓶中，并加入0.8g乳化剂span-80，在40℃，搅拌速度500rpm的条件下，乳化20min，制成乳化液。保持500rpm搅拌速度，向前述乳化液中加入盐酸酸化的25％戊二醛溶液(pH＝2)2.0mL。保持500rpm搅拌转速反应90min后可得微胶囊分散液。减压抽滤前述微胶囊分散液，将滤出物经石油醚，无水乙醇，蒸馏水充分洗涤后冷冻干燥即可得到微胶囊。
(2)取质量分数如下：按步骤(1)的微胶囊2％、水性聚丙烯酸酯粘合剂2％、OP-10分散剂3％、芯材液体(由山茶提取物、可可花提取物以质量比2:1的比例混合制成)20％、远红外纳米陶瓷粉2％、8％吐温-80、余量为海藻酸钠溶液。在室温条件下，先将芯材液体加入海藻酸钠溶液中，搅拌5min，然后加入分散剂、水性聚丙烯酸酯粘合剂、微胶囊和远红外纳米陶瓷粉，搅拌3min使之初步分散后，高速剪切分散20min制成均一稳定的微胶囊复合整理剂。
(3)将上述微胶囊复合整理剂通过直接涂层方式对非织造布进行单面涂层整理，涂层完成后，在非织造布具有微胶囊复合整理剂的表面喷涂质量分数为20％氯化钙溶液，静置15min，使表面海藻酸钠大分子充分交联。再经过50℃烘干15min即可得到天然植物提取物复合衬垫材料。
实施例3
(1)微胶囊制备：将芯材液体(山茶提取物)与质量分数5％的聚乙烯醇溶液以质量比1:1的比例混合均匀制成混合液。取该混合液8g加入盛有60ml正己烷的锥形瓶中，并加入0.4g乳化剂span-80，在50℃，搅拌速度800rpm的条件下，乳化20min，制成乳化液。保持800rpm搅拌速度，向前述乳化液中加入盐酸酸化的25％戊二醛溶液(pH＝2)2.5mL。保持800rpm搅拌转速反应75min后可得微胶囊分散液。减压抽滤前述微胶囊分散液，将滤出物经石油醚，无水乙醇，蒸馏水充分洗涤后冷冻干燥即可得到微胶囊。
(2)取质量分数如下：按步骤(1)的微胶囊10％、水性聚氨酯粘合剂3％、OP-10分散剂3％、芯材液体(山茶提取物)10％、远红外纳米陶瓷粉2％、余量为海藻酸钠溶液。在室温条件下，先将芯材液体加入海藻酸钠溶液中，机械搅拌5min使之充分混合，然后加入分散剂、水性聚氨酯粘合剂、微胶囊和远红外纳米陶瓷粉，搅拌5min使之初步分散后，高速剪切分散20min制成均一稳定的微胶囊复合整理剂。
(3)将涤纶非织造布在上述微胶囊复合整理剂中浸渍2h后取出，其中非织造布上微胶囊整理剂的覆盖率为100％。然后在非织造布具有微胶囊复合整理剂的表面喷涂20％氯化钙溶液，静置15min使海藻酸钠大分子充分交联，再经过45℃烘干20min，得到微胶囊复合衬垫材料。
Claims (2)
1.一种微胶囊复合衬垫材料的制备方法，其特征在于由以下步骤组成：
(1)微胶囊的制备：在室温条件下，先将芯材溶液、壁材和乳化剂均匀混合，而后加入到反应介质中搅拌乳化5-25min，得到乳化分散体系；向乳化分散体系中加入交联剂和过量盐酸并搅拌，在40℃-60℃条件下反应60-90min，得到微胶囊分散液；减压抽滤微胶囊分散液，依次以石油醚、无水乙醇和蒸馏水洗涤除去未反应物质，得到微胶囊；
所述芯材溶液和壁材的质量比为20-30:1，乳化剂的质量为芯材溶液和壁材总质量的4%-20%，交联剂的质量为壁材质量的2.5-5倍；
所述芯材溶液为水溶性天然植物提取物；所述壁材为聚乙烯醇、聚乙二醇、海藻酸钠或壳聚糖中的至少一种；所述乳化剂为司盘-80、司盘-60、OP-10或吐温-80中的至少一种；所述反应介质为正庚烷、正己烷或石油醚中的至少一种；所述交联剂为甲醛或戊二醛的至少一种；
(2)微胶囊复合整理剂的制备：取质量分数如下：步骤（1）的微胶囊2%-20%、远红外纳米陶瓷粉1%-10%、芯材溶液2%-20%、粘合剂0.5%-5%、分散剂1%-5%、余量为海藻酸钠溶液；在室温条件下，另取芯材溶液加入到海藻酸钠溶液中搅拌2-5min，然后加入步骤（1）得到的微胶囊、远红外纳米陶瓷粉、分散剂和粘合剂，搅拌3-5min使之初步分散，再高速搅拌10-20min，使之混合均匀，得到微胶囊复合整理剂；
所述粘合剂为水性聚氨酯粘合剂或水性聚丙烯酸酯粘合剂中的至少一种；所述分散剂是十二烷基硫酸钠、OP-10或吐温-80中的至少一种；
(3)微胶囊复合衬垫材料的制备：将步骤(2)中制备的微胶囊复合整理剂通过涂覆、浸渍或浸轧工艺复合在非织造布上，然后对非织造布具有微胶囊复合整理剂的表面喷洒质量分数为10%-20%的氯化钙溶液，静置10-20分钟后，最后将非织造布在40℃-60℃下烘干10-30min，得到微胶囊复合衬垫材料。
2.根据权利要求1所述的微胶囊复合衬垫材料的制备方法，其特征在于所述水溶性天然植物提取物为山茶提取物、三叶草花提取物或可可花提取物中的至少一种。
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