CN109529737A - 一种聚氨酯胶囊的一步制备方法 - Google Patents

一种聚氨酯胶囊的一步制备方法 Download PDF

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CN109529737A
CN109529737A CN201910021636.7A CN201910021636A CN109529737A CN 109529737 A CN109529737 A CN 109529737A CN 201910021636 A CN201910021636 A CN 201910021636A CN 109529737 A CN109529737 A CN 109529737A
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李伟
孙少峰
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Tianjin Polytechnic University
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Abstract

本发明提供了一种新型聚氨酯胶囊的一步制备方法，其中以脂肪族异氰酸酯、疏水性胺、疏水性醇作为反应单体，将其与芯材物质混溶共同作为油相，通过调节体系温度及反应时间等参数，使异氰酸酯、胺、醇达到聚合条件而迁移至油水界面反应成壁，从而将芯材包覆。聚氨酯胶囊采用内原位聚合法制备得到，此研究方法工艺简单、耗能低，整个过程采用一步法制得胶囊产物，且胶囊化效率高，是一种绿色节能的生产工艺，应用范围十分广泛。

Description

一种聚氨酯胶囊的一步制备方法
技术领域
本发明涉及一种聚氨酯胶囊的一步制备方法，具体涉及到通过内原位聚合法制备具有核壳结构的聚氨酯微胶囊。
背景技术
胶囊是指采用胶囊化技术得到的具有核壳结构的微球，该技术通过将固体、液体或气体包覆于微型容器而对其起到保护或控制释放作用。随着胶囊化技术的逐渐成熟，胶囊在生物、医学、农药、建筑、食品等领域的应用日益广泛。
胶囊的合成通常采用原位聚合或界面聚合法。其中，原位聚合法制备胶囊的壁材主要是氨基树脂，然而以密胺树脂和脲醛树脂为壁材的胶囊在使用中会释放出有毒的甲醛，不可避免地威胁人体健康、引起环境污染。界面聚合法通常操作简单，对单体配比要求较低，聚合反应条件温和且反应速度较快，可广泛用于聚脲、聚氨酯胶囊的制备。
界面聚合法制备聚氨酯微胶囊过程中，通常将异氰酸酯类单体或低聚物与油相芯材混溶作为油相，油相在带羟基的亲水性表面活性剂作用下均匀分散于水相中，从而得到水包油型乳液，通过向体系中滴加水溶性胺使异氰酸酯、胺与醇在油水界面处发生聚合反应而形成聚氨酯壁材。界面聚合过程中，异氰酸酯大多选用甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)等有毒性芳香族异氰酸酯，需要控制多元胺的加入方式来解决异氰酸酯与胺反应速率过快的问题，且二异氰酸酯与水之间的副反应也会干扰胶囊产物的形貌。
专利CN106582463A“一种聚氨酯微胶囊分散液的制备方法及其产物”中，通过将多胺水溶液加入到水包油乳液中制备微胶囊浆料，制备工艺复杂，且胶囊悬浮液中不可避免地残留未反应完全的多胺水溶液，不符合绿色和谐发展理念。
发明内容
本发明提供了一种新型聚氨酯胶囊的一步制备方法，其中聚氨酯壳材是由脂肪族异氰酸酯、疏水性胺与疏水性醇通过内原位聚合得到的。
本发明制备聚氨酯胶囊的具体步骤如下：
(1)将含有异氰酸酯基团的脂肪族异氰酸酯、疏水性胺与疏水性醇按一定比例溶解在芯材物质里，以形成油相；
(2)按质量计，将100份油相物质加入到200～3000份浓度为0.1～50wt％的乳化剂水溶液中，剪切乳化得到水包油型乳液；
(3)将步骤(2)得到的水包油型乳液转移至三口烧瓶中搅拌，室温下反应一段时间后再升温熟化，即得到聚氨酯胶囊悬浮液；
(4)将步骤(3)得到的胶囊悬浮液进行进一步抽滤、洗涤、干燥处理，便可得到具有核壳结构的胶囊产品。
所述脂肪族异氰酸酯包括1，6-己二异氰酸酯，异佛尔酮二异氰酸酯，三甲基己烷二异氰酸酯中的任意一种或任意几种以任意比的混合物。
所述疏水性胺为聚天门冬氨酸酯，十八烯胺，4，4′-二辛基二苯胺，聚醚胺，萘胺，芳香胺，所组成的组中的至少一种。
所述疏水性醇为聚丙二醇，癸二醇，雌二醇，1，12-十二烷二醇，所组成的组中的至少一种。
所述芯材物质为脂肪酸酯、脂肪醇、脂肪酸、烷烃、卤化烷烃、香精油中的任意一种或任意几种以任意比的混合物；其中，所述脂肪酸酯为正十二烷酸、正十四烷酸、正十六烷酸、正十八烷酸、正二十烷酸与甲醇、乙醇、丙醇、异丙醇、丁醇经酯化合成的烷基酯中的任意一种或任意几种任意比的混合物；所述脂肪醇为C10～C20的正烷醇中的任意一种或任意几种任意比的混合物；所述脂肪酸为C8～C20的正脂肪酸中的任意一种或任意几种任意比的混合物；所述烷烃为C14～C60的正烷烃中的任意一种或任意几种任意比的混合物；所述卤化烷烃为氯化十八烷、氯化十六烷中的任意一种或任意比的混合物；所述香精油为天然香精中的柏树精油、玫瑰香精、茉莉油、柠檬油、椰子香精、薰衣草香精、安息香脂、鸢尾香脂、檀香油、岩兰草油中的至少一种、人工合成香精中合成麝香、结晶玫、香兰素、香豆素、乙酰丁香酚、苯甲酸苄酯、苯乙酸芳芳樟酯中的任意一种或任意几种任意比的混合物。
所述乳化剂为聚乙烯醇、聚乙烯吡咯烷酮、山梨糖醇酐油酸酯、乳化剂OP10、脂肪醇聚氧乙烯醚硫酸钠、苯乙烯马来酸酐共聚物、脂肪醇聚氧乙烯醚、土耳其红油、烷基苯磺酸钠、十二烷基磺酸钠，海藻酸丙二酯、聚氧乙烯山梨糖醇酐单油酸酯、烷基硫酸钠、拉开粉所组成的组中的至少一种。
所述脂肪族异氰酸酯、疏水性胺及疏水性醇总和，与芯材物质的比例为：1∶0.1～1∶20。
所述熟化温度为：30～100℃。
所述熟化时间为：0.5～50h。
本发明将脂肪族异氰酸酯、疏水性胺与疏水性醇与芯材物质混溶共同作为油相，通过调节体系温度及反应时间等参数，使异氰酸酯、胺与醇达到聚合条件而迁移至油水界面反应成壁。这种制备方法工艺简单、耗能低，整个过程采用一步法制得胶囊产物，且胶囊化效率高，是一种绿色节能的生产工艺，应用范围十分广泛。
附图说明
图1是实施例1所制备的聚氨酯微胶囊形貌图(扫描电子显微图片)
具体实施方式
以下通过具体实施例进一步说明本发明描述的方法，但是并不意味着本发明局限于这些实施例。
实施例1：
一种聚氨酯胶囊的一步制备方法，包括如下步骤：
(1)称取25g异佛尔酮二异氰酸酯，15g聚天门冬氨酸酯F2850，20g聚丙二醇-1000，加入到120g硬脂酸丁酯中混合均匀，以形成油相；
(2)将油相物质加入到500g苯乙烯马来酸酐共聚物钠盐浓度为10wt％的水溶液中，使用5000rpm转速进行高速剪切乳化15min，得到均一的水包油乳液；
(3)将乳液转移至三口烧瓶中，25℃条件下以400rpm速度进行搅拌，反应2h后再缓慢升温至60℃熟化0.5h，即得到胶囊悬浮液；
(4)将胶囊悬浮液进行进一步抽滤、洗涤、干燥处理，便可得到具有核壳结构的聚氨酯包覆硬脂酸丁酯胶囊产品。
本实施例制得的聚氨酯胶囊形貌如图1所示，从图中可知，本实施例制得的胶囊表面光滑致密，呈规整的圆球状。
实施例2：
一种聚氨酯胶囊的一步制备方法，包括如下步骤：
(1)称取55g 1，6-己二异氰酸酯，60g聚醚胺，49g癸二醇，加入到16g正十四烷酸中混合均匀，以形成油相；
(2)将油相物质加入到500g脂肪醇聚氧乙烯醚浓度为15wt％的水溶液中，使用6000rpm转速进行高速剪切乳化15min，得到均一的水包油乳液；
(3)将乳液转移至三口烧瓶中，25℃条件下以400rpm速度进行搅拌，反应2h后再缓慢升温至100℃熟化10h，即得到胶囊悬浮液；
(4)将胶囊悬浮液进行进一步抽滤、洗涤、干燥处理，便可得到具有核壳结构的聚氨酯包覆正十四烷酸胶囊产品。
实施例3：
(1)称取10g异佛尔酮二异氰酸酯，6g十八烯胺，4g雌二醇，加入到160g薰衣草香精中混合均匀，以形成油相；
(2)将油相物质加入到500g十二烷基磺酸钠浓度为15wt％的水溶液中，使用7000rpm转速进行高速剪切乳化15min，得到均一的水包油乳液；
(3)将乳液转移至三口烧瓶中，25℃条件下以500rpm速度进行搅拌，反应3h后再缓慢升温至55℃熟化30h，即得到胶囊悬浮液；
(4)将胶囊悬浮液进行进一步抽滤、洗涤、干燥处理，便可得到具有核壳结构的聚氨酯包覆薰衣草香精胶囊产品。
实施例4：
(1)称取4g三甲基己烷二异氰酸酯，3g聚天门冬氨酸酯F220，2g 1，12-十二烷二醇，加入到171g氯化十八烷中混合均匀，以形成油相；
(2)将油相物质加入到500g乳化剂OP-10浓度为15wt％的水溶液中，使用8000rpm转速进行高速剪切乳化15min，得到均一的水包油乳液；
(3)将乳液转移至三口烧瓶中，25℃条件下以500rpm速度进行搅拌，反应2.5h后再缓慢升温至30℃熟化50h，即得到胶囊悬浮液；
(4)将胶囊悬浮液进行进一步抽滤、洗涤、干燥处理，便可得到具有核壳结构的聚氨酯包覆氯化十八烷胶囊产品。

Claims (9)

1.一种具有核壳结构的聚氨酯胶囊的一步制备方法，其包括如下步骤：
(1)将含有异氰酸酯基团的脂肪族异氰酸酯、疏水性胺、疏水性醇按一定比例溶解在芯材物质里，以形成油相；
(2)按质量计，将100份油相物质加入到200～3000份浓度为0.1～50wt％的乳化剂水溶液中，剪切乳化得到水包油型乳液；
(3)将步骤(2)得到的水包油型乳液转移至三口烧瓶中搅拌，室温下反应一段时间后再升温熟化，即得到具有核壳结构的聚氨酯胶囊；
(4)将步骤(3)得到的胶囊悬浮液进行进一步抽滤、洗涤、干燥处理，便可得到最终的胶囊产品。
2.如权利要求1所述的制备方法，其特征在于：所述脂肪族异氰酸酯为1，6-己二异氰酸酯，异佛尔酮二异氰酸酯，三甲基己烷二异氰酸酯中的任意一种或任意几种以任意比的混合物。
3.如权利要求1所述的制备方法，其特征在于：所述疏水性胺为聚天门冬氨酸酯，十八烯胺，4，4′-二辛基二苯胺，聚醚胺，萘胺，芳香胺，所组成的组中的至少一种。
4.如权利要求1所述的制备方法，其特征在于：所述疏水性醇为聚丙二醇，癸二醇，雌二醇，1，12-十二烷二醇，所组成的组中的至少一种。
5.如权利要求1所述的制备方法，其特征在于：所述芯材物质为脂肪酸酯、脂肪醇、脂肪酸、烷烃、卤化烷烃、香精油中的任意一种或任意几种以任意比的混合物；其中，所述脂肪酸酯为正十二烷酸、正十四烷酸、正十六烷酸、正十八烷酸、正二十烷酸与甲醇、乙醇、丙醇、异丙醇、丁醇经酯化合成的烷基酯中的任意一种或任意几种任意比的混合物；所述脂肪醇为C10～C20的正烷醇中的任意一种或任意几种任意比的混合物；所述脂肪酸为C8～C20的正脂肪酸中的任意一种或任意几种任意比的混合物；所述烷烃为C14～C60的正烷烃中的任意一种或任意几种任意比的混合物；所述卤化烷烃为氯化十八烷、氯化十六烷中的任意一种或任意比的混合物；所述香精油为天然香精中的柏树精油、玫瑰香精、茉莉油、柠檬油、椰子香精、薰衣草香精、安息香脂、鸢尾香脂、檀香油、岩兰草油中的至少一种、人工合成香精中合成麝香、结晶玫、香兰素、香豆素、乙酰丁香酚、苯甲酸苄酯、苯乙酸芳芳樟酯中的任意一种或任意几种任意比的混合物。
6.如权利要求1所述的制备方法，其特征在于：所述乳化剂为聚乙烯醇、聚乙烯吡咯烷酮、山梨糖醇酐油酸酯、乳化剂OP10、脂肪醇聚氧乙烯醚硫酸钠、苯乙烯马来酸酐共聚物、脂肪醇聚氧乙烯醚、土耳其红油、烷基苯磺酸钠、十二烷基磺酸钠，海藻酸丙二酯、聚氧乙烯山梨糖醇酐单油酸酯、烷基硫酸钠、拉开粉所组成的组中的至少一种。
7.如权利要求1所述的制备方法，其特征在于：所述脂肪族异氰酸酯、疏水性胺及疏水性醇总和，与芯材物质的比例为：1∶0.1～1∶20。
8.如权利要求1所述的制备方法，其特征在于：所述熟化温度为：30～100℃。
9.如权利要求1所述的制备方法，其特征在于：所述熟化时间为：0.5～50h。
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