CN115135407A - 以水溶性组合物为内包物的两层无缝胶囊 - Google Patents
以水溶性组合物为内包物的两层无缝胶囊 Download PDFInfo
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- CN115135407A CN115135407A CN202180014882.5A CN202180014882A CN115135407A CN 115135407 A CN115135407 A CN 115135407A CN 202180014882 A CN202180014882 A CN 202180014882A CN 115135407 A CN115135407 A CN 115135407A
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- water
- capsule
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- soluble
- seamless capsule
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/206—Hardening; drying
Abstract
本申请提供一种以水溶性组合物为内包物的两层无缝软胶囊,通过由紫外线固化性组合物制备胶囊覆膜,制造出内包物的因透过覆膜所致的挥发性小的、由胶囊覆膜和作为水溶性组合物的内包物构成的两层无缝胶囊。
Description
技术领域
本发明涉及一种两层无缝胶囊,其由从紫外线固化性树脂组合物制备的胶囊覆膜和作为水溶性组合物的内包物构成。本发明的胶囊可以以水溶性香料等作为内包物。
背景技术
在无缝胶囊制造中采用的滴加法(又称浸没固化法)是利用液-液(内包液-覆膜液、覆膜液-冷却油液)之间的表面张力或者气-液(空气-覆膜液)之间的表面张力的胶囊制造方法。以往,广泛使用如下的制法:分别将水溶性的覆膜用组合物(例如明胶等的水溶液)从同心双层喷嘴的外侧喷嘴、将疏水性的内包液从内侧喷嘴向已冷却的油液喷出,形成同心双层液滴,将外侧的液滴(覆膜液)通过冷却而凝胶化,制成胶囊。在该制造方法中存在如下问题:当用作覆膜的覆膜用组合物为水溶性时,胶囊内包物限于与覆膜用组合物具有表面张力的油脂或油溶性物质的油脂溶液等,水溶性成分无法制成胶囊。因此,开发了使水溶性成分分散到油性液体中(例如,参照专利文献1)、或者使其乳化(例如,参照专利文献2和3)而成为胶囊的方法。
此外,作为被封入到香烟的过滤嘴部分中的胶囊,提出了如下的胶囊:由选自结冷胶、琼脂、藻酸盐、角叉菜胶、果胶、阿拉伯胶、茄替胶、普鲁兰胶、甘露胶或改性淀粉中的至少一种亲水胶体单独,或它们的混合物,或者与明胶的混合物形成壳;以亲油性或部分溶于乙醇的物质或产品、或油/水/油型的乳剂为芯(例如,参照专利文献4)。
另一方面,作为内包物为亲水性物质的胶囊,提出了如下的以亲水性物质为内包物的无缝胶囊:在由内包物和包覆该内包物的覆膜形成的无缝胶囊中,在内包物和覆膜之间夹着蔗糖的低级脂肪酸酯(例如,参照专利文献5)。然而,在这样的胶囊中,覆膜与芯中所含的成分的分隔不充分,只能暂时防止芯中所含的成分与胶囊覆膜直接接触。
[现有技术文献]
[专利文献]
[专利文献1]日本特开平1-186815号公报
[专利文献2]日本特开平11-342329号公报
[专利文献3]日本特开平9-327501号公报
[专利文献4]日本特开2014-166188号公报
[专利文献5]日本特开平3-52639号公报
发明内容
发明要解决的课题
本发明的课题在于提供一种以水溶性组合物为内包物的两层无缝胶囊。
解决课题的方法
本发明的发明人对使用水或水溶性香味剂等水溶性组合物作为胶囊内包物时的各种覆膜组成进行了研究后发现,通过由紫外线固化性树脂组合物制备胶囊覆膜,内包物因透过覆膜而导致的挥发性变小,从而香料成分的挥发变少,由此完成了本发明。此外,本发明可以应用于三层以上的无缝胶囊。
即,本发明如下所述。
[1]一种两层无缝胶囊,由从紫外线固化性树脂组合物制备的胶囊覆膜和为水或水溶性组合物即内包物构成。
[2]如上述[1]所述的无缝胶囊,其特征在于,紫外线固化性树脂组合物的粘度为20~2000mPa·s。
[3]如上述[1]或[2]所述的无缝胶囊,其特征在于,紫外线固化性树脂组合物为丙烯酸系树脂组合物、环氧系树脂组合物或有机硅树脂组合物。
[4]如上述[1]~[3]中任一项所述的无缝胶囊,其特征在于,丙烯酸系树脂组合物含有丙烯酸系低聚物、丙烯酸系单体和光聚合引发剂。
[5]如上述[1]~[4]中任一项所述的无缝胶囊,其特征在于,水溶性组合物含有水、水溶性香料、水溶性醇类、甘油或丙二醇。
[6]如上述[1]~[5]中任一项所述的无缝胶囊,其特征在于,利用三维X射线显微镜测量的胶囊覆膜的最薄部的膜厚度为100μm以上。
[7]如上述[1]~[6]中任一项所述的无缝胶囊,其特征在于,直径为1~6mm。
[8]如上述[1]~[7]中任一项所述的无缝胶囊,其特征在于,在20℃下保存60天后的质量减少小于5%。
[9]如上述[1]~[8]中任一项所述的无缝胶囊,其特征在于,被封装在香烟过滤嘴中。
[10]一种具备内包物和包覆内包物的覆膜的两层无缝胶囊的制造方法,其特征在于,具备:
(a)作为内包物而准备(调制)水或水溶性组合物的工序;
(b)作为胶囊覆膜液而准备紫外线固化性树脂组合物的工序;
(c)使用同心双喷嘴,从外侧喷嘴将所述胶囊覆膜液、从内侧喷嘴将所述水或水溶性组合物向形成用液喷出,形成两层液滴,通过对该两层液滴照射紫外线,使胶囊覆膜液固化而成为胶囊覆膜的工序。发明效果
根据本发明,可以提供内包物中的挥发性成分的挥发较少的无缝软胶囊。
具体实施方式
作为本发明的两层无缝胶囊,只要是由从紫外线固化性树脂组合物制备(调制)的胶囊薄膜和作为水溶性组合物的内包物构成的两层无缝胶囊即可,没有特别的限制,所述胶囊覆膜通过对紫外线固化性树脂组合物照射紫外线而得到,该紫外线固化(性)树脂根据反应机理的不同而大致分为自由基聚合型树脂和阳离子聚合型树脂。
在上述紫外线固化树脂为自由基聚合型树脂的情况下,作为自由基聚合型树脂,可以优选举出丙烯酸系树脂或有机硅树脂,上述丙烯酸系树脂只要是构成聚合物骨架的要素是(甲基)丙烯酸单体即可,没有特别的限制,例如可以举出选自(甲基)丙烯酸、(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂酯、丙烯酸十八酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸2-三氟乙酯等的(甲基)丙烯酸的(氟代)烷基酯、(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丙酯、(甲基)丙烯酸4-羟丁酯、(甲基)丙烯酸缩水甘油酯、(甲基)丙烯酸甲基缩水甘油酯、(甲基)丙烯酸3,4-环氧环己基甲基酯、(甲基)丙烯酰吗啉、(甲基)丙烯酸烯丙酯等中的一种或两种以上的(甲基)丙烯酸聚合物。这里,除非特别明述,“(甲基)丙烯酸酯”(或“(甲基)丙烯酸”)是指甲基丙烯酸酯(或甲基丙烯酸)和/或丙烯酸酯(或丙烯酸)。
作为上述丙烯酸系树脂组合物,可以优选举出含有光聚合性(甲基)丙烯酸酯系低聚物和/或光聚合性(甲基)丙烯酸酯系单体和光聚合引发剂的丙烯酸系树脂组合物。
作为上述光聚合性(甲基)丙烯酸酯系低聚物,只要是分子内具有作为自由基聚合性官能团的丙烯酰基的(甲基)丙烯酸酯低聚物即可,没有特别限制,可以举出具有选自聚亚烷基、聚丁二烯、氢化聚丁二烯、聚异戊二烯和氢化聚异戊二烯的各骨架中的一种或两种以上骨架的(甲基)丙烯酸酯低聚物或氨基甲酸酯(甲基)丙烯酸酯低聚物。
作为上述丙烯酸酯系单体没有特别限定,可以举出丙烯酸2-乙基己酯、丙烯酸2-羟乙酯、2-羟乙基丙烯酰磷酸酯等的单官能单体,二丙烯酸1,3-丁二醇酯、二丙烯酸1,6-己二醇酯、丙烯酸二乙二醇酯等的双官能单体,三羟甲基丙烷三丙烯酸酯、季戊四醇三丙烯酸酯、二季戊四醇六丙烯酸酯等的三官能以上的丙烯酸单体。这些单体既可以单独使用,也可以将两种以上组合使用。
作为上述丙烯酰系树脂组合物中所含的光聚合引发剂,只要是能够感应紫外线而引发自由基聚合的化合物即可,没有特别限定,例如可以举出二苯甲酮、苯甲酰乙醚、苯甲酰甲醚、苯甲酰异丙醚等苯甲酰烷基醚类;2-(邻氯苯基)-4,5-二苯基咪唑二聚体、2-(邻氯苯基)-4,5-双-(间甲氧基苯基)咪唑二聚体、2-(对甲氧基苯基)-4,5-二苯基咪唑二聚体等的2,4,5-三芳基咪唑二聚体类;二苄基硫醚(シヘンゾイルスルフィド)、硫化四甲基秋兰姆等的硫化合物等。
作为上述丙烯酰系树脂组合物,也可以使用市售品,具体而言,可以举出TB3042B、TB3066、TB3013D、TB3067、TB3064E、TB3094B(均为三键株式会社制),Hitaroid 7975、Hitaroid 7988、Hitaroid 7975D(均为日立化成株式会社制),UV-7605B、UV-7620EA(均为三菱化学控股株式会社制),Aronix系列(东亚合成株式会社制)等。
有机硅树脂是一种以硅氧烷键为主链的聚合化合物。作为有机硅树脂组合物,也可以使用市售品,具体而言,可以举出TB3161、TB3163、TB3164D(均为三键株式会社制),KUV-3433-UV、KER-4700-UV、KER-4800-UV(均为信越化学工业株式会社制)等。
在上述紫外线固化树脂为阳离子聚合型树脂的情况下,作为该阳离子聚合型树脂,可优选举出环氧系树脂;作为上述环氧系树脂,可以举出双酚A型环氧树脂、双酚F型环氧树脂、双酚S型环氧树脂、双酚AD型环氧树脂、萘型环氧树脂、联苯型环氧树脂、缩水甘油胺型环氧树脂、溴化双酚A型环氧树脂、氢化双酚A型环氧树脂、脂环式环氧树脂、双环戊二烯型环氧树脂、苯酚酚醛清漆型环氧树脂、邻甲酚酚醛清漆型环氧树脂等一种或多种环氧树脂。
作为上述环氧系树脂组合物,可以优选举出含有形成环氧树脂的阳离子聚合性化合物以及光聚合引发剂的环氧系树脂组合物。
上述形成环氧树脂的阳离子聚合性化合物可以举出在一个分子中具有一个或两个以上具有阳离子聚合性基团的环氧基团的化合物;具体而言,可以举出环戊二烯二氧化物、(3,4-环氧环己基)甲基-3,4-环氧环己烷羧酸酯、双(2,3-环氧环戊基)醚、双(3,4-环氧环己基甲基)己二酸酯、双(3,4-环氧-6-甲基环己基甲基)己二酸酯、(3,4-环氧-6-甲基环己基)甲基-3,4-环氧-6-甲基环己烷羧酸酯、双(3,4-环氧环己基甲基)缩醛、乙二醇的双(3,4-环氧环己基)醚、乙二醇的3,4-环氧环己烷羧酸二酯、(3,4-环氧环己基)甲醇、(3,4-环氧环己基)乙基三甲氧基硅烷、3-乙基-3-(3,4-环氧环己基甲基)氧甲基氧杂环丁烷等的含有脂环式环氧基的环氧化合物;乙二醇二缩水甘油醚、丙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚、聚丙二醇二缩水甘油醚、1,4-丁二醇二缩水甘油醚、新戊二醇二缩水甘油醚、1,6-己二醇二缩水甘油醚、甘油二缩水甘油醚、双甘油四缩水甘油醚、三羟甲基丙烷三缩水甘油醚、螺二醇二缩水甘油醚、2,6-二缩水甘油基苯基醚、山梨糖醇聚缩水甘油醚、异氰脲酸三缩水甘油酯、双酚A二缩水甘油醚、二氧化丁二烯、邻苯二甲酸二缩水甘油酯、3-乙基-3-缩水甘油氧基甲基氧杂环丁烷、卤化双酚A型环氧树脂、双酚F型环氧树脂、邻、间、对甲酚酚醛清漆型环氧树脂、苯酚酚醛清漆型环氧树脂等的含有脂肪族环氧基的环氧化合物;乙烯基环己烯二氧化物、二氧化柠檬烯等的含有脂环式环氧基和脂肪族环氧基的环氧化合物;等等;这些化合物可以单独使用或将两种以上组合使用。
作为上述环氧系树脂组合物中所含的光聚合引发剂,可以举出感应紫外线而产生阳离子聚合引发剂的化合物,例如可以举出ArN2·PFe-、ArN2·SbFe-、ArN2·AsFe-、(ArN2 +)2SnCl6 -、ArN2·FeCl4 -等的重氮盐(其中Ar为C6H5);对苯基苄基甲基锍盐、对苯基二甲基锍盐、对羟基苯基苄基甲基锍盐等苄基甲基锍盐,或三苯基锍盐、二苯基-4-噻吩氧基苯基锍盐等三芳基锍盐等的芳基锍盐。
作为上述环氧系树脂组合物,也可以使用市售品,具体而言,可以举出TB3121D(三键株式会社制)、Hitaroid 7663(日立化成株式会社制)、Aron Oxetane(东亚合成株式会社制))、Luxidia系列(DIC株式会社制)等。
在上述紫外线固化性树脂组合物中还可以添加光敏剂、高分子胶凝剂、胶凝助剂、覆膜增强剂、增塑剂、着色剂等。
作为上述紫外线固化性树脂组合物的粘度,可以举出20~2000mPa·s,优选为100~1500mPa·s。如果粘度较高,则容易卷入气泡,制造时的处置变得困难,难以得到良好的胶囊。
作为本发明两层无缝胶囊的内包物,只要是水溶性组合物(水性组合物)即可,没有特别限定,也可以在水中溶解多种亲水性物质。作为本发明中的亲水性物质,只要是分子结构的一部分具有羟基、羧基、氨基、酮基、磺基等容易与水分子之间形成键的官能团,可溶于水的物质即可,没有特别限定;具体而言,可以举出水、水溶性醇、甘油、丙二醇等水溶性溶剂、水溶性维生素、糖醇、天然甜味剂、人造甜味剂、低聚糖类、多糖类、水溶性香料等。
作为上述水溶性维生素,可以举出维生素B1(硫胺素)、维生素B2(核黄素)、维生素B3(烟酸、烟酰胺)、维生素B5(泛酸、右泛醇)、维生素B6(吡哆醇、磷酸吡哆醛、吡哆胺)、维生素B7(生物素)、维生素B9(叶酸)、维生素B12(氰钴胺、甲基钴胺)等维生素B族和维生素C(抗坏血酸、脱氢抗坏血酸)。
作为上述糖醇,可以举出赤藓糖醇、木糖醇、山梨糖醇、帕拉金糖醇、麦芽糖醇、乳糖醇和甘露糖醇。
作为上述天然甜味剂,可以举出蔗糖、甜叶菊、甘草甜素和罗汉果。另外,作为人造甜味剂,可以举出糖精、阿斯巴甜、乙酰舒泛钾、三氯蔗糖等。
作为上述低聚糖类,可以举出低聚果糖、低聚半乳糖、低聚木糖、低聚帕拉金糖、低聚琼脂糖、甲壳质低聚糖、低聚异麦芽糖、低聚麦芽糖、棉子糖、乳果糖等。此外,作为上述多糖类,可以举出海藻酸丙二醇酯、阿拉伯胶、黄芪胶、刺梧桐胶、茄替胶、黄原胶、瓜尔豆胶、刺槐豆胶、塔拉胶、λ-角叉菜胶、μ-角叉菜胶、ν-角叉菜胶、纤维素和淀粉等冷却时不凝胶化的水溶性多糖类。
作为上述水溶性香料,只要是具有增强食品等原本带有的香味(增香)、补充食品原材料原有香味(赋香)、在因加工工序中的加热香味或发酵臭味而产生不适合食品的气味时对味道进行矫正(掩蔽)等作用,具有亲水性物质性质的香料组合物即可,没有特别限制,可以举出水溶性天然香料、水溶性合成香料、水溶性香料、水包油型乳化香料。
具体可以举出:将植物材料经干燥、切碎、粉碎等处理后,用水、乙醇、1,3-丁二醇、丙二醇、甘油等水溶性溶剂提取的所谓回收香味剂;将植物添加到乙醇中并进行搅拌后,在低温下放置,使其分离成含有香料物质的下层(含水乙醇层)和含有水不溶性组分的上层,通过过滤等方法回收下层的含水乙醇层而制备的香料;用有机溶剂提取植物材料,加入乙醇、甘油、丙二醇等并回收溶剂而获得香气浓缩物,由此制备的水溶性香料(例如,日本专利6032991号公报)。
作为上述水溶性天然香料,可以举出青柠、葡萄柚和橙子等柑橘系天然香料、芒果系天然香料、苹果系天然香料、葡萄香精、菠萝系天然香料、草莓系天然香料等。
作为上述水溶性合成香料,只要是化学合成的水溶性合成香料即可,没有特别限制,可以举出己醇、苯乙醇、顺-3-己烯醇、橙花油、异戊醇、香茅醇、薄荷醇、1-戊醇、肉桂醇、1-辛烯-3-醇、紫苏醇、法尼醇、芳樟醇、松油醇、香叶醇、苯甲醇、糠醇等。
作为上述水溶性香料(香精),可以举出将通过调配许多种油溶性和/或水溶性天然香料、合成香料而制得的香味剂基料用乙醇、甘油等溶于水的物质稀释而成的香味剂香料,可以例举出柠檬香精、青柠香精、葡萄柚香精、橙子香精、柚子香精、苹果香精、甜瓜香精、薄荷香精、蜂蜜香精、草莓香精、黑加仑香精、蔓越莓香精、樱桃香精、菠萝香精、木瓜香精,香蕉香精、蓝莓香精、芒果香精、桃香精、梨香精、绿茶香精、红茶香精、可可香精、巧克力香精、咖啡香精、酸奶香精、肉桂香精、生姜香精、百里香香精、肉豆蔻香精、薄荷香精、香草香精等。
作为上述水包油型乳化香料,可以举出使用阿拉伯胶溶液、羧甲基纤维素、皂苷、卵磷脂等作为乳化剂将含有油溶性天然香料/合成香料的香味剂的香料乳化分散在水溶液中而得到的水包油型乳液(乳化香料);可以例举出菠萝乳化香料、橙子乳化香料、咖啡乳化香料、黄油乳化香料、奶酪乳化香料等。
作为上述粉末香料,可以举出将调配许多种天然香料或合成香料而成的香味剂基料与糊精、天然胶质、糖、淀粉等赋形剂一起乳化后喷雾干燥而成粉末状的水溶性香料,可以例举出柠檬粉末香料、橙子粉末香料、苹果粉末香料、黄油粉末香料、奶酪粉末香料、香草粉末香料。
在不损害本发明效果的范围内,可以进一步添加水溶性色素、增稠多糖类、果胶等膳食纤维来调制上述内包物。
作为本发明的两层无缝胶囊的制造方法,可以举出以往使用的无缝胶囊的制造方法,例如滴加法;从同心双喷嘴的外侧喷嘴将覆膜液的紫外线固化性树脂组合物,从内侧喷嘴将内包物的水溶性组合物分别同时喷出,向形成用液中导入,通过表面张力形成两层液滴。两层液滴的外侧的作为覆膜液的紫外线固化性树脂组合物在于形成用液中移动的期间中被照射紫外线而固化,成为胶囊覆膜,成为内包水溶性组合物的胶囊。
在上述两层液滴中,作为使紫外线固化性树脂组合物中的树脂固化的方法,只要是能够照射紫外线而使覆膜固化的方法即可,没有特别限定,可以例举出将胶囊与形成用液一起导入到玻璃或石英等的紫外线透过性较高的材质的管中,以夹着该管的方式从1个或2个以上方向照射UV光源的方法。
作为本发明的通过紫外线使树脂组合物固化时的紫外线波长,优选为处于210nm~470nm、更优选为处于270~410nm的能量区域的波长。作为光强度,可以举出累积光量为5kJ/m2~50kJ/m2,优选为10kJ/m2~35kJ/m2;为了得到这样的光量,为了得到规定的累积光量,需要适当改变胶囊的移动速度和照射速度,例如可以例示,当需要累积光量为15kJ/m2时,将胶囊的移动速度设为5cm/s,将照射速度设为3W/cm2(工作距离5mm),进行2秒以上的照射。
作为本发明两层结构无缝胶囊的制造方法中的形成用液,可以优选举出水或具有粘性的水溶性组合物,具体可以举出阿拉伯树胶、阿拉伯半乳聚糖、卡拉亚树胶、茄替胶、黄芪胶、刺槐豆胶、瓜尔豆胶、洋车前子胶、罗望子胶、塔拉胶、海藻酸类、角叉菜胶、琼脂、低分子化琼脂、叉红藻胶、果胶、可得然胶、黄原胶、结冷胶、普鲁兰胶、纤维素、壳聚糖等所谓的增稠多糖水溶液、可溶性淀粉、淀粉糊、山梨糖醇液等液体糖醇、甘油等多元醇、还原麦芽糖糖浆等糖浆类等,只要是通过溶解于水或者与水混合而使水具有粘性的物质即可,没有特别限制,只要通过适当改变在水中的稀释率来调整到适合使用的粘度即可。
在通常的胶囊制造中,一般需要耗时较长的干燥工序。在本发明的紫外线照射后的胶囊制造工序中,不一定需要利用通风的旋转干燥或真空干燥法等的干燥工序,能够提高制造工序的效率,这也是极其有利的方面。
本发明的胶囊可以通过以某种方法使胶囊覆膜破裂或添加裂纹等来释放内包物以供使用。作为使胶囊覆膜破裂的方法,例如可以使用人体的一部分或某种工具进行挤压。作为对胶囊膜添加裂纹的方法,例如可以使用刀等的锋利的工具添加切口。
作为本发明胶囊的挥发性(率),在以胶囊在20℃下保存60天后的质量减少率表示时,可以举出小于5%、优选为小于3%。
作为本发明胶囊的胶囊覆膜的最薄部的膜厚,优选为100μm以上。胶囊覆膜的最薄部的膜厚可以用三维X射线显微镜测量。
作为本发明的无缝胶囊的形状没有特别限定,通常为球形。还可以通过在成型时施加若干外力等的方法来做成橄榄球形(OVAL)或椭圆形(OBLONG)等的球形以外的形状。
作为本发明的无缝胶囊的粒径,可以举出1~6mm,优选为2~5mm。
作为本发明的无缝胶囊的质量,可以举出10~300mg,优选为20~200mg,更优选为50~150mg。
作为本发明的无缝胶囊的用途,可举出封入到香烟过滤嘴中的香料胶囊、芳香剂、化妆品、日用品。
以下,通过实施例更具体地说明本发明,但本发明的技术范围不限于这些示例。
[实施例]
[实施例1]
在表1中示出了在以下实施例中使用的紫外线固化性树脂。
[表1]
※粘度:B型粘度计(TOKIMEC公司制)
(内包水的胶囊)
作为紫外线固化性树脂组合物,使用从含有丙烯酸酯低聚物、丙烯酸酯单体、丙烯酸和光聚合引发剂的、表1中列出的紫外线固化性树脂A得到的丙烯酸酯树脂组合物,制备胶囊覆膜,以水为内包物,制成两层无缝胶囊。
使用同心双层喷嘴(富士胶囊公司制),通过从外侧喷嘴喷出丙烯酸酯树脂组合物、从内侧喷嘴喷出水,形成两层液滴。将粘度调整为10mPa·s(25℃;B型粘度计)的形成用液中的上述两层液滴的移动速度设为5cm/s。
将上述两层液滴与形成用液一起导入到20cm玻璃管中,以接着该玻璃管的方式从两个方向设置两个线型UV光源(E110II-HD,牛尾电机公司),照射紫外线(波长365nm),进行覆膜的固化。由于用于将紫外线固化性树脂组合物固化的累积光量为15kJ/m2,所以调整形成用液的流速以使胶囊的移动速度成为5cm/s左右,以照射强度3W/cm2(工作距离5mm)照射2秒以上。
(挥发性试验)
对于上述内包水的胶囊,使用“高分辨率三维X射线显微镜Nano3DX”(理学公司制)测量胶囊覆膜的最薄部的膜厚,取5个胶囊覆膜的最薄部的膜厚实测值为100μm以上的胶囊,测量平均总质量,于20℃条件下保存于玻璃瓶中,基于第30天和第60天测量的总质量,计算与保存开始日的质量相比的减少率,将其结果示于表2。
[表2]
(结果)
由表2可知,在使用水作为内包物的情况下,最薄部的膜厚为100μm以上的胶囊60天后的质量变化小于5%,挥发性较低,可以认为实现了内包物的封入。
(挥发性严苛试验)
对以水和上述葡萄柚香味水溶液作为内包物、使用紫外线固化性树脂A作为紫外线固化性树脂组合物制备了胶囊覆膜的胶囊的挥发性进行了严苛试验。在测量胶囊的质量后,将胶囊在真空条件(50hPa)下存放30分钟,然后测量质量,计算减少率。将结果示于表3。
[表3]
严苛试验(内包液透过性评价)
*:比较例1中“減少率”为2%,但挥发成分在胶囊内包物中仅含有10%(用MCT稀释),作为挥发性成分的挥发量而言,大约为20%.
由表3可知,以往的卡拉胶覆膜胶囊(比较例)的质量减少率为挥发性成分量的约20%,考虑到是香料中的挥发性成分通过并透过薄膜而泄漏了。另一方面,在具有从紫外线固化性树脂组合物制备的覆膜的内包水的胶囊和内包葡萄柚香精的胶囊中,在真空条件下没有质量变化(0%),因此确认了本发明的胶囊覆膜能够将内包物中所含的挥发成分封入。
[实施例2]
(使用其他树脂的内包水的胶囊-1)
作为紫外线固化性树脂组合物,使用从在表1中列出的紫外线固化性树脂B得到的有机硅树脂组合物制备胶囊覆膜,以水为内包物,与实施例1同样进行两层无缝胶囊的制造,分别能够正常地制造出胶囊。
将上述两层液滴与固化用液形成用液一起导入到20cm的无色透明管中,以夹着该管的方式从两个方向设置两个线型UV光源(E110II-HD,牛尾电机株式会社制),照射紫外线(波长365nm),进行覆膜的固化,结果能够形成胶囊。
[比较例2]
(使用其他树脂的内包水的胶囊-2)
作为紫外线固化性树脂组合物,使用在表1中列出的紫外线固化性树脂C得到的丙烯酸系树脂组合物制备胶囊薄膜,以水为内包物,尝试按照实施例1制作两层无缝胶囊,结果无法形成良好的胶囊。
[工业可利用性]
本发明的无缝胶囊可作为能够长期稳定地保持亲水性挥发性物质的内包水溶性组合物的无缝胶囊而应用于医药品、药妆品、化妆品、家用日用品、工业用品等领域。
Claims (10)
1.一种两层无缝胶囊,由从紫外线固化性树脂组合物制备的胶囊覆膜和为水或水溶性组合物的内包物构成。
2.如权利要求1所述的无缝胶囊,其特征在于,紫外线固化性树脂组合物的粘度为20~2000mPa·s。
3.如权利要求1或2所述的无缝胶囊,其特征在于,紫外线固化性树脂组合物为丙烯酸系树脂组合物、环氧系树脂组合物或有机硅树脂组合物。
4.如权利要求1~3中任一项所述的无缝胶囊,其特征在于,丙烯酸系树脂组合物含有丙烯酸系低聚物、丙烯酸系单体和光聚合引发剂。
5.如权利要求1~4中任一项所述的无缝胶囊,其特征在于,水溶性组合物含有水、水溶性香料、水溶性醇类、甘油或丙二醇。
6.如权利要求1~5中任一项所述的无缝胶囊,其特征在于,利用三维X射线显微镜测量的胶囊覆膜的最薄部的膜厚度为100μm以上。
7.如权利要求1~6中任一项所述的无缝胶囊,其特征在于,直径为1~6mm。
8.如权利要求1~7中任一项所述的无缝胶囊,其特征在于,在20℃下保存60天后的质量减少小于5%。
9.如权利要求1~8中任一项所述的无缝胶囊,其特征在于,被封入在香烟的过滤嘴中。
10.一种具备内包物和包覆内包物的覆膜的两层无缝胶囊的制造方法,其特征在于,具备:
(a)作为内包物而准备水或水溶性组合物的工序;
(b)作为胶囊覆膜液而准备紫外线固化性树脂组合物的工序;
(c)使用同心双喷嘴,从外侧喷嘴将所述胶囊覆膜液、从内侧喷嘴将所述水或水溶性组合物向形成用液喷出,形成两层液滴,通过对该两层液滴照射紫外线,使胶囊覆膜液固化而成为胶囊覆膜的工序。
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- 2021-03-26 JP JP2022510739A patent/JP7383318B2/ja active Active
- 2021-03-26 CN CN202180014882.5A patent/CN115135407A/zh active Pending
- 2021-03-26 EP EP21774018.2A patent/EP4129414A4/en active Pending
- 2021-03-26 WO PCT/JP2021/012876 patent/WO2021193921A1/ja active Application Filing
- 2021-03-26 US US17/911,904 patent/US20230148278A1/en active Pending
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EP4129414A1 (en) | 2023-02-08 |
EP4129414A4 (en) | 2024-04-03 |
JPWO2021193921A1 (zh) | 2021-09-30 |
WO2021193921A1 (ja) | 2021-09-30 |
US20230148278A1 (en) | 2023-05-11 |
JP7383318B2 (ja) | 2023-11-20 |
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