CN108425248A - 一种纳米温控缓释芳香微胶囊的制备方法 - Google Patents
一种纳米温控缓释芳香微胶囊的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米温控缓释芳香微胶囊的制备方法,该纳米温控缓释芳香微胶囊以相变材料为载体与香料形成共熔体作为芯材,以高分子聚合物为壁材,通过混合、乳化和乳液聚合过程制得。本发明得到一种纳米温控缓释芳香微胶囊,优势在于有两道缓释机制。一是利用相变材料作为载体实现温控缓释;二是致密的高分子聚合物壁材。该产品环保无毒、机械强度高、耐热性好。可用于纺织、日化用品和建筑物等增香留香。
Description
技术领域
本发明涉及一种微胶囊制备方法,尤其是涉及一种具有温度控制芳香气息释放速率的纳米级芳香微胶囊的制备方法。
背景技术
芳香微胶囊是用成膜材料将液体香精包裹形成微小颗粒。如果在芳香微胶囊芯材中添一定量的能够与香精形成共熔的相变材料。则在相变材料熔融温度以下,芯材中的固体相变材料可将香精包住,实现自封闭,使香精的释放速率大大降低;当外界温度大于相变材料的熔点时,香精可通过熔融的相变材料和具有微孔结构的囊壁快速释放出来,通过相变材料的融化和凝结来实现芳香微胶囊的温控缓释。
例如公开号为CN103642462A的实用新型专利公开了一种毫米级温控缓释芳香凝胶胶囊的制备方法,由有机相变材料微胶囊和香精混合物作为凝胶胶囊的芯材,所制备的凝胶胶囊既具有温度调节功能而且具有温控缓释芳香气息的功能。
此外,公开号为CN103464063A的实用新型专利公开了一种温控芳香双层微胶囊及其制备方法,该方法以聚甲基丙烯酸甲酯为壁材先将有机相变材料包覆形成微胶囊,然后采用β-环糊精包覆吸附了香精的有机相变微胶囊。通过相变微胶囊的蓄热调温功能控制微胶囊中香精的释放速率。
以上制作方法先将相变材料微胶囊化后与香精混合再进行包覆处理,实际上相变材料对香味释放速率的控制较弱,容易造成温度对香气释放速率影响不均匀。若直接将相变材料与香精混合形成共熔体则能真正实现香精缓释的温度响应,并且有利于香精微胶囊粒的包覆。能得到粒径更小,包覆率高的纳米级温控缓释芳香微胶囊。
发明内容
本发明的目的在于提供一种纳米温控缓释芳香微胶囊的制备方法,利用微胶囊技术,以有机相变材料和油溶性香精作为微胶囊芯材、高分子聚合物为壁材,形成微胶囊缓释结构,芯材中的固体相变材料可将香精包住,实现自封闭,使香精的释放速率大大降低;当外界温度大于相变材料的熔点时,香精可通过熔融的相变材料和具有微孔结构的囊壁快速释放出来,通过相变材料的融化和凝结来实现芳香微胶囊的温控缓释。
为了解决上述技术问题,采用如下技术方案:
一种纳米温控缓释芳香微胶囊的制备方法,其特征在于包括如下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料:
(2)芯材组分制备:将上述比例的相变材料载体和香精在30-35℃下,密闭容器内,以800-1200r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的单体和引发剂在30-35℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在30-45℃下搅拌活化,制得水相组分;
(5)原料乳化:在30-45℃的温度下,将所述的油相组分加入到水相组分中,并且以12000-20000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65-80℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
优选后,所述的相变材料载体为脂肪醇、脂肪酸或它们的共熔体。该相变材料能够与香精形成良好的共熔体系,从而达到温控缓释效果。常用的相变材料载体为硬脂酸丁酯、十四醇、月桂酸等油溶性有机相变材料,适用于纺织服装的整理。
优选后,所述的单体为甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸叔丁酯、丙烯酸异辛酯、二乙烯基苯、苯乙烯、二甲基丙烯酸乙二醇酯中的一种或者多种;
优选后,所述单体为甲基丙烯酸甲酯和丙烯酸丁酯的共聚物。
优选后,所述乳化剂为离子型乳化剂。
优选后,所述乳化剂为十二烷基苯磺酸钠。
优选后,所述的引发剂为偶氮二异庚腈、偶氮二异丁腈、偶氮二异丁酸二甲酯或过氧化二苯甲酰。
优选后,所述的引发剂为偶氮二异庚腈。
由于采用上述技术方案,具有以下有益效果:
1、利用微胶囊技术,以有机相变材料和油溶性香精作为微胶囊芯材、高分子聚合物为壁材,形成微胶囊缓释结构,芯材中的固体相变材料可将香精包住,实现自封闭,使香精的释放速率大大降低;当外界温度大于相变材料的熔点时,香精可通过熔融的相变材料和具有微孔结构的囊壁快速释放出来,通过相变材料的融化和凝结来实现,当温度低于芯材熔点时香精的释放速率减缓;
2、本方法制备的芳香微胶囊的粒径明显低于现有技术的同类产品,达到纳米级别,颗粒的比表面积大,使得微胶囊与目标物之间的物理吸附作用很强,在使用过程中微胶囊颗粒不会从被施加物的表面脱落。
3、本发明基于微胶囊技术,制得纳米温控缓释芳香微胶囊,可应用与纺织、日化和建筑等领域,赋予被施加物品以周围环境温度的变化控制香味释放速度的功能。
4、本发明简化了工艺步骤、减少了能源消耗。
附图说明
下面结合附图对本发明作进一步说明:
图1为本发明实施例1制备的纳米温控缓释芳香微胶囊的电子显微镜图;
图2为本发明实施例1制备的纳米温控缓释芳香微胶囊的粒径分布图;
图3为本发明实施例5制备的纳米温控缓释芳香微胶囊的DSC曲线及微胶囊香精释放速率与纯香精释放速率对比图;
图4为本发明实施例5制备的纳米温控缓释芳香微胶囊在不同温度下自然放置微胶囊的释香速率。
具体实施方式
本发明提供了一种纳米温控缓释芳香微胶囊的制备方法,包括以下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料,20-60份的相变材料载体、20-60份的香精、30-90份的单体、0.3-1.0份的引发剂、3-6份的乳化剂和200-600份的水;
(2)芯材组分制备:将上述比例的相变材料载体和香精在30-35℃下,密闭容器内,以800-1200r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的单体和引发剂在30-35℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在30-45℃下搅拌活化,制得水相组分;
(5)原料乳化:在30-45℃的温度下,将所述的油相组分加入到水相组分中,并且以12000-20000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65-80℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
下面通过具体的实施例对本发明做进一步的描述。本发明的温控缓释芳香微胶囊的表面形貌和性能的表征除特别标明的以外,均使用下面的设备:
采用德国蔡司公司ULTRA55热场发射扫描电子显微镜观测、喷金后的温控缓释芳香微胶囊的表面形貌。
采用英国马尔文公司Mastersizer 2000激光粒度分析仪测试温控缓释芳香微胶囊的粒度。
采用美国TA公司Q2000差示扫描量热仪,在氮气保护下,测试10℃/min升温过程和-10℃/min降温过程的DSC扫描曲线,得到温控缓释芳香微胶囊芯材的相变温度。
下面结合具体的实施例对本发明作进一步说明:
实施例1
一种纳米温控缓释芳香微胶囊的制备方法,包括以下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料,40份的硬脂酸丁酯、20份的薰衣草香精、50份的甲基丙烯酸甲酯、10份的丙烯酸正丁酯、0.9份的偶氮二异庚腈、4.8份的十二烷基苯磺酸钠和480份的水;
(2)芯材组分制备:将上述比例的硬脂酸丁酯和香精在32℃下,密闭容器内,以1000r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的甲基丙烯酸甲酯、丙烯酸正丁酯和偶氮二异庚腈在32℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在40℃下搅拌活化,制得水相组分;
(5)原料乳化:在35℃的温度下,将所述油相组分加入到水相组分中,并且以12000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
所得微胶囊粉末用电子显微镜观察,发现微胶囊形貌为光滑的球形,见附图1;用激光粒度仪测量发现,微胶囊的粒径在300nm左右,且分布较为集中,见附图2.
实施例2
一种纳米温控缓释芳香微胶囊的制备方法,包括以下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料,40份的硬脂酸甲酯、20份的玫瑰香精、50份的甲基丙烯酸甲酯、10份的丙烯酸正丁酯、0.9份的偶氮二异庚腈、4.8份的十二烷基苯磺酸钠和480份的水;
(2)芯材组分制备:将上述比例的硬脂酸丁酯和香精在32℃下,密闭容器内,以1000r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的甲基丙烯酸甲酯、丙烯酸正丁酯和偶氮二异庚腈在32℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在40℃下搅拌活化,制得水相组分;
(5)原料乳化:在35℃的温度下,将所述油相组分加入到水相组分中,并且以16000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
实施例3
一种纳米温控缓释芳香微胶囊的制备方法,包括以下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料,30份的硬脂酸甲酯、60份的古龙香精、25份的甲基丙烯酸甲酯、5份的丙烯酸正丁酯、0.9份的偶氮二异庚腈、4.8份的十二烷基苯磺酸钠和480份的水;
(2)芯材组分制备:将上述比例的硬脂酸丁酯和香精在32℃下,密闭容器内,以1000r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的甲基丙烯酸甲酯、丙烯酸正丁酯和偶氮二异庚腈在32℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在40℃下搅拌活化,制得水相组分;
(5)原料乳化:在35℃的温度下,将所述油相组分加入到水相组分中,并且以20000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
实施例4
一种纳米温控缓释芳香微胶囊的制备方法,包括以下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料40份的硬脂酸甲酯、20份的茉莉香精、50份的甲基丙烯酸甲酯、10份的丙烯酸正丁酯、0.9份的偶氮二异庚腈、2.4份的十二烷基苯磺酸钠和240份的水;
(2)芯材组分制备:将上述比例的硬脂酸丁酯和香精在32℃下,密闭容器内,以1000r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的甲基丙烯酸甲酯、丙烯酸正丁酯和偶氮二异庚腈在32℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在40℃下搅拌活化,制得水相组分;
(5)原料乳化:在35℃的温度下,将所述油相组分加入到水相组分中,并且以20000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
实施例5
一种纳米温控缓释芳香微胶囊的制备方法,包括以下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料,30份的硬脂酸甲酯、30份的香草香精、55份的甲基丙烯酸甲酯、5份的丙烯酸正丁酯、0.9份的偶氮二异庚腈、4.8份的十二烷基苯磺酸钠和480份的水;
(2)芯材组分制备:将上述比例的硬脂酸丁酯和香精在32℃下,密闭容器内,以1000r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的甲基丙烯酸甲酯、丙烯酸正丁酯和偶氮二异庚腈在32℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在40℃下搅拌活化,制得水相组分;
(5)原料乳化:在35℃的温度下,将所述油相组分加入到水相组分中,并且以24000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
用差示扫描量热仪测量微胶囊的相转变温度峰值为18℃,对微胶囊粉末香味释放速率进行测试,见附图3,结果显示所制备的微胶囊在相变温度以上香精的释放速率明显加快,说明所加入的载体对香精的缓释具有调控作用。
对所制备的微胶囊在不同温度下的释香持久性进行测试,见附图4,结果表明在15℃时微胶囊的保香能力明显高于25℃和35℃。
应用例1
将织物在实施例5所制备的微胶囊乳液中浸轧一次,60℃烘干,即可制得芳香织物。对所制备的芳香织物留香性进行调查结果如表1所示,结果表明所制备的芳香微胶囊整理在织物上,自然放置半年之后仍然有香精残留。
表1本发明所制备的微胶囊在不同织物上应用的香精残留量
注:以整理后织物上香精的含量为100%做对比。
以上仅为本发明的具体实施例,但本发明的技术特征并不局限于此。任何以本发明为基础,为解决基本相同的技术问题,实现基本相同的技术效果,所作出地简单变化、等同替换或者修饰等,皆涵盖于本发明的保护范围之中。
Claims (8)
1.一种纳米温控缓释芳香微胶囊的制备方法,其特征在于包括如下步骤:
(1)原料准备:所述纳米温控缓释芳香微胶囊包括以下重量分数的原材料:
(2)芯材组分制备:将上述比例的相变材料载体和香精在30-35℃下,密闭容器内,以800-1200r/min搅拌混匀成芯材组分;
(3)油相组分制备:将(2)制备的芯材组分与(1)中的单体和引发剂在30-35℃下,密闭容器内搅拌混匀成油相组分;
(4)水相组分制备:将(1)中所述比例的乳化剂和去离子水在30-45℃下搅拌活化,制得水相组分;
(5)原料乳化:在30-45℃的温度下,将所述的油相组分加入到水相组分中,并且以12000-20000r/min的转速进行搅拌乳化,制得均匀乳液;
(6)单体聚合:将上述的均匀乳液在氮气保护下,在65-80℃下加热5-8小时,引发聚合反应,制得纳米温控缓释芳香微胶囊乳液。
2.根据权利要求1所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述的相变材料载体为脂肪醇、脂肪酸或它们的共熔体。
3.根据权利要求1所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述的单体为甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸叔丁酯、丙烯酸异辛酯、二乙烯基苯、苯乙烯、二甲基丙烯酸乙二醇酯中的一种或者多种。
4.根据权利要求3所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述单体为甲基丙烯酸甲酯和丙烯酸丁酯的共聚物。
5.根据权利要求1所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述乳化剂为离子型乳化剂。
6.根据权利要求5所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述乳化剂为十二烷基苯磺酸钠。
7.根据权利要求1所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述的引发剂为偶氮二异庚腈、偶氮二异丁腈、偶氮二异丁酸二甲酯或过氧化二苯甲酰。
8.根据权利要求7所述的一种纳米温控缓释芳香微胶囊的制备方法,其特征在于:所述的引发剂为偶氮二异庚腈。
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