CN111961248A - 面霜用无毒多孔微球及其制备方法 - Google Patents

面霜用无毒多孔微球及其制备方法 Download PDF

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CN111961248A
CN111961248A CN202010648113.8A CN202010648113A CN111961248A CN 111961248 A CN111961248 A CN 111961248A CN 202010648113 A CN202010648113 A CN 202010648113A CN 111961248 A CN111961248 A CN 111961248A
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nontoxic
microspheres
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叶志泉
王金权
王健
钱伟
许钰洁
季晶玲
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Huaiyin Institute of Technology
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Abstract

本发明涉及高分子微球材料制备领域，公开了一种面霜用无毒多孔微球及其制备方法，该多孔微球所用原料及原料重量份数为：分析纯甲基丙烯酸甲酯50‑70份，引发剂偶氮二异丁酸二甲酯4‑5份，交联剂6‑8份，分散剂6‑8份。本发明通过实用偶氮二异丁酸二甲酯为主要引发剂，并通过悬浮聚合法来制备一种粒径稳定在2‑5μm左右的多孔无毒面霜用微球，有效缓解一般化妆产品对皮肤的刺激性和毒害性，提高活性物的稳定性，延长活性物对肌肤的作用时间。以水相为连续相进行悬浮聚合使得温度可控，所得微球分子质量高，交联度及孔结构易控制，且生产过程不会对环境造成污染。

Description

面霜用无毒多孔微球及其制备方法
技术领域
本发明涉及高分子微球材料制备领域，特别涉及一种面霜用无毒多孔微球及其制备方法。
背景技术
现用于面霜的微球产品在制备中多以偶氮二异丁腈和过氧化苯甲酰为引发剂，这两种引发剂都具有一定的毒性。偶氮二异丁腈遇热会分解放出氮气和含-(CH2)2-C-CN基有机腈化物，该有机腈化物对人体有较大的毒害作用，在制备过程中具有一定的安全隐患。而过氧化苯甲酰在高温分解时难以分解完全，所制产品难免会有一定残留，而且由于过氧化苯甲酰低毒，对皮肤和粘膜具有刺激作用。这使得一些面部皮肤敏感的人用了面霜以后，面部不适，出现红疹。
制备微米级大粒径聚合物微球比较有效的方法有悬浮聚合法，种子聚合法和分散聚合法。其中种子聚合法工艺相对复杂，由于种子微球在达到溶胀平衡时的溶胀度是有限的，用一步溶胀法难以达到所需尺寸，必须采用两步到三步才能达到目的。而分散聚合法虽然可一步聚合达到粒径均一的微球。但是由于致孔剂或功能材料一开始就溶解于分解相，无法随着聚合的进行进入微球内，用此法难以制得多孔或包有功能材料的微球。
发明内容
发明目的：针对现有技术中存在的问题，本发明提供一种面霜用无毒多孔微球及其制备方法。其具有原料来源广，易获得，化学稳定性高，粒径均一（稳定在2-5μm左右）,多孔，对活性物负载量高，无毒等特点。
技术方案：本发明提供了一种面霜用无毒多孔微球，所用原料及原料重量份数为：分析纯甲基丙烯酸甲酯50-70份，引发剂偶氮二异丁酸二甲酯4-5份，交联剂6-8份，分散剂6-8份。
优选地，所述交联剂为以下任意一种或其组合：二乙烯基苯、N，N-亚甲基双丙烯酰胺、二甲基丙烯酸乙二醇酯。
优选地，所述分散剂为以下任意一种或其组合：聚乙烯醇、聚乙烯吡咯酮、羧甲基纤维素。
优选地，所述甲基丙烯酸甲酯的纯度为99%。
优选地，所述偶氮二异丁酸二甲酯的纯度为75%。
本发明公开了一种面霜用无毒多孔微球的制备方法，包括以下步骤：S1：按照原料配比称取甲基丙烯酸甲酯、引发剂偶氮二异丁酸二甲酯、致孔剂、交联剂，混合搅拌均匀后得到油相溶液Ａ；S2：将分散剂与水混合搅拌均匀后获得分散剂水溶液B；S3：将所述油相溶液A加入到所述分散剂水溶液B中，均质乳化后得到悬浮液C；S4：将所述悬浮液Ｃ转移至圆底烧瓶中，通入压力为0.08MPa~0.2MPa的氮气后升温至83℃聚合３h，然后再停止搅拌升温至90℃保温３ｈ进行熟化；S5：降至室温后抽滤、洗涤、干燥后得面霜用无毒多孔微球。
优选地，所述S5具体包括以下步骤：S5-1：降至室温后采用减压过滤得到滤饼；S5-2：将所述滤饼分别采用去离子水及无水乙醇洗涤；S5-3：将洗涤后的所述滤饼在60℃真空下干燥20min，得到白色微球；S5-4：将所述白色微球依次用甲苯、丙酮反复搅拌清洗数次（以抽取致孔剂），再用去离子水和无水乙醇洗涤多次，洗去甲苯和丙酮；S5-5：经115℃干燥6小时后得所述面霜用无毒多孔微球。
优选地，所述致孔剂为以下任意一种或其组合：液体石蜡、脂肪酸、脂肪醇中的一种或几种的混合物。
有益效果：本发明通过使用偶氮二异丁酸二甲酯为主要引发剂并通过悬浮聚合法来制备一种粒径稳定在微米尺寸的多孔无毒面霜用微球，该引发剂活性适中，聚合反应容易控制，聚合过程中能使产品转换率提高1%，反应后无残渣，有效降低综合成本，并且所分解产物无毒无害。再通过对反应聚合后聚合物中的致孔剂进行洗涤抽取，制得具有多孔结构的微球。本发明中的多孔微球本身具有较大的比表面积和多孔结构，加入到面霜中之后，能够使得面霜中其他活性物进入到微球孔隙中，使得面霜中的活性物能缓慢释放，减缓面霜对皮肤的刺激性和毒性，大大提高了活性物的稳定性，延长活性物对肌肤的作用时间。
在制备过程中本发明以水相为连续相进行悬浮聚合，体系粘度低，聚合过程中在搅拌和分散剂的作用下使得单体和引发剂以小液滴的形式分散于水中，此时每个小液滴相当于一个本体聚合体系，链转移少，故所得微球分子质量高。当每个小液滴发生聚合反应时，由于各个小液滴外部都是大量的水，故反应热能快速导出，使得体系温度可控，不会出现局部过热的现象。悬浮聚合过程中，又因整个体系是O/W型，单体是疏水性的，致孔剂也是疏水性的，油滴内聚合稳定，使得孔结构易控制且生产过程不会对环境造成污染，再通过对均质机转速的控制使得所制微球粒径稳定在2-5μm。
本发明所用制备方法即为悬浮聚合法，不仅工艺简单，聚合温度容易控制，而且可制备粒径均一的多孔聚合物微球。通过对加入不同粒径微球的面霜进行肤感测试，最终结果表明，当加入粒径在2-5μm的微球时肤感最佳，延伸性相对较好。
附图说明
图1为实施方式1中制备得到的粒径均一且稳定在2-5μm的面霜用无毒多孔微球的SEM图片。
具体实施方式
下面结合具体实施方式对本发明进行详细的介绍。
实施方式1：
本实施方式提了一种面霜用无毒多孔微球，所用原料及原料重量份数为：纯度为99%的分析纯甲基丙烯酸甲酯55份，纯度为75%的引发剂偶氮二异丁酸二甲酯5份，交联剂二乙烯基苯6份，分散剂聚乙烯醇6份。
上述面霜用无毒多孔微球的制备方法如下：
步骤一：制备油相溶液A
先称取甲基丙烯酸甲酯55份，引发剂偶氮二异丁酸二甲酯4份，致孔剂液体石蜡5份，交联剂二乙烯基苯6份混在一起，然后用磁力搅拌器以转速180rpm，搅拌时长3min将它们充分搅拌。待搅拌均匀后得到油相溶液Ａ。
步骤二：制备分散剂水溶液B
称取6份的分散剂聚乙烯醇并与300份水混合，用磁力搅拌器以转速180rpm，搅拌时长2min将它们充分搅拌，待混合均匀后获得分散剂水溶液B。
步骤三：制备悬浮液C
将油相溶液A加入到分散剂水溶液B中，用均质机在转速6500rpm下均质乳化6min，得到悬浮液C。
步骤四：熟化微球
将悬浮液Ｃ转移至带有搅拌器、氮气装置、温度计以及冷凝管的圆底烧瓶中，将圆底烧瓶放入电热恒温水浴锅中，通入0.09MPa的氮气，以转速为150r/min，升温至83℃聚合３h，然后再停止搅拌升温至90℃ 保温３ｈ。
步骤五：降至室温后抽滤、洗涤、干燥后得面霜用无毒多孔微球
降至室温后采用减压过滤得到滤饼，将滤饼分别采用去离子水及无水乙醇洗涤３次，将洗涤后的滤饼放入真空干燥箱中，在 60℃真空下干燥20min得到白色微球，将干燥后的微球依次用甲苯、丙酮反复搅拌清洗数次，以抽取致孔剂，再用去离子水和无水乙醇洗涤多次，洗去甲苯和丙酮。最后经115℃干燥6小时后（确保甲苯、丙酮无残留）得到无毒、多孔、粒径稳定在2-5μm的面霜用微球。
实施方式2：
本实施方式提了一种面霜用无毒多孔微球，所用原料及原料重量份数为：纯度为99%的分析纯甲基丙烯酸甲酯55份，纯度为75%的引发剂偶氮二异丁酸二甲酯5份，交联剂二乙烯基苯7份，分散剂聚乙烯醇6份。
上述面霜用无毒多孔微球的制备方法如下：
步骤一：先称取甲基丙烯酸甲酯55份，引发剂偶氮二异丁酸二甲酯4份，致孔剂脂肪酸5份，交联剂二乙烯基苯7份并混在一起，然后用磁力搅拌器以转速180rpm，搅拌时长3min将它们充分搅拌。待搅拌均匀后得到油相溶液Ａ。
步骤二：与实施方式1完全相同，此处不做赘述。
步骤三：制备悬浮液C
将油相溶液A加入到分散剂水溶液B中，用均质机在转速7500rpm下均质乳化6min，得到悬浮液C。
本实施方式最终得到无毒、多孔、粒径稳定在2-5μm的面霜用微球。
实施方式3：
本实施方式提了一种面霜用无毒多孔微球，所用原料及原料重量份数为：纯度为99%的分析纯甲基丙烯酸甲酯55份，纯度为75%的引发剂偶氮二异丁酸二甲酯5份，交联剂二乙烯基苯8份，分散剂聚乙烯醇6份。
上述面霜用无毒多孔微球的制备方法如下：
步骤一：先称取甲基丙烯酸甲酯55份，引发剂偶氮二异丁酸二甲酯4份，致孔剂脂肪醇6份，交联剂二乙烯基苯8份并混在一起，然后用磁力搅拌器以转速180rpm，搅拌时长3min将它们充分搅拌。待搅拌均匀后得到油相溶液Ａ。
步骤二：与实施方式1完全相同，此处不做赘述。
步骤三：制备悬浮液C
将油相溶液A加入到分散剂水溶液B中，用均质机在转速8500rpm下均质乳化6min，得到悬浮液C。
本实施方式最终得到无毒、多孔、粒径稳定在2-5μm的面霜用微球。
上述实施方式只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所做的等效变换或修饰，都应涵盖在本发明的保护范围之内。

Claims (8)

1.一种面霜用无毒多孔微球，其特征在于，所用原料及原料重量份数为：分析纯甲基丙烯酸甲酯50-70份，引发剂偶氮二异丁酸二甲酯4-5份，交联剂6-8份，分散剂6-8份。
2.根据权利要求1所述的面霜用无毒多孔微球，其特征在于，所述交联剂为以下任意一种或其组合：
二乙烯基苯、N，N-亚甲基双丙烯酰胺、二甲基丙烯酸乙二醇酯。
3.根据权利要求1所述的面霜用无毒多孔微球，其特征在于，所述分散剂为以下任意一种或其组合：
聚乙烯醇、聚乙烯吡咯酮、羧甲基纤维素。
4.根据权利要求1至3中任一项所述的面霜用无毒多孔微球，其特征在于：所述甲基丙烯酸甲酯的纯度为99%。
5.根据权利要求1至3中任一项所述的面霜用无毒多孔微球，其特征在于：所述偶氮二异丁酸二甲酯的纯度为75%。
6.一种面霜用无毒多孔微球的制备方法，其特征在于，包括以下步骤：
S1：按照原料配比称取甲基丙烯酸甲酯、引发剂偶氮二异丁酸二甲酯、致孔剂、交联剂，混合搅拌均匀后得到油相溶液Ａ；
S2：将分散剂与水混合搅拌均匀后获得分散剂水溶液B；
S3：将所述油相溶液A加入到所述分散剂水溶液B中，均质乳化后得到悬浮液C；
S4：将所述悬浮液Ｃ转移至圆底烧瓶中，通入压力为0.08MPa~0.2MPa的氮气后升温至83℃聚合３h，然后再停止搅拌升温至90℃保温３ｈ进行熟化；
S5：降至室温后抽滤、洗涤、干燥后得面霜用无毒多孔微球。
7.根据权利要求6所述的面霜用无毒多孔微球的制备方法，其特征在于，所述S5具体包括以下步骤：
S5-1：降至室温后采用减压过滤得到滤饼；
S5-2：将所述滤饼分别采用去离子水及无水乙醇洗涤；
S5-3：将洗涤后的所述滤饼在60℃真空下干燥20min，得到白色微球；
S5-4：将所述白色微球依次用甲苯、丙酮反复搅拌清洗数次（以抽取致孔剂），再用去离子水和无水乙醇洗涤多次，洗去甲苯和丙酮；
S5-5：经115℃干燥6小时后得所述面霜用无毒多孔微球。
8.根据权利要求6或7所述的面霜用无毒多孔微球，其特征在于，所述致孔剂为以下任意一种或其组合：
液体石蜡、脂肪酸、脂肪醇中的一种或几种的混合物。
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