CN108815017A - 抑菌型sma乳液的制备方法 - Google Patents

抑菌型sma乳液的制备方法 Download PDF

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CN108815017A
CN108815017A CN201811019509.5A CN201811019509A CN108815017A CN 108815017 A CN108815017 A CN 108815017A CN 201811019509 A CN201811019509 A CN 201811019509A CN 108815017 A CN108815017 A CN 108815017A
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sma
lotion
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CN108815017B (zh
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葛瑞娟
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Hainan Sandi Pharmaceutical Co.,Ltd.
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8105—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • A61K8/8117—Homopolymers or copolymers of aromatic olefines, e.g. polystyrene; Compositions of derivatives of such polymers
    • A—HUMAN NECESSITIES
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/524—Preservatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/58—Metal complex; Coordination compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/81—Preparation or application process involves irradiation

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Abstract

本发明公开了一种抑菌型SMA乳液的制备方法，以SMA为聚合物基质，加入AgNO3，借助紫外光还原纳米银，通过SMA酸酐酐环上羰基和银之间的络合作用，从而将具有抑菌性能的纳米银稳定地负载在SMA胶体粒子上，进一步加入油相液体乳化得到抑菌型乳液，该乳液有望用于化妆品中，延长其使用周期。

Description

抑菌型SMA乳液的制备方法
技术领域
本发明属于高分子材料与纳米材料领域，具体涉及一种抑菌型SMA乳液的制备方法。
背景技术
目前的化妆品中一般使用保质期较短，这是因为时间久了，化妆品乳液中会产生一些菌种，导致化妆品乳液变质，用在脸上由于菌种刺激皮肤导致皮肤过敏。
SMA(苯乙烯-马来酸酐共聚物)为一种高分子材料，其本身是结构含有亲水的马来酸酐基元和疏水的苯乙烯基元，可作为高分子表面活性剂、良好的分散剂、相容剂等，其能够在一定的溶剂中形成纳米胶体粒子从而稳定乳状液。
纳米银的典型特性是抗菌性，银的杀菌机制不同于化学合成的抗菌剂，主要是基于重金属离子对细菌蛋白质的变性作用，因而具有广谱杀菌及很少产生耐药菌的特点。在纳米银浓度相同的条件下，作用时间越长，抑菌率越高。纳米银有良好的热稳定性，经高温处理后仍然有良好的抑菌效果。
发明内容
本发明要解决的技术问题是为了克服现有技术中化妆品等乳液时间久了产生菌种的缺陷，提供一种抑菌型SMA乳液的制备方法，该法制得的抑菌型SMA乳液有望作为化妆品乳液的添加剂使用。
本发明是通过下述技术方案来解决上述技术问题：一种抑菌型SMA乳液的制备方法，其特点在于，由以下步骤构成：(1)称取大分子SMA0.5-0.7g，溶于10-15ml的有机溶剂中，剧烈搅拌，同时缓慢滴加水(最好选用超纯水)，当出现蓝色乳光时，将此溶液缓慢滴加于100ml水(最好选用超纯水)中，并剧烈搅拌得到SMA纳米胶体粒子。(2)取上述SMA纳米胶体粒子溶液10ml，滴加0.2mol/L的AgNO3溶液15μL，用锡箔纸包裹避光，在磁力搅拌作用下搅拌3小时，使胶体粒子和硝酸银充分混合，然后置于紫外灯下曝光，制得载银的纳米胶体粒子(nano SMA-Ag)溶液。(3)取步骤(2)得到的载银的纳米胶体粒子溶液3mL，加入3mL油相液体，用高速分散器进行乳化，转速为5000-8000r/min，均质2-3min，得到抑菌型乳液。
所述步骤(1)中的有机溶剂为DMF。所述步骤(2)中紫外灯下曝光时间为5-10min。所述步骤(3)中的油相液体为白油。所述步骤(3)中的高速分散器转速为5000r/min，均质2min。所述SMA的分子量Mn＝100000-150000。
本发明的积极进步效果在于：(1)采用廉价的高分子SMA作为基质，利用酸酐上羰基和Ag之间的络合作用，能够将纳米银稳定地负载在高分子基质载体上；(2)充分利用SMA的表面活性制得纳米胶体粒子，能够稳定乳液；(3)借助紫外光辐照从AgNO3中还原出纳米银，并实现在SMA胶体粒子上的负载，充分利用光能，避免传统还原剂NaBH4的使用，绿色环保，且短时间的紫外辐照不会对SMA造成降解；(4)制得的抑菌型乳液具有抑菌功能，且SMA本身作为良好的分散剂，有望添加到化妆品等乳液中，提高化妆品等乳液的抑菌性，延长使用周期。
附图说明
图1为载银的纳米胶体粒子TEM图。
图2为载银的纳米胶体粒子溶液(nano SMA-Ag)的乳化后数码照片。
图3为抑菌型乳液液滴显微镜结果。
具体实施方式
下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围之中。
实施例1
(1)称取大分子SMA(Mn＝100000)0.5g，溶于10ml的有机溶剂DMF中，剧烈搅拌，同时缓慢滴加超纯水，当出现蓝色乳光时，将此溶液缓慢滴加于100ml超纯水中，并剧烈搅拌得到SMA纳米胶体粒子。(2)取上述SMA纳米胶体粒子溶液10ml，滴加0.2mol/L的AgNO3溶液15μL，用锡箔纸包裹避光，在磁力搅拌作用下搅拌3小时，使胶体粒子和硝酸银充分混合，然后置于紫外灯下曝光5min，制得载银的纳米胶体粒子(nano SMA-Ag)溶液。(3)取步骤(2)得到的载银的纳米胶体粒子溶液3mL，加入3mL白油，用高速分散器进行乳化，转速为5000r/min，均质2min，得到抑菌型乳液。
实施例2
将实施例1中的步骤2制得的载银的纳米胶体粒子(nano SMA-Ag)溶液稀释后，用0.45μm滤膜除尘后，滴一滴至铜网上，室温干燥1天后用TEM观察形貌，结果如图1所示。结果显示，纳米Ag粒径约为8～16nm(由于Ag与SMA胶体粒子存在对比度问题，TEM中SMA胶体粒子不清晰)，从TEM图中看出，纳米Ag能够很好的分散在SMA胶体粒子的表面或周围，这是由于SMA聚合物含有大量羰基能够与纳米Ag络合。
实施例3
实施例1中载银的纳米胶体粒子溶液加入白油乳化后照片如图2所示。可见具有较好的乳化性能，乳液性状也较为稳定。
实施例4
将实施例1制得的抑菌型乳液，取一滴稀释，在光学显微镜下观察形貌，如图3所示，结果表明可形成较为稳定的乳液，乳液滴粒径大约为20μm，粒子分布较为均匀，即乳化性能较优。
实施例5
将实施例1中SMA分子量Mn分别替换成低分子量和高分子量的SMA进行乳液稳定性考察，如表1所示。结果显示，中分子量(Mn＝100000，150000)的SMA的乳液稳定性能更好。
表1载银的SMA纳米胶体粒子的乳化性能参数
虽然以上描述了本发明的具体实施方式，但是本领域的技术人员应当理解，这仅是举例说明，本发明的保护范围是由所附权利要求书限定的。本领域的技术人员在不背离本发明的原理和实质的前提下，可以对这些实施方式做出多种变更或修改，但这些变更和修改均落入本发明的保护范围。

Claims (6)

1.一种抑菌型SMA乳液的制备方法，其特征在于，由以下步骤构成：(1)称取大分子SMA0.5-0.7g，溶于10-15ml的有机溶剂中，剧烈搅拌，同时缓慢滴加水(最好选用超纯水)，当出现蓝色乳光时，将此溶液缓慢滴加于100ml水(最好选用超纯水)中，并剧烈搅拌得到SMA纳米胶体粒子；(2)取上述SMA纳米胶体粒子溶液10ml，滴加0.2mol/L的AgNO3溶液15μL，用锡箔纸包裹避光，在磁力搅拌作用下搅拌3小时，使胶体粒子和硝酸银充分混合，然后置于紫外灯下曝光，制得载银的纳米胶体粒子(nano SMA-Ag)溶液；(3)取步骤(2)得到的载银的纳米胶体粒子溶液3mL，加入3mL油相液体，用高速分散器进行乳化，转速为5000-8000r/min，均质2-3min，得到抑菌型乳液。
2.如权利要求1所述的抑菌型SMA乳液的制备方法，其特征在于，所述步骤(1)中的有机溶剂为DMF。
3.如权利要求1所述的抑菌型SMA乳液的制备方法，其特征在于，所述步骤(2)中紫外灯下曝光时间为5-10min。
4.如权利要求1所述的抑菌型SMA乳液的制备方法，其特征在于，所述步骤(3)中的油相液体为白油。
5.如权利要求1所述的抑菌型SMA乳液的制备方法，其特征在于，所述步骤(3)中的高速分散器转速为5000r/min，均质2min。
6.如权利要求1所述的抑菌型SMA乳液的制备方法，其特征在于，所述SMA的分子量Mn＝100000-150000。
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1622853A (zh) * 2001-12-27 2005-06-01 宝力科莱株式会社 含银纳米粒子的功能性微胶囊的制备方法
CN102532376A (zh) * 2010-12-28 2012-07-04 合肥杰事杰新材料股份有限公司 利用紫外光辐照制备纳米Ag/PVP复合材料的方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1622853A (zh) * 2001-12-27 2005-06-01 宝力科莱株式会社 含银纳米粒子的功能性微胶囊的制备方法
CN102532376A (zh) * 2010-12-28 2012-07-04 合肥杰事杰新材料股份有限公司 利用紫外光辐照制备纳米Ag/PVP复合材料的方法

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