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CN114983841A - Water-in-oil peony sun block without silicone oil and preparation method thereof - Google Patents

Water-in-oil peony sun block without silicone oil and preparation method thereof Download PDF

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CN114983841A
CN114983841A CN202210677575.1A CN202210677575A CN114983841A CN 114983841 A CN114983841 A CN 114983841A CN 202210677575 A CN202210677575 A CN 202210677575A CN 114983841 A CN114983841 A CN 114983841A
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sunscreen
oil
carbonate
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CN114983841B (en
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韩婕珺
罗彩钿
王斌
龚天贵
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Meichulai Hangzhou Cosmetics Co ltd
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    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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Abstract

本发明公开了一种不含硅油的油包水牡丹防晒乳及其制备方法,属于化妆品技术领域;本发明的一种防晒乳包括以下质量份的组分:防晒剂18.02‑23.2份、乳化剂1‑2.2份、增稠剂0.01‑0.45份、成膜剂0.01‑1份、硅石0.1‑2份、溶剂20‑80份、酯烷混合物0.04‑22份,所述酯烷混合物由碳酸二乙基己酯、碳酸二辛酯、C12‑15醇苯甲酸酯和C9‑12烷组成;本发明提供的防晒乳中不含硅油,能够避免硅油对人体皮肤以及对环境的破坏作用;同时本发明提供的防晒乳肤感清爽、极低过敏反应率、能有效抑制油脂分泌、减少经皮水分流失、且具有较高的SPF值;另外,本发明提供的防晒乳制备方法简单,操作简便。The invention discloses a water-in-oil peony sunscreen lotion without silicone oil and a preparation method thereof, belonging to the technical field of cosmetics; a sunscreen lotion of the invention comprises the following components in parts by mass: 18.02-23.2 parts of a sunscreen agent, an emulsifier 1-2.2 parts, thickener 0.01-0.45 parts, film-forming agent 0.01-1 part, silica 0.1-2 parts, solvent 20-80 parts, ester-alkane mixture 0.04-22 parts, the ester-alkane mixture is composed of diethyl carbonate It is composed of hexyl hexyl ester, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane; the sunscreen provided by the invention does not contain silicone oil, which can avoid the destructive effect of silicone oil on human skin and the environment; The sunscreen lotion provided by the invention has refreshing skin feeling, extremely low allergic reaction rate, can effectively inhibit oil secretion, reduce transdermal water loss, and has a high SPF value; in addition, the sunscreen lotion provided by the invention has a simple preparation method and simple operation.

Description

一种不含硅油的油包水牡丹防晒乳及其制备方法A kind of water-in-oil peony sunscreen lotion without silicone oil and preparation method thereof

技术领域technical field

本发明属于化妆品技术领域,尤其涉及一种不含硅油的油包水牡丹防晒乳及其制备方法。The invention belongs to the technical field of cosmetics, and in particular relates to a water-in-oil peony sunscreen lotion without silicone oil and a preparation method thereof.

背景技术Background technique

近年来国内外研究发现,皮肤受到外界环境各种压力受损因素主要有:干燥空气,气温剧烈变化,细菌,病毒,空气污染及光污染以及损伤等,而其中光损伤导致的结果将是皮肤晒伤,色沉和光老化。当皮肤接受紫外线过度暴晒后,会损伤表皮细胞,活化酪胺酸酶,加速色素合成,破坏皮肤的保湿功能,使皮肤变得干燥,让真皮层中的弹力纤维受损,造成细纹产生。在强烈照射下,还会造成肌肤发炎、灼伤,严重者会造成皮肤癌,所以防晒是人体护肤必不可少的一环,其防晒产品的选择也变得尤其重要。In recent years, studies at home and abroad have found that the skin is damaged by various external pressure factors: dry air, drastic changes in temperature, bacteria, viruses, air pollution and light pollution, and damage, among which the result of light damage will be skin sunburn. injury, pigmentation and photoaging. When the skin is exposed to excessive ultraviolet rays, it will damage epidermal cells, activate tyrosinase, accelerate pigment synthesis, destroy the skin's moisturizing function, make the skin dry, damage the elastic fibers in the dermis, and cause fine lines. Under strong irradiation, it will also cause skin inflammation, burns, and even skin cancer in severe cases. Therefore, sunscreen is an indispensable part of human skin care, and the choice of sunscreen products has become particularly important.

防晒产品一般分为水包油防晒和油包水防晒,水包油防晒耐水性较差,不适合长期在户外工作的人群,而油包水防晒的耐水性强,不管是对于室内还是户外都具有高效的防晒作用,但是市面上的油包水防晒为了达到清薄的肤感,大多数都会选择以硅油体系为主,却忽略了硅油本身对其人体也具有一定的危害。硅油属于非极性油脂,具有极强的渗透作用,一些皮肤敏感者在使用硅油体系的防晒产品时会出现皮肤发红发痒的症状,不仅没对皮肤起到保护作用,反而还损伤了皮肤。并且现在提倡环境保护,一些市面上常用的防晒剂对其大自然也有一定的危害作用,据研究表明,每年有大约6-14000 吨防晒剂冲洗并进入珊瑚礁区,数千种防晒产品含有两种最具有威胁性的化学物质,就是甲氧基肉桂酸乙基己酯,二苯甲酮-3,这两种防晒因子,吸收紫外线,使珊瑚礁发生白化反应,其中二苯甲酮-3还会阻止婴儿珊瑚的生长,在实验室测试中对几种不同的珊瑚物种都有毒,导致珊瑚在较低的温度下漂白,并降低它们对气候变化的适应能力。Sunscreen products are generally divided into oil-in-water sunscreens and water-in-oil sunscreens. Oil-in-water sunscreens have poor water resistance and are not suitable for people who work outdoors for a long time, while water-in-oil sunscreens have strong water resistance, both indoors and outdoors. It has a high-efficiency sunscreen effect, but in order to achieve a thin skin feel, most of the water-in-oil sunscreens on the market will choose a silicone oil system, but ignore that the silicone oil itself also has certain harm to the human body. Silicone oil is a non-polar oil and has a strong penetrating effect. Some people with sensitive skin will experience redness and itching when using sunscreen products with silicone oil system, which not only does not protect the skin, but also damages the skin. . And now environmental protection is advocated. Some commonly used sunscreens on the market also have a certain harmful effect on nature. According to research, about 6-14,000 tons of sunscreens are washed and entered into coral reef areas every year. Thousands of sunscreen products contain two types of sunscreens. The most threatening chemicals are ethylhexyl methoxycinnamate and benzophenone-3. These two sunscreen factors absorb ultraviolet rays and cause bleaching of coral reefs. Among them, benzophenone-3 will also Stops the growth of baby corals, which are toxic to several different coral species in laboratory tests, causes corals to bleach at cooler temperatures, and reduces their resilience to climate change.

目前化妆品中尚未发明一种既对人体皮肤友好、又对环境友好的,且美丽修行全绿的不含硅油的油包水牡丹防晒乳这一方向做研究。At present, there is no silicone oil-free water-in-oil peony sunscreen in cosmetics that is friendly to human skin and environment, and is beautiful and full of green.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于克服上述现有技术的不足之处而提供一种不含硅油、对环境友好、对人体皮肤友好的防晒乳及其制备方法。The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art and provide a sunscreen that does not contain silicone oil, is environmentally friendly, and is friendly to human skin and a preparation method thereof.

为实现上述目的,本发明采取的技术方案为:一种不含硅油的油包水牡丹防晒乳,所述防晒乳包括以下质量份的组分:防晒剂18.02-23.2份、乳化剂1-2.2 份、增稠剂0.01-0.45份、成膜剂0.01-1份、硅石0.1-2份、溶剂20-80份、酯烷混合物0.04-22份;所述酯烷混合物由碳酸二乙基己酯、碳酸二辛酯、C12-15 醇苯甲酸酯和C9-12烷组成。In order to achieve the above purpose, the technical scheme adopted in the present invention is: a water-in-oil peony sunscreen lotion without silicone oil, the sunscreen lotion comprises the following components by mass: 18.02-23.2 parts of sunscreen agent, 1-2.2 parts of emulsifier parts, 0.01-0.45 parts of thickener, 0.01-1 part of film-forming agent, 0.1-2 parts of silica, 20-80 parts of solvent, 0.04-22 parts of ester alkane mixture; the ester alkane mixture is composed of diethylhexyl carbonate , dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane composition.

本发明提供的不含硅油的油包水牡丹防晒乳中采用酯烷混合物替代常规的硅油,一方面能够避免硅油对人体皮肤以及对环境的破坏作用,另一方面,通过四者成分的组合使用,能够使得到的防晒剂的效果超越常规使用硅油的效果,其能够取得更低的过敏反应率、更高的油脂分泌抑制率、更少的经皮水分流失。具体的,碳酸二乙基己酯具有极低的粘度、高铺展性并且对晶体活性物质具有良好的增溶性,可以很好的分散防晒剂,使得制备得到的防晒乳肤感清爽;碳酸二辛酯是一种新型的润肤剂,其具有极干爽的肤感和良好的铺展性,其效果可与挥发性硅油相媲美,对防晒剂有良好的溶解性,能够减少制备得到的防晒乳的油腻感;C12-15醇苯甲酸酯对防晒剂的溶解性极佳,从而使得制备得到的防晒乳肤感清爽不粘腻;C9-12烷源自植物原料的高纯度烷烃,属于非极性油脂,其肤感清爽、滑感明显、铺展性极强,有类似硅油的肤感,能够减少防晒乳的油腻感;本发明通过将四种组分组合使用,能够达到单独使用所无法取得的效果。The silicone oil-free water-in-oil peony sunscreen provided by the present invention adopts ester alkane mixture to replace conventional silicone oil, on the one hand, the destructive effect of silicone oil on human skin and the environment can be avoided, and on the other hand, the combination of the four components can be used. , which can make the effect of the obtained sunscreen exceed the effect of conventional use of silicone oil, which can achieve lower allergic reaction rate, higher oil secretion inhibition rate, and less transdermal water loss. Specifically, diethylhexyl carbonate has extremely low viscosity, high spreadability, and good solubilization of crystalline active substances, and can well disperse sunscreen agents, so that the prepared sunscreen lotion feels refreshing on the skin; dioctyl carbonate Ester is a new type of emollient, which has a very dry skin feel and good spreadability, its effect is comparable to that of volatile silicone oil, has good solubility for sunscreen agents, and can reduce the amount of sunscreen prepared. Greasy feeling; C12-15 alcohol benzoate has excellent solubility for sunscreens, so that the prepared sunscreen feels refreshing and non-sticky; C9-12 alkanes are high-purity alkanes derived from plant raw materials, which belong to non-polar It has a refreshing skin feel, obvious slippery feeling, and extremely strong spreadability, and has a skin feel similar to silicone oil, which can reduce the greasy feeling of sunscreen lotion; the present invention can achieve the achievement that cannot be achieved by using the four components in combination. Effect.

作为本发明所述防晒乳的优选实施方式,所述碳酸二乙基己酯、碳酸二辛酯、C12-15醇苯甲酸酯和C9-12烷的质量比为碳酸二乙基己酯:碳酸二辛酯: C12-15醇苯甲酸酯:C9-12烷=(0.01-4):(0.01-6):(0.01-6):(0.01-6)。As a preferred embodiment of the sunscreen lotion of the present invention, the mass ratio of the diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane is diethylhexyl carbonate: Dioctyl carbonate: C12-15 alcohol benzoate: C9-12 alkane=(0.01-4):(0.01-6):(0.01-6):(0.01-6).

作为本发明所述防晒乳的优选实施方式,所述碳酸二乙基己酯、碳酸二辛酯、C12-15醇苯甲酸酯和C9-12烷的质量比为碳酸二乙基己酯:碳酸二辛酯: C12-15醇苯甲酸酯:C9-12烷=(1.8-2.2):(1.8-2.2):(1.8-2.2):(2.6-3.4)。As a preferred embodiment of the sunscreen lotion of the present invention, the mass ratio of the diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane is diethylhexyl carbonate: Dioctyl carbonate: C12-15 alcohol benzoate: C9-12 alkane = (1.8-2.2): (1.8-2.2): (1.8-2.2): (2.6-3.4).

当碳酸二乙基己酯、碳酸二辛酯、C12-15醇苯甲酸酯和C9-12烷的质量比为碳酸二乙基己酯:碳酸二辛酯:C12-15醇苯甲酸酯:C9-12烷=(1.8-2.2): (1.8-2.2):(1.8-2.2):(2.6-3.4)时,得到的防晒乳的肤感清爽度最好,感觉清爽的志愿者的占比达99%。When the mass ratio of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: C12-15 alcohol benzoate : C9-12 alkane=(1.8-2.2): (1.8-2.2): (1.8-2.2): (2.6-3.4), the obtained sunscreen has the best skin feeling, and the percentage of volunteers who feel fresh than 99%.

作为本发明所述防晒乳的优选实施方式,所述防晒乳还包括以下质量份的组分:抗氧化剂0.12-0.6份、皮肤调理剂0.1-1.83份、防腐剂0.1-0.5份、螯合剂0.01-0.05份。As a preferred embodiment of the sunscreen lotion of the present invention, the sunscreen lotion further includes the following components in parts by mass: 0.12-0.6 parts of antioxidants, 0.1-1.83 parts of skin conditioners, 0.1-0.5 parts of preservatives, and 0.01 parts of chelating agents -0.05 servings.

作为本发明所述防晒乳的优选实施方式,所述防晒剂包括植物防晒剂和非植物防晒剂;所述植物防晒剂包括牡丹籽油和牡丹发酵液,所述非植物防晒剂包括二氧化钛、对甲氧基肉桂酸异戊酯、双-乙基己氧苯酚甲氧苯基三嗪、水杨酸乙基己酯、苯基苯并咪唑磺酸中的至少一种。As a preferred embodiment of the sunscreen lotion of the present invention, the sunscreen agents include plant sunscreen agents and non-plant sunscreen agents; the plant sunscreen agents include peony seed oil and peony fermentation broth, and the non-plant sunscreen agents include titanium dioxide, At least one of isoamyl methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyltriazine, ethylhexyl salicylate, and phenylbenzimidazole sulfonic acid.

作为本发明所述防晒乳的优选实施方式,所述植物防晒剂与非植物防晒剂的质量比为(0.02-1.2):(18-22)。As a preferred embodiment of the sunscreen of the present invention, the mass ratio of the plant sunscreen agent to the non-plant sunscreen agent is (0.02-1.2): (18-22).

本发明选择植物防晒剂和非植物防晒剂复配使用,植物防晒剂的存在能够协助非植物防晒剂增加防晒指数;同时本发明选择的防晒剂的种类都是对皮肤友好、温和不刺激、美丽修行全绿、绿色环保的防晒剂。其中二氧化钛为硬脂酸和氢氧化铝处理的,替代常规的硅处理的钛白粉;对甲氧基肉桂酸异戊酯,分子量为192.21,法规限用量为10%,是甲氧基肉桂酸乙基己酯的替代品;双-乙基己氧苯酚甲氧苯基三嗪是一种新型广谱紫外线吸收剂,分子量为 627.8,主要吸收310-343nm波长的紫外线,具有脂溶性及光稳定性,法规限用量为10%;水杨酸乙基己酯,分子量为250.34,属于UVB防晒剂,主要吸收280-340nm波长的紫外线,法规限用量为5%;苯基苯并咪唑磺酸,水溶性UVB防晒剂,分子量为274.3,主要吸收280-320nm波长的紫外线,法规限用量为8%(以酸计)。通过植物防晒剂和不同种类的非植物防晒剂的共同作用,从而能够有效吸附中长波紫外线,达到显著的防晒效果。In the present invention, a plant sunscreen agent and a non-plant sunscreen agent are selected for compound use, and the presence of the plant sunscreen agent can help the non-plant sunscreen agent to increase the SPF; at the same time, the types of sunscreen agents selected in the present invention are all skin-friendly, mild, non-irritating, and beautiful. Practice an all-green, green and environmentally friendly sunscreen. Among them, titanium dioxide is treated with stearic acid and aluminum hydroxide, replacing the conventional silicon-treated titanium dioxide; isoamyl p-methoxycinnamate, with a molecular weight of 192.21, and a legal limit of 10%, is ethyl methoxycinnamate. Substitute for ethylhexyl ester; bis-ethylhexyloxyphenol methoxyphenyltriazine is a new type of broad-spectrum UV absorber with a molecular weight of 627.8, which mainly absorbs ultraviolet rays with a wavelength of 310-343nm, and has lipid solubility and photostability , the legal limit is 10%; ethylhexyl salicylate, with a molecular weight of 250.34, belongs to UVB sunscreens, mainly absorbing ultraviolet rays with a wavelength of 280-340nm, and the legal limit is 5%; phenylbenzimidazole sulfonic acid, water-soluble It is a UVB sunscreen agent with a molecular weight of 274.3, mainly absorbing ultraviolet rays with a wavelength of 280-320 nm, and the regulatory limit is 8% (calculated as acid). Through the joint action of plant sunscreen agents and different types of non-plant sunscreen agents, medium and long-wave ultraviolet rays can be effectively absorbed, and a significant sunscreen effect can be achieved.

作为本发明所述防晒乳的优选实施方式,所述乳化剂包括聚甘油类乳化剂、司盘、吐温、液晶乳化剂中的至少一种;所述增稠剂包括二硬脂二甲铵锂蒙脱石;所述成膜剂包括VP/VA共聚物、丙烯酸(酯)类/丙烯酸乙基己酯共聚物、丙烯酸(酯)类/甲基丙烯酸二甲基氨乙酯共聚物、聚酰胺-8中的至少一种;所述溶剂包括水、乙醇中的至少一种。As a preferred embodiment of the sunscreen lotion of the present invention, the emulsifier includes at least one of polyglycerol emulsifier, Span, Tween, and liquid crystal emulsifier; the thickener includes distearyl dimethylammonium Hectorite; the film-forming agent includes VP/VA copolymer, acrylic acid (ester) type/ethylhexyl acrylate copolymer, acrylic acid (ester) type/dimethylaminoethyl methacrylate copolymer, polymer At least one of amide-8; the solvent includes at least one of water and ethanol.

作为本发明所述防晒乳的优选实施方式,所述乳化剂包括聚甘油-3二异硬脂酸酯和山梨坦异硬脂酸酯;所述增稠剂包括二硬脂二甲铵锂蒙脱石;所述成膜剂包括VP/十六碳烯共聚物;所述溶剂包括水和乙醇。As a preferred embodiment of the sunscreen of the present invention, the emulsifier includes polyglycerol-3 diisostearate and sorbitan isostearate; the thickener includes distearyl dimethylammonium lithium monoxide Destone; the film-forming agent includes VP/hexadecene copolymer; the solvent includes water and ethanol.

作为本发明所述防晒乳的优选实施方式,所述抗氧化剂包括生育酚乙酸酯、肌肽、四氢甲基嘧啶羧酸中的至少一种;所述皮肤调理剂包括精氨酸、表棓儿茶酚棓酸葡糖苷(EGCD)中的至少一种;所述防腐剂包括氯化钠、对羟基苯乙酮中的至少一种;所述螯合剂包括EDTA-2Na、柠檬酸钠、葡萄糖酸钠中的至少一种。As a preferred embodiment of the sunscreen of the present invention, the antioxidant includes at least one of tocopheryl acetate, carnosine, and tetrahydromethylpyrimidine carboxylic acid; the skin conditioning agent includes arginine, epigallium At least one of catechol gallic acid glucoside (EGCD); the preservative includes at least one of sodium chloride, p-hydroxyacetophenone; the chelating agent includes EDTA-2Na, sodium citrate, glucose at least one of sodium.

作为本发明所述防晒乳的优选实施方式,所述抗氧化剂包括生育酚乙酸酯、肌肽和四氢甲基嘧啶羧酸;所述皮肤调理剂包括精氨酸和表棓儿茶酚棓酸葡糖苷;所述防腐剂包括氯化钠和对羟基苯乙酮;所述螯合剂包括葡萄糖酸钠。As a preferred embodiment of the sunscreen of the present invention, the antioxidants include tocopheryl acetate, carnosine and tetrahydromethylpyrimidine carboxylic acid; the skin conditioning agents include arginine and epigallocatecholgallic acid glucoside; the preservatives include sodium chloride and p-hydroxyacetophenone; the chelating agent includes sodium gluconate.

另外,本发明提供了一种所述防晒乳的制备方法,包括以下步骤:In addition, the present invention provides a preparation method of the sunscreen, comprising the following steps:

(1)研磨B相原料至粒度为30-60目后加入预先升温溶解的A相,研磨混合均匀;(1) Grinding the phase B raw materials to a particle size of 30-60 meshes adds the phase A preliminarily heated and dissolved, and grinds and mixes evenly;

(2)往步骤(1)研磨混合均匀后的体系中加入预先搅拌活化成凝胶状态的C相,均质后加入D相,升温搅拌,再少量多次的加入E相水溶液,边加边搅拌,加入完毕后,均质、降温;(2) Add phase C that is pre-stirred and activated to a gel state into the system after grinding and mixing in step (1), add phase D after homogenization, heat up and stir, and then add phase E aqueous solution in small amounts and multiple times, while adding edges Stir, after adding, homogenize and cool down;

(3)往步骤(2)降温后的体系中加入预先溶解的F相和G相,搅拌均匀后再加入H相,均质、过滤,得防晒乳;(3) adding pre-dissolved phase F and phase G to the system after cooling in step (2), stirring evenly and then adding phase H, homogenizing and filtering to obtain sunscreen lotion;

所述A相为对甲氧基肉桂酸异戊酯、双-乙基己氧苯酚甲氧苯基三嗪、水杨酸乙基己酯和苯基苯并咪唑磺酸;所述B相为碳酸二乙基己酯、碳酸二辛酯、C12-15醇苯甲酸酯、C9-12烷生育酚乙酸酯、牡丹籽油、二氧化钛、硅石、聚甘油-3二异硬脂酸酯和山梨坦异硬脂酸酯;所述C相为二硬脂二甲铵锂蒙脱石;所述D相为VP/十六碳烯共聚物;所述E相为水、甘油、丁二醇、氯化钠、对羟基苯乙酮和葡萄糖酸钠;所述F相为水、牡丹发酵液、四氢甲基嘧啶羧酸、表棓儿茶酚棓酸葡糖苷和肌肽;所述G相为精氨酸;所述H相为乙醇。The A phase is isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenyl benzimidazole sulfonic acid; the B phase is Diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, C9-12 alkyl tocopheryl acetate, peony seed oil, titanium dioxide, silica, polyglycerol-3 diisostearate and Sorbitan isostearate; Described C phase is distearyldimethylammonium hectorite; Described D phase is VP/hexadecene copolymer; Described E phase is water, glycerol, butylene glycol , sodium chloride, p-hydroxyacetophenone and sodium gluconate; the F phase is water, peony fermentation broth, tetrahydromethylpyrimidine carboxylic acid, epigallocatecholgallate glucoside and carnosine; the G phase is arginine; the H phase is ethanol.

作为本发明所述制备方法的优选实施方式,所述F相中的水在防晒乳中的质量份为1.8-2.2质量份。As a preferred embodiment of the preparation method of the present invention, the mass part of the water in the F phase in the sunscreen lotion is 1.8-2.2 mass parts.

作为本发明所述制备方法的优选实施方式,所述步骤(1)中升温溶解的A 相的温度为60-70℃,所述步骤(2)中,升温搅拌的温度为70-80℃,降温后的温度为40-45℃。As a preferred embodiment of the preparation method of the present invention, in the step (1), the temperature of the phase A that is heated and dissolved is 60-70°C, and in the step (2), the temperature of the temperature-raising and stirring is 70-80°C, The temperature after cooling is 40-45°C.

作为本发明所述制备方法的优选实施方式,所述步骤(2)中,均质后加入 D相中的均质时间为2-5分钟,均质速度为600-800r/min,均质、降温的均质为中高速均质3-5分钟,其中,均质速度为800-1000r/min;所述步骤(3)中均质时间为0.5-1.5分钟,均质速度为400-600r/min。As a preferred embodiment of the preparation method of the present invention, in the step (2), the homogenization time added to the D phase after homogenization is 2-5 minutes, the homogenization speed is 600-800r/min, the homogenization, The homogenization of cooling is medium and high-speed homogenization for 3-5 minutes, wherein the homogenization speed is 800-1000r/min; in the step (3), the homogenization time is 0.5-1.5 minutes, and the homogenization speed is 400-600r/min min.

作为本发明所述制备方法的优选实施方式,所述步骤(3)中,过滤的滤布的目数为200目。As a preferred embodiment of the preparation method of the present invention, in the step (3), the mesh number of the filter cloth to be filtered is 200 meshes.

与现有技术相比,本发明的有益效果为:Compared with the prior art, the beneficial effects of the present invention are:

第一:本发明提供的防晒乳中不含硅油,能够避免硅油对人体皮肤以及对环境的破坏作用;First: the sunscreen provided by the present invention does not contain silicone oil, which can avoid the destructive effect of silicone oil on human skin and the environment;

第二:本发明提供的防晒乳肤感清爽、极低过敏反应率、能有效抑制油脂分泌、减少经皮水分流失、且具有较高的SPF值;Second: the sunscreen lotion provided by the present invention has a refreshing skin feeling, extremely low allergic reaction rate, can effectively inhibit oil secretion, reduce transepidermal water loss, and has a high SPF value;

第三:本发明提供的防晒乳制备方法简单,操作简便。Third: the preparation method of the sunscreen lotion provided by the present invention is simple and easy to operate.

具体实施方式Detailed ways

为更好的说明本发明的目的、技术方案和优点,下面将结合具体实施例对本发明作进一步说明。In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below with reference to specific embodiments.

实施例1-7Examples 1-7

实施例1-7提供了一种防晒乳,所述防晒乳的组成如表1所示,表1中填写的是组分的质量份,但是整体配方的总质量份是100份,因此表中的余量表示补充配方至100份;其中乳化剂是聚甘油-3二异硬脂酸酯和山梨坦异硬脂酸酯以质量比为2.5:1复配,增稠剂是二硬脂二甲铵锂蒙脱石,成膜剂是VP/十六碳烯共聚物,保湿剂是甘油和丁二醇以质量比为1:1.5复配,螯合剂是葡萄糖酸钠。Embodiment 1-7 provides a kind of sunscreen lotion, the composition of the sunscreen lotion is shown in Table 1, the mass parts of the components are filled in in Table 1, but the total mass parts of the overall formula is 100 parts, so in the table The balance of the formula means supplementing the formula to 100 parts; wherein the emulsifier is polyglycerol-3 diisostearate and sorbitan isostearate in a mass ratio of 2.5:1, and the thickener is distearate diisostearate. Methylammonium hectorite, the film-forming agent is VP/hexadecene copolymer, the humectant is a compound of glycerol and butanediol in a mass ratio of 1:1.5, and the chelating agent is sodium gluconate.

表1:实施例1-7的防晒乳的配方表Table 1: Formulation table of the sunscreen lotions of Examples 1-7

Figure BDA0003692925890000061
Figure BDA0003692925890000061

Figure BDA0003692925890000071
Figure BDA0003692925890000071

其中,实施例1-7的制备方法如下:Wherein, the preparation method of embodiment 1-7 is as follows:

(1)研磨B相原料至粒度为30-60目后加入预先升温至65℃溶解的A相,研磨混合均匀;(1) Grind the B-phase raw materials to a particle size of 30-60 mesh, add the A-phase pre-heated to 65°C to dissolve, and grind and mix evenly;

(2)往步骤(1)研磨混合均匀后的体系中加入预先搅拌活化成凝胶状态的C相,在速度为700r/min下均质3.5分钟后加入D相原料,升温至75℃搅拌,再少量多次的加入E相水溶液,边加边搅拌乳化均匀,加入完毕后,在速度为 900r/min下均质4分钟,搅拌均匀后改为在速度为45r/min下边搅拌边降温至 42℃;(2) adding the C phase that is stirred and activated into a gel state in advance to the system after the grinding and mixing in step (1), homogenizing for 3.5 minutes at a speed of 700 r/min, adding the D phase raw materials, warming up to 75 ℃ and stirring, Add the E-phase aqueous solution in a small amount and several times, and stir to emulsify evenly. After the addition is completed, homogenize for 4 minutes at a speed of 900 r/min. °C;

(3)往步骤(2)降温后的体系中加入预先溶解的F相和G相,搅拌均匀后再加入H相,在速度为500r/min下均质1分钟,各项指标合格后用200目滤布过滤,得防晒乳;(3) Add pre-dissolved phase F and phase G to the system after cooling in step (2), stir evenly and then add phase H, and homogenize for 1 minute at a speed of 500 r/min. After each index is qualified, use 200 Filter with filter cloth to get sunscreen lotion;

所述A相为对甲氧基肉桂酸异戊酯、双-乙基己氧苯酚甲氧苯基三嗪、水杨酸乙基己酯和苯基苯并咪唑磺酸;所述B相为碳酸二乙基己酯、碳酸二辛酯、 C12-15醇苯甲酸酯、C9-12烷、生育酚乙酸酯、牡丹籽油、二氧化钛、硅石、乳化剂;所述C相为增稠剂;所述D相为成膜剂;所述E相为水、甘油、丁二醇、氯化钠、对羟基苯乙酮和葡萄糖酸钠;所述F相为水、牡丹发酵液、四氢甲基嘧啶羧酸、EGCG和肌肽;所述G相为精氨酸;所述H相为乙醇;其中F 相中的水为2质量份。The A phase is isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenyl benzimidazole sulfonic acid; the B phase is Diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, C9-12 alkane, tocopheryl acetate, peony seed oil, titanium dioxide, silica, emulsifier; the C phase is thickening The D phase is a film-forming agent; the E phase is water, glycerol, butanediol, sodium chloride, p-hydroxyacetophenone and sodium gluconate; the F phase is water, peony fermentation broth, four Hydrogen methyl pyrimidine carboxylic acid, EGCG and carnosine; the G phase is arginine; the H phase is ethanol; wherein the water in the F phase is 2 parts by mass.

对比例1-11Comparative Examples 1-11

本发明对比例1-11提供了一种防晒乳,所述防晒乳的组成如表2所示,表 2中填写的是组分的质量份,但是整体配方的总质量份是100份,因此表中的余量表示补充配方至100份;其中除了硅油外,其余组分与实施例1-7中完全一致,制备方法中也与实施例1-7中完全一致,只是将硅油替代相应的酯烷混合物作为 B相中的一部分。Comparative Example 1-11 of the present invention provides a sunscreen lotion, the composition of which is shown in Table 2, and the mass parts of the components are filled in in Table 2, but the total mass parts of the overall formula is 100 parts, so The balance in the table represents the supplementary formula to 100 parts; except for the silicone oil, the other components are completely the same as those in Examples 1-7, and the preparation method is also completely the same as that in Examples 1-7, except that the silicone oil is replaced with the corresponding The ester alkane mixture is part of Phase B.

表2:对比例1-11的防晒乳的配方表Table 2: Formula table of sunscreen lotions of Comparative Examples 1-11

Figure BDA0003692925890000081
Figure BDA0003692925890000081

Figure BDA0003692925890000091
Figure BDA0003692925890000091

效果例1Effect example 1

本发明效果例探究实施例1-7和对比例1-11得到的防晒乳的清爽度;The effect examples of the present invention explore the freshness of the sunscreen lotions obtained in Examples 1-7 and Comparative Examples 1-11;

测试方法:招募不同年龄段的志愿者共200名,用清水清洗双臂,用无屑吸水干纸巾吸干多余水分,并在环境温度20-22℃,湿度为40-60%的条件下静坐5分钟,取测试样品0.5g涂抹在手臂上的相应位置上,评价其肤感感受,计算其相应选择人数的百分比,清爽度百分比=(选择测试样品人数/总人数) *100%;测试结果如表3所示;Test method: recruit a total of 200 volunteers of different ages, wash their arms with clean water, absorb excess water with lint-free absorbent paper towels, and sit quietly at an ambient temperature of 20-22°C and a humidity of 40-60% For 5 minutes, take 0.5g of the test sample and apply it to the corresponding position on the arm, evaluate its skin feel, and calculate the percentage of the corresponding selected number of people. as shown in Table 3;

表3:实施例1-7和对比例1-11得到的防晒乳的清爽度测试表Table 3: The freshness test table of the sunscreen lotions obtained in Examples 1-7 and Comparative Examples 1-11

Figure BDA0003692925890000092
Figure BDA0003692925890000092

Figure BDA0003692925890000101
Figure BDA0003692925890000101

从表3中可以看出,当采用本发明的技术方案得到防晒乳具有优异的清爽度,清爽度百分比在82%以上,甚至可以达到99%,将实施例1-7的结果与对比例1相比,可以发现采用本发明中的酯烷混合物能够有效替代常规硅油的效果,且清爽度百分比相当,甚至更高;从实施例1-4中可以看出,当酯烷混合物中四种成分的质量比不变,但是改变在防晒乳中的质量份时,得到的清爽度也会存在差异;从实施例1、实施例5-6中可以看出,当酯烷混合物的总量一样时,四种成分的质量比发生变化,也会对清爽度百分比带来影响,其中当碳酸二乙基己酯、碳酸二辛酯、C12-15醇苯甲酸酯、C9-12烷的质量比为2:2:2:3时,得到清爽度百分比最优;从实施例1和对比例1-8中可以看出,当减少酯烷混合物中的某一种或某几种组分并相应的用硅油替代时,得到的产品的清爽效果都呈明显下降趋势,下降幅度在17.17-60.61%之间;从实施例1和对比例9中可以看出,当酯烷混合物的总质量份不变时,但是酯烷混合物中成分的配比不在本发明给出的范围内时,得到的产品的清爽度也明显下降;从实施例1和对比例10 中可以看出,当进一步增加酯烷混合物的添加量时,并不会改善产品的清爽度,反而会使得清爽感变差;从实施例1和对比例11中可以看出,当将酯烷混合物中的成分用相似的成分替代时,无法取得相当的相当效果。As can be seen from Table 3, when the technical solution of the present invention is used to obtain a sunscreen lotion with excellent freshness, the percentage of freshness is above 82%, and can even reach 99%. Compare the results of Examples 1-7 with Comparative Example 1 In comparison, it can be found that the ester alkane mixture of the present invention can effectively replace the effect of conventional silicone oil, and the percentage of refreshing degree is equivalent or even higher; it can be seen from Examples 1-4 that when the four components in the ester alkane mixture are used However, when the mass ratio in the sunscreen lotion is changed, the obtained freshness will also be different; it can be seen from Example 1 and Examples 5-6 that when the total amount of the ester alkane mixture is the same , the change of the mass ratio of the four components will also have an impact on the percentage of freshness. When the ratio is 2:2:2:3, the best percentage of freshness is obtained; it can be seen from Example 1 and Comparative Examples 1-8 that when one or several components in the ester alkane mixture are reduced and corresponding When replaced with silicone oil, the refreshing effect of the obtained products showed an obvious downward trend, and the decline range was between 17.17-60.61%; it can be seen from Example 1 and Comparative Example 9 that when the total mass of the ester-alkane mixture was not However, when the ratio of the ingredients in the ester alkane mixture is not within the range given by the present invention, the freshness of the obtained product also decreases significantly; as can be seen from Example 1 and Comparative Example 10, when the ester alkane is further increased When the amount of the mixture is added, it will not improve the refreshing degree of the product, but will make the refreshing feeling worse; it can be seen from Example 1 and Comparative Example 11 that when the ingredients in the ester alkane mixture are replaced with similar ingredients , cannot achieve a comparable effect.

效果例2Effect example 2

本发明效果例采用斑贴实验探究实施例1-7和对比例1-11得到的防晒乳引起人体皮肤不良反应的潜在可能性;The effect example of the present invention adopts a patch test to explore the potential of the sunscreens obtained in Examples 1-7 and Comparative Examples 1-11 to cause adverse reactions to human skin;

1、受试者选择:1. Subject selection:

1)选择18-60岁符合试验要求的志愿者作为受试对象1) Select volunteers aged 18-60 who meet the test requirements as subjects

2)不能选择有下列情况者作为受试者2) Those with the following conditions cannot be selected as subjects

(1)近一周使用抗组胺药或近一个月内使用免疫抑制剂者(1) Those who have used antihistamines in the past week or immunosuppressants in the past month

(2)近两个月内受试部位应用任何抗炎药物者(2) Those who have applied any anti-inflammatory drugs to the test site within the past two months

(3)受试者患有炎症性皮肤病临床未愈者(3) Subjects suffering from inflammatory skin disease clinically unhealed

(4)胰岛素依赖性糖尿病患者(4) Patients with insulin-dependent diabetes mellitus

(5)正在接受治疗的哮喘或其他慢性呼吸系统疾病患者(5) Patients with asthma or other chronic respiratory diseases who are receiving treatment

(6)在近6个月内接受抗癌化疗者(6) Those who received anticancer chemotherapy within the past 6 months

(7)免疫缺陷或自身免疫性疾病患者(7) Patients with immunodeficiency or autoimmune disease

(8)哺乳期或妊娠妇女(8) Lactating or pregnant women

(9)双侧乳房切除及双侧腋下淋巴结切除者(9) Bilateral mastectomy and bilateral axillary lymph node resection

(10)在皮肤待试部位由于瘢痕、色素、萎缩、鲜红斑痣或其他瑕疵而影响试验结果的判定者(10) Judges who affect the test results due to scars, pigments, atrophy, port-wine stains or other blemishes on the skin to be tested

(11)参加其他的临床试验研究者(11) Participate in other clinical trial investigators

(12)体质高度敏感者(12) People with highly sensitive constitution

2、测试方法:2. Test method:

1)按受试者入选标准选择参加试验的人员,至少30名;1) According to the subject selection criteria, select at least 30 people to participate in the trial;

2)选用面积不超过50mm2、深度约1mm的合格斑试器材。将受试物放入斑试器小室内,用量约为0.020g-0.025g(固体或半固体)或0.020mL-0.025mL (液体)。受试物为实施例1-7和对比例1-11制备得到的产品,对照组为空白对照(不置任何物质)。将加有受试物的斑试器用低致敏胶带贴敷于受试者的背部或前臂曲侧,用手掌轻压使之均匀地贴敷于皮肤上,持续24h。2) Select qualified spot test equipment with an area of no more than 50mm 2 and a depth of about 1mm. Put the test substance into the small chamber of the plaque tester, and the dosage is about 0.020g-0.025g (solid or semi-solid) or 0.020mL-0.025mL (liquid). The test substances are the products prepared in Examples 1-7 and Comparative Examples 1-11, and the control group is a blank control (without any substance). The patch tester with the test substance was applied to the subject's back or the curved side of the forearm with hypoallergenic tape, and lightly pressed with the palm of the hand to make it evenly applied to the skin for 24 hours.

3)分别于去除受试物斑试器后30min(待压痕消失后)、24h和48h按表4 标准观察皮肤反应,并记录观察结果。3) 30min (after the indentation disappears), 24h and 48h after removing the test object spot tester, respectively, observe the skin reaction according to the standard in Table 4, and record the observation results.

表4:皮肤封闭型斑贴试验皮肤反应分级标准Table 4: Skin occlusion patch test skin reaction grading standard

Figure BDA0003692925890000111
Figure BDA0003692925890000111

Figure BDA0003692925890000121
Figure BDA0003692925890000121

3、测试结果:3. Test results:

记录斑贴试验结果表5所示;Record patch test results shown in Table 5;

表5:斑贴试验结果表(本次测试总人数为30人)Table 5: Patch test results table (the total number of people in this test is 30)

Figure BDA0003692925890000122
Figure BDA0003692925890000122

从表5中可以看出,采用本发明的技术方案制备得到的防晒乳斑贴试验结果30人都无明显刺激,在对比例中,含有硅油的含量越高,刺激性越强,其中纯硅油体系(对比例1)斑贴试验结果最严重,在0.5h出现了10例1反应等级, 4例2反应等级;从实施例1和对比例10、对比例11的数据中也可以看出,进一步增加酯烷混合物的添加量或者是用其他相似成分替代酯烷混合物中的组分时,都会对产品带来一定的刺激性。As can be seen from Table 5, the sunscreen milk patch test results prepared by the technical solution of the present invention have no obvious irritation for 30 people. In the comparative example, the higher the content of silicone oil, the stronger the irritation, wherein pure silicone oil The patch test results of the system (Comparative Example 1) were the most serious, with 10 cases of 1 reaction grade and 4 cases of 2 reaction grade appearing at 0.5h; Further increasing the addition amount of the ester alkane mixture or replacing the components in the ester alkane mixture with other similar ingredients will bring some irritation to the product.

效果例3Effect example 3

本发明效果例探究实施例1-7和对比例1-11得到的防晒乳的控油能力;通过测量吸油胶带吸收皮脂后的透明度,测得皮肤表面油脂量;具体测试方法:挑选190名油性或混合性肤质志愿者,年龄在20-35岁之间,随机分成19组,每组10人,每组分别涂抹不同的测试样品,其中一组作为空白对照,不涂抹任何产品。志愿者先用碱性皂基洗面奶清洗额头,清水冲洗干净之后用无屑吸水干纸巾吸干额头水分,然后在环境温度20-22℃,湿度为40-60%的条件下静坐 30分钟,不能喝水和饮料,保持轻松且不触碰额头,然后用CK测试仪的油分探头SM815在额头上不同位置测试油脂分泌量,测量3次,取平均值作为初始值,取(2.0±0.1)mg/m3用量的样品用硅胶指套均匀的涂抹在额头指定区域上,待涂抹完静坐,分别测1小时、6小时的皮脂分泌量,同样取不同位置测量3次,取平均值,计算皮肤表面油脂分泌的抑制率,评价其测试结果。CK测试仪油分探头SM815用于检测皮肤油脂含量,测量值越小,说明皮肤油脂含量越低;抑制率=[(使用后-使用前)/使用前]*100%;测试结果如表6所示;The effect example of the present invention explores the oil-controlling ability of the sunscreen lotions obtained in Examples 1-7 and Comparative Examples 1-11; by measuring the transparency of the oil-absorbing tape after absorbing sebum, the amount of oil on the skin surface is measured; specific test method: select 190 oily or Combination skin volunteers, aged 20-35 years old, were randomly divided into 19 groups of 10 people. Each group applied different test samples, and one group was used as a blank control without applying any product. Volunteers first washed their foreheads with alkaline soap-based facial cleanser, rinsed with clean water, and then used lint-free absorbent paper towels to dry their foreheads, and then sat for 30 minutes at an ambient temperature of 20-22°C and a humidity of 40-60%. Can not drink water and beverages, keep it relaxed and do not touch the forehead, and then use the oil probe SM815 of the CK tester to test the oil secretion at different positions on the forehead, measure 3 times, take the average value as the initial value, take (2.0±0.1) The sample with the dosage of mg/m 3 is evenly smeared on the designated area of the forehead with a silicone fingertip. After smearing, sit still, measure the amount of sebum secretion for 1 hour and 6 hours respectively, and also measure 3 times at different positions, take the average value, and calculate The inhibition rate of oil secretion on the skin surface, and the test results were evaluated. CK tester oil probe SM815 is used to detect the skin oil content, the smaller the measurement value, the lower the skin oil content; the inhibition rate=[(after use-before use)/before use]*100%; the test results are shown in Table 6 Show;

表6:控油测试试验结果表Table 6: Test result table of oil control test

Figure BDA0003692925890000131
Figure BDA0003692925890000131

Figure BDA0003692925890000141
Figure BDA0003692925890000141

从表6中可以看出,采用本发明的技术方案得到的防晒乳具有有效的控油效果,在1小时时,对油脂的抑制率在27.84%以上,在6小时时,对油脂的抑制率在24.19%以上,即本发明采用的无硅油体系中酯烷混合物的添加量极少的情况下(实施例4)都能达到与对比例1中硅油体系相当的控油效果;从实施例 1和对比例1中可以看出,当酯烷混合物的添加量与硅油一样时,实施例1得到的产品的控油效果显著优于对比例1产品的控油效果,其中1小时时、6小时时,实施例1对油脂的抑制率相较于对比例1提升幅度分别为13.00%、28.70%,从数据中也可以发现,本发明的控油效果的持久性是要优于硅油体系的。As can be seen from Table 6, the sunscreen obtained by the technical solution of the present invention has an effective oil control effect. At 1 hour, the inhibition rate of oil and fat is above 27.84%, and at 6 hours, the inhibition rate of oil and fat is 24.19% or more, that is, when the addition amount of the ester alkane mixture in the silicone-free oil system adopted by the present invention is extremely small (Example 4), the oil control effect equivalent to that of the silicone oil system in Comparative Example 1 can be achieved; It can be seen from the ratio 1 that when the addition amount of the ester alkane mixture is the same as that of the silicone oil, the oil control effect of the product obtained in Example 1 is significantly better than that of the product in Comparative Example 1. Compared with Comparative Example 1, the inhibition rate of 1 to oil is increased by 13.00% and 28.70% respectively. It can also be found from the data that the durability of the oil control effect of the present invention is better than that of the silicone oil system.

效果例4Effect example 4

本发明效果例探究实施例1-7和对比例1-11得到的防晒乳的皮肤屏障修护效果,通过志愿者在正常情况下连续使用测试产品28天,通过CK仪器探头分析测量皮肤经表水分流失TEWL值,评估该测试样品的皮肤屏障修护功效,具体测试方法:挑选30名志愿者,在温度20-22℃,湿度为40-60%的环境下,用清水洗去手臂上的油脂和灰尘,静坐30分钟,不能喝水和饮料,志愿者放松心情,手臂裸露,避免触碰手臂,在测试样品使用前,用CK测试仪器探头在样品涂抹侧和空白对照侧的测量区域内不同位置测量3次,分别取平均值作为样品涂抹侧和对照侧的初始值,记为D0,然后取相应的测试样品涂抹在指定区域中,需完全覆盖各测量区域,每天早上涂抹一次,连续涂抹28天,在样品涂抹侧和空白对照侧的测量区域内不同位置测量3次,分别取平均值作为样品涂抹侧和对照侧的测量值,记为D28,比较各测试组的经皮水分流失TEWL值,计算其变化率,变化率=[(使用后-使用前)/使用前]*100%;测试结果如表7所示;The effect example of the present invention explores the skin barrier repairing effect of the sunscreen lotions obtained in Examples 1-7 and Comparative Examples 1-11. Volunteers use the test product for 28 days under normal conditions, and the CK instrument probe is used to analyze and measure the skin surface. The TEWL value of water loss is used to evaluate the skin barrier repairing effect of the test sample. The specific test method: select 30 volunteers, and wash off the skin on the arm with water under the environment of temperature 20-22 ℃ and humidity 40-60%. Grease and dust, sit still for 30 minutes, can not drink water and beverages, the volunteers are relaxed, the arms are bare, avoid touching the arms, before the test sample is used, use the CK test instrument probe in the measurement area on the smeared side and the blank control side of the sample Measure 3 times at different positions, take the average value as the initial value of the smeared side and the control side of the sample, denoted as D0, and then take the corresponding test sample and smear it in the designated area. After smearing for 28 days, measure 3 times at different positions in the measurement area on the smeared side of the sample and the blank control side, and take the average value as the measured value on the smeared side and the control side of the sample, denoted as D28, and compare the transepidermal water loss of each test group. TEWL value, calculate its change rate, change rate=[(after use-before use)/before use]*100%; the test results are shown in Table 7;

表7:经皮水分流失测试数据表Table 7: Transdermal Water Loss Test Data Sheet

Figure BDA0003692925890000142
Figure BDA0003692925890000142

Figure BDA0003692925890000151
Figure BDA0003692925890000151

从表7的实验数据可得,采用本发明的技术方案得到的防晒乳能够明显的降低经皮水分流失,而对比例1-8中硅油含量越高,其降低经皮水分流失的效果越差,这充分说明了硅油对于人体皮肤具有一定的刺激性。As can be seen from the experimental data in Table 7, the sunscreen obtained by using the technical solution of the present invention can significantly reduce the transdermal water loss, and the higher the silicone oil content in Comparative Examples 1-8, the worse the effect of reducing the transdermal water loss. , which fully shows that silicone oil is irritating to human skin.

效果例5Effect example 5

本发明效果例探究实施例1-7和对比例1-11得到的防晒乳的SPF值;根据防晒化妆品中紫外线吸收剂和屏蔽剂可以阻挡紫外线的性质,将防晒化妆品涂在特殊胶带上,用不同波长的紫外线照射,测定样品的吸光度值,依据测定值大小直接评价防晒效果;具体测试方法:使用全自动涂布平台和涂布器,在精确厚度的石英片上重复地涂布防晒样品,得到多片重现性良好,涂膜厚度精确的防晒样品涂层。涂膜检测对比厚度为5微米;用紫外可见分光光度计计量涂膜样品吸收曲线,记录290纳米到400纳米之间的吸收值;用HPA美肤灯模拟阳光照射涂膜样品,灯源能量为6.7毫瓦/平方厘米,照射剂量相当于北纬31度夏天正午1小时的太阳光辐照量;照射完之后用紫外可见分光光度计计量样品涂膜吸收曲线,将测得的值代入ISO2443计算公式,计算样品的SPF值和PA 值;测试结果如表8所示;The effect examples of the present invention explore the SPF values of the sunscreen lotions obtained in Examples 1-7 and Comparative Examples 1-11; Irradiate with ultraviolet rays of different wavelengths, measure the absorbance value of the sample, and directly evaluate the sunscreen effect according to the size of the measured value; specific test method: use a fully automatic coating platform and applicator to repeatedly coat the sunscreen sample on a quartz sheet of precise thickness to obtain Multiple sunscreen sample coatings with good reproducibility and accurate film thickness. The contrast thickness of the coating film is 5 microns; the absorption curve of the coating film sample is measured with a UV-visible spectrophotometer, and the absorption value between 290 nm and 400 nm is recorded; the HPA skin beautifying lamp is used to simulate sunlight to illuminate the coating film sample, and the energy of the lamp source is 6.7 mW/square centimeter, the irradiation dose is equivalent to the sunlight irradiation for 1 hour at noon in summer at 31 degrees north latitude; after irradiation, use an ultraviolet-visible spectrophotometer to measure the absorption curve of the sample coating film, and substitute the measured value into the ISO2443 calculation formula , calculate the SPF value and PA value of the sample; the test results are shown in Table 8;

表8:防晒乳的防晒能力测试结果表Table 8: Sunscreen ability test result table of sunscreen lotion

Figure BDA0003692925890000152
Figure BDA0003692925890000152

Figure BDA0003692925890000161
Figure BDA0003692925890000161

从表8中可以发现,采用本发明的技术方案制备得到的防晒乳具有优异的防晒性能,SPF值大于41.6,PA+++。It can be found from Table 8 that the sunscreen lotion prepared by the technical solution of the present invention has excellent sunscreen performance, the SPF value is greater than 41.6, and the PA+++.

最后应当说明的是,以上实施例以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention rather than limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should The technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The water-in-oil peony sun block free of silicone oil is characterized by comprising the following components in parts by mass: 18.02-23.2 parts of sun-screening agent, 1-2.2 parts of emulsifier, 0.01-0.45 part of thickening agent, 0.01-1 part of film-forming agent, 0.1-2 parts of silica, 20-80 parts of solvent and 0.04-22 parts of ester-alkane mixture;
the mixture of ester and alkyl is composed of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkyl.
2. The suncare cream of claim 1, wherein the mass ratio of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, and C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoates: c9-12 ═ c.01-4: (0.01-6): (0.01-6): (0.01-6).
3. The sunscreen according to claim 2 wherein the mass ratio of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoate: c9-12 alkyl ═ 1.8-2.2: (1.8-2.2): (1.8-2.2): (2.6-3.4).
4. The suncare milk of claim 1, further comprising the following components in parts by mass: 0.12 to 0.6 portion of antioxidant, 0.1 to 1.83 portions of skin conditioner, 0.1 to 0.5 portion of preservative and 0.01 to 0.05 portion of chelating agent.
5. The suntan emulsion of claim 1, wherein the sunscreens include plant sunscreens and non-plant sunscreens; the plant sunscreen agent comprises peony seed oil and peony fermentation liquor, and the non-plant sunscreen agent comprises at least one of titanium dioxide, isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenyl benzimidazole sulfonic acid.
6. The suntan lotion of claim 5, wherein the mass ratio of plant sunscreens to non-plant sunscreens is (0.02-1.2): (18-22).
7. The sun-block emulsion according to claim 1, wherein the emulsifier comprises at least one of polyglycerol emulsifier, span, tween, liquid crystal emulsifier; the thickener comprises disteardimonium hectorite; the film forming agent comprises at least one of VP/VA copolymer, acrylic acid (ester)/ethylhexyl acrylate copolymer, acrylic acid (ester)/dimethylaminoethyl methacrylate copolymer and polyamide-8; the solvent comprises at least one of water and ethanol.
8. The suncare milk of claim 4, wherein the antioxidant comprises at least one of tocopherol acetate, carnosine, and tetrahydromethylpyrimidine carboxylic acid; the skin conditioner comprises at least one of arginine, epigallocatechin gallate glucoside; the preservative comprises at least one of sodium chloride and p-hydroxyacetophenone; the chelating agent comprises at least one of EDTA-2Na, sodium citrate and sodium gluconate.
9. A process for the preparation of a sun-screen according to any of claims 1 to 8, comprising the steps of:
(1) grinding the raw material of the phase B until the granularity is 30-60 meshes, adding the phase A which is heated and dissolved in advance, grinding and mixing uniformly;
(2) adding a C phase which is stirred and activated into a gel state in advance into the system which is ground and uniformly mixed in the step (1), adding a D phase after homogenizing, heating and stirring, adding a small amount of E phase aqueous solution for multiple times while stirring, homogenizing and cooling after the addition is finished;
(3) adding the F phase and the G phase which are dissolved in advance into the system cooled in the step (2), uniformly stirring, then adding the H phase, homogenizing and filtering to obtain the sun-block emulsion;
the phase A is isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenylbenzimidazole sulfonic acid; the phase B is diethyl hexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, C9-12 alkyl tocopheryl acetate, peony seed oil, titanium dioxide, silica, polyglycerol-3 diisostearate and sorbitan isostearate; the phase C is disteardimonium hectorite; the phase D is a VP/hexadecene copolymer; the phase E is water, glycerol, butanediol, sodium chloride, p-hydroxyacetophenone and sodium gluconate; the F phase is water, peony fermentation liquor, tetrahydro-methyl pyrimidine carboxylic acid, epigallocatechin gallate glucoside and carnosine; the G phase is arginine; the H phase is ethanol.
10. The method according to claim 9, wherein the temperature of the phase A dissolved by heating in the step (1) is 60 to 70 ℃, the temperature of the phase A dissolved by heating in the step (2) is 70 to 80 ℃, and the temperature after cooling is 40 to 45 ℃.
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