WO2023056732A1 - 一种治疗皮肤真菌的产品及其微粉化制备方法 - Google Patents
一种治疗皮肤真菌的产品及其微粉化制备方法 Download PDFInfo
- Publication number
- WO2023056732A1 WO2023056732A1 PCT/CN2022/082857 CN2022082857W WO2023056732A1 WO 2023056732 A1 WO2023056732 A1 WO 2023056732A1 CN 2022082857 W CN2022082857 W CN 2022082857W WO 2023056732 A1 WO2023056732 A1 WO 2023056732A1
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- WIPO (PCT)
- Prior art keywords
- selenium disulfide
- ultrafine powder
- disulfide
- selenium
- water
- Prior art date
Links
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Classifications
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- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/145—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic compounds
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- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1611—Inorganic compounds
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Definitions
- the invention provides a stable selenium disulfide lotion composition for treating skin fungus and a micronization preparation method thereof.
- the product is used as an external lotion for removing dandruff and hair care, and is used in the field of medicine or cosmetics.
- Selenium disulfide has anti-fungal and anti-seborrhea effects. It is often used as 1% or 2.5% selenium disulfide external lotion for anti-dandruff, anti-fungal, anti-scalp seborrheic dermatitis, etc.
- CN105326672A and CN105456287A disclose selenium disulfide ultrafine powders with a particle size of 1-50 ⁇ m and their preparation and application in lotion products.
- the particle size of selenium disulfide in the agent is too large (such as greater than 50 ⁇ m), the selenium disulfide lotion is easily delaminated and other unstable phenomena, or the particle size of selenium disulfide is too small (such as less than 1 ⁇ m) increases the probability of passing through the skin barrier, resulting in Risk of skin toxic side effects of selenium disulfide lotion.
- the glycerin content exceeds 40% in the selenium disulfide ultrafine powder that aforementioned patent technology makes, contains a large amount of glycerin influences or limits the selenium disulfide ultrafine powder and
- the matrix is formulated into lotion products, for example, it is difficult to formulate with a water-in-oil emulsion matrix into a uniformly dispersed and stable selenium disulfide lotion; in addition, the prepared selenium disulfide ultrafine powder has a large particle range, and the D90 exceeds 30 ⁇ m , the uniformity of the particle distribution is not good enough, which is unfavorable to the stability of the selenium disulfide lotion product, making it difficult for the content of selenium disulfide in the lotion to reach 2% or more, otherwise the lotion product is prone to delamination and other unstable phenomena.
- selenium disulfide itself is insoluble in the lotion matrix
- the dispersion uniformity and suspension stability of selenium disulfide in the lotion matrix directly affect the product quality of the selenium disulfide lotion.
- Selenium disulfide lotion products need to be further improved in terms of dispersion uniformity, suspension stability and use safety, so as to improve the safety, effectiveness and compliance of product use.
- the present invention provides a new ultrafine powder of selenium disulfide with a particle size in the range of 1-50 ⁇ m and its application in lotion products. Compared with the prior art, it not only greatly reduces the glycerol content in the selenium disulfide ultrafine powder, but also has a smaller range of product particles and better distribution uniformity, which is conducive to the preparation of selenium disulfide lotion products, and is conducive to improving The quality and application safety and effectiveness of selenium disulfide lotion products.
- the present invention provides a kind of selenium disulfide ultrafine powder, the particle diameter of described selenium disulfide ultrafine powder is (1.0 ⁇ 50.0) ⁇ m, it is characterized in that described selenium disulfide ultrafine powder has D90 of (1.0 ⁇ 15.0) ⁇ m particle size distribution.
- the above-mentioned ultrafine powder of selenium disulfide is prepared by grinding and pulverizing selenium disulfide, glycerin, bentonite, titanium dioxide and water evenly.
- the above-mentioned selenium disulfide superfine powder is made of selenium disulfide, glycerol, bentonite, titanium dioxide and water at 1.0: 1.0: 1.4: The mass ratio of 2.0: 4.6 is prepared by grinding and pulverizing after mixing evenly.
- the pH thereof is adjusted to 3.0-5.0.
- the above-mentioned ultrafine powder of selenium disulfide is characterized in that the D90 of the ultrafine powder of selenium disulfide is (1.0-7.0) ⁇ m.
- a stable selenium disulfide lotion composition which includes selenium disulfide as an active ingredient, and pharmaceutical, daily chemical or food adjuvants and water, characterized in that, The mass percentage of selenium disulfide in the composition is (0.1-3.0)%, and the selenium disulfide is the ultrafine powder of selenium disulfide described above.
- the mass percentage of selenium disulfide is (1.0 ⁇ 3.0)%; for example, when used as a medicine, the disulfide The mass percentage content of selenium disulfide in the selenium sulfide lotion composition is 2.5%.
- the mass percentage of selenium disulfide is (0.1-1.0)%.
- the above-mentioned stable selenium disulfide lotion composition of the present invention wherein said adjuvant is selected from conditioning agent, moisturizing agent, surfactant, buffering agent, chelating agent, preservative, essence, one or one in water more than one species.
- said adjuvant is selected from conditioning agent, moisturizing agent, surfactant, buffering agent, chelating agent, preservative, essence, one or one in water more than one species.
- the stable selenium disulfide lotion composition described above wherein:
- the conditioner is selected from the group consisting of lanolin or its derivatives, stearyl alcohol or its derivatives, cetyl alcohol or its derivatives, dimethylsiloxane, amino-modified silicone oil, emulsified silicone oil, cationic guar gum or polyquaternary Ammonium salts.
- humectant is selected from glycerin, propylene glycol, petrolatum, polyethylene glycol or sorbitol.
- the surfactant is selected from chitosan, lauryl dimethoxyamine, sodium lauryl sulfate, sodium lauryl sarcosinate, lauryl monoethanolamine sulfate, sodium lauryl glutamate, Glyceryl Monostearate, Glyceryl Monoricinoleate, Coco Glycinate, Sodium Methyl Cocoyl Taurate, Sodium Cocoamidopropionate, Lauryl Diethanolamide, Lauryl Diethanolamide Methyl Betaine, Sodium Lauryl Ether Sulfate, Lauryl Betaine, N,N-Oleoyl Methyl Sulfonate, Alkanolamide, Lauryl Dimethyl Acetate, Ethylene Glycol Monostearate, Ethylene Glycol Distearate, Fatty Alcohol Polyoxyethylene Ether Sulfate, N-N Sodium Oleoyl Methyl Taurate.
- the buffering agent is a salt and/or a pH adjusting agent, for example selected from sodium chloride, sodium monophosphate, sodium metaphosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, citric acid, formic acid, tartaric acid or sodium hydroxide.
- a pH adjusting agent for example selected from sodium chloride, sodium monophosphate, sodium metaphosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, citric acid, formic acid, tartaric acid or sodium hydroxide.
- the chelating agent is selected from disodium edetate and tetrasodium edetate.
- the preservative is selected from sodium benzoate, potassium sorbate, sodium dehydroacetate, methylparaben, ethylparaben, propylparaben, butylparaben, methylisothiazolinone, phenoxyethanol propionic acid Calcium, Sodium Diacetate, Sodium Lactate.
- the essence can be the essence commonly used in the field of food, medicine or daily chemical products.
- the amount of the auxiliary materials contained therein is not particularly limited, and can be in accordance with the conventional amount of various auxiliary materials in medicinal lotions or cosmetic lotions in the art.
- the above-mentioned composition is composed of the following raw and auxiliary materials in terms of mass percentage: 0.1% ⁇ 3.0% selenium disulfide ultrafine powder and moisturizing agent in terms of selenium disulfide 1.0% ⁇ 10.0%, surfactant 1.0% ⁇ 30.0%, conditioner 0 ⁇ 5.0%, chelating agent 0 ⁇ 3.0%, preservative 0 ⁇ 3.0%, essence 0 ⁇ 1.0%, and water balance.
- the amount of the buffering agent is to adjust the appropriate pH value of the composition, and the preferred pH value of the composition of the present invention is between 3.0-5.0.
- a method for preparing the above-mentioned stable selenium disulfide lotion composition comprising the following steps: (1) preparing the ultrafine powder of selenium disulfide; (2) Preparing the auxiliary material matrix; (3) adding the selenium disulfide ultrafine powder obtained in the step (1) to the auxiliary material matrix obtained in the step (2) and mixing.
- step (1) the selenium disulfide ultrafine powder is prepared in step (1), and the selenium disulfide, glycerin, bentonite, titanium dioxide and water are mixed and then ground and pulverized to obtain a particle size of ( 1.0 ⁇ 50.0) ⁇ m, D90 is (1.0 ⁇ 15.0) ⁇ m selenium disulfide ultrafine powder.
- the ultrafine powder of selenium disulfide having a D90 of (1.0-7.0) ⁇ m is obtained.
- the milling and pulverizing can be a conventional milling and pulverizing method in the art, for example, milling and pulverizing in a mill-type ultrafine pulverizer, or pulverizing in a ball mill.
- the auxiliary material matrix can be water-in-oil type (W/O type) or oil-in-water type (O/W) according to the needs of selenium disulfide lotion products
- W/O type water-in-oil type
- O/W oil-in-water type
- the particle size measurement of the selenium disulfide ultrafine powder of the present invention is carried out by the conventional particle size measurement method in this area.
- the particle size is determined using a Baxter or Malvern particle sizer.
- the present invention surprisingly obtains that the grinding material liquid mixed with selenium disulfide, titanium dioxide, bentonite, glycerin and water in a specific ratio has a particle size of (1.0-50.0) ⁇ m and a D90 under the conventional milling process.
- selenium disulfide ultrafine powder with a particle size distribution of (1.0 ⁇ 15.0) ⁇ m
- the prepared selenium disulfide ultrafine powder not only overcomes the problem of high glycerin content in the selenium disulfide ultrafine powder of the prior art Defects, and the range of selenium disulfide ultrafine powder particles is smaller, and the distribution uniformity is better, which is conducive to the preparation of selenium disulfide lotion products and the improvement of the quality of selenium disulfide lotion products.
- Fig. 1 Selenium disulfide superfine powder particle size distribution measurement figure that embodiment 1 makes
- Fig. 2 Selenium disulfide superfine powder particle size distribution measurement figure that embodiment 2 makes
- Fig. 3 According to CN105456287A method, the selenium disulfide ultrafine powder particle size distribution measurement figure
- Embodiment 1 the preparation of selenium disulfide ultrafine powder
- Embodiment 2 the preparation of selenium disulfide ultrafine powder
- the materials are fed as ball mills according to the following composition and proportion (parts by weight): 1.0 parts of selenium disulfide dry powder, 1.0 parts of pharmaceutical grade glycerin, 1.4 parts of pharmaceutical grade bentonite, and 2.0 parts of pharmaceutical grade titanium dioxide and 4.6 parts of deionized water, and adjust the pH value of the ball mill in the range of 3.0-5.0 with citric acid and sodium dihydrogen phosphate.
- Embodiment 3 selenium sulfide lotion
- 1.0% selenium disulfide anti-dandruff hair care lotion is made of the following raw materials by mass percentage: 10.0% of the selenium disulfide ultrafine powder made in Example 1 (calculated as 1.0% by selenium disulfide), wool Lipid 1.0%, cetyl alcohol 2.0%, stearyl alcohol 2.0%, petrolatum 1.5%, chitosan 0.3%, 10% (mass) formic acid 0.7%, lauryl dimethoxyamine (OB-2) 2.0%, water-soluble essence 0.2%, deionized water balance.
- OB-2 lauryl dimethoxyamine
- Embodiment 4 selenium sulfide lotion
- selenium disulfide anti-dandruff hair care lotion is made of the following raw materials by mass percentage: the selenium disulfide ultrafine powder 25.0% (calculated as 2.5% with selenium disulfide) that embodiment 2 makes, ten Octyl alcohol 2.0%, glycerin 5.0%, sodium lauryl ether sulfate 5.0%, alkanolamide 4.5%, N-oleoyl-N-methylsulfuric acid sodium 2.3%, lauryl dimethyl betaine 2.3 %, sodium lauryl sulfate 5.5%, glyceryl monostearate 1.0%, lanolin 0.2%, essence 0.2%, the balance of deionized water, adjust the pH value with citric acid and sodium dihydrogen phosphate to 3.5- 4.5.
- the selenium disulfide lotion that embodiment 3 and embodiment 4 make has uniform dispersibility, and through the accelerated stability investigation test of 6 months, the result stability is good; During the investigation period of placing 24 months at normal temperature, the product has no See stratification, and the particles are evenly dispersed.
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Abstract
一种二硫化硒超微粉体及其微粉化制备方法，所述二硫化硒超微粉体的粒径为1.0-50.0μm，是由二硫化硒、甘油、皂土、二氧化钛和水按1.0:1.0:1.4:2.0:4.6的质量比例混合均匀后碾磨粉碎制得，并具有D90为1.0-15.0μm的粒径分布。所述二硫化硒超微粉有利于二硫化硒产品配制和提高二硫化硒洗剂产品的品质。
Description
本发明提供一种用于治疗皮肤真菌的稳定的二硫化硒洗剂组合物及其微粉化制备方法，产品用作祛屑护发的外用洗剂，用于药品或化妆品领域。
二硫化硒，具抗真菌、抗皮脂溢出作用，常以1%或2.5%二硫化硒外用洗剂，用于祛屑、 抗真菌、抗头皮脂溢性皮炎等。
二硫化硒由于在水或有机溶剂中几乎不溶，影响了洗剂等产品的开发或应用。微粉化新技术的发展和应用，提高了二硫化硒洗剂产品开发。CN105326672A、CN105456287A公开了粒径1-50 μm的二硫化硒超微粉体及其制备以及在洗剂产品中应用，与已有二硫化硒洗剂产品相比，克服了传统的二硫化硒洗剂中二硫化硒粒径过大（如大于50 μm）造成二硫化硒洗剂容易分层等不稳定现象，或者二硫化硒粒径太小（如小于1μm）增加了通过皮肤屏障概率，造成二硫化硒洗剂对皮肤毒副作用的风险。然而，为使二硫化硒超微粉体分散均匀，前述专利技术制得的二硫化硒超微粉体中甘油含量超过40%，含有大量的甘油影响或限制了二硫化硒超微粉体与基质配制成洗剂产品，例如难以与油包水型乳液基质配制成为分散均匀的稳定的二硫化硒洗剂；另外，所制得的二硫化硒超微粉体微粒范围较大，D90超过30μm，微粒分布均匀性不够好，对二硫化硒洗剂产品稳定性不利，使得二硫化硒在洗剂中的含量很难达到2%或以上，否则洗剂产品容易出现分层等不稳定现象。
由于二硫化硒本身在洗剂基质不溶解，二硫化硒在洗剂基质中的分散均匀性和悬浮稳定性直接影响了二硫化硒洗剂的产品质量。二硫化硒洗剂产品在分散均匀性、悬浮稳定性以及使用安全性方面还需要进一步改善，以提高产品使用的安全性、有效性和顺应性。
为克服上述的现有技术缺陷，本发明提供了一种粒径在1-50 μm范围内的新的二硫化硒超微粉体及其在洗剂产品中应用。与现有技术相比，其不仅大大降低了二硫化硒超微粉体中甘油含量，而且产品微粒范围更小，分布均匀性更好，有利于配制二硫化硒洗剂产品，并且有利于提高二硫化硒洗剂产品的品质和应用的安全性和有效性。
本发明技术方案如下：
本发明提供了一种二硫化硒超微粉体，所述二硫化硒超微粉体的粒径为(1.0~50.0)μm，其特征在于所述的二硫化硒超微粉体具有D90为(1.0~15.0)μm的粒径分布。
上述所述的二硫化硒超微粉体，是由二硫化硒、甘油、皂土、二氧化钛和水混合均匀后经碾磨粉碎而制得。
优选地，上述所述的二硫化硒超微粉体，是由二硫化硒、甘油、皂土、二氧化钛和水按1.0: 1.0: 1.4 :
2.0: 4.6的质量比例混合均匀后经碾磨粉碎而制得。
优选地，上述所述的二硫化硒超微粉体，二硫化硒、甘油、皂土、二氧化钛和水混合均匀后，调节其pH值为3.0-5.0。
优选地，上述所述的二硫化硒超微粉体，其特征在于所述的二硫化硒超微粉体的D90为(1.0~7.0)μm。
作为本发明另一目的，还提供一种稳定的二硫化硒洗剂组合物，其包含作为有效成分的二硫化硒，以及药用、日化用或食品用的辅料和水，其特征在于，所述组合物中二硫化硒质量百分含量为(0.1~3.0)%，并且所述二硫化硒是使用上述所述的二硫化硒超微粉体。
优选地，上述所述的稳定的二硫化硒洗剂组合物，用作药品时，其中二硫化硒质量百分含量为(1.0~3.0)%；例如，用作药品时，其中所述的二硫化硒洗剂组合物中二硫化硒质量百分含量为2.5%。
优选地，上述所述的稳定的二硫化硒洗剂组合物，用作化妆品时，其中二硫化硒质量百分含量为(0.1~1.0)%。
本发明上述所述的稳定的二硫化硒洗剂组合物，其中所述的辅料选自调理剂、保湿剂、表面活性剂、缓冲剂、螯合剂、防腐剂、香精、水中的一种或一种以上。
优选地，上述所述的稳定的二硫化硒洗剂组合物，其中：
所述调理剂选自羊毛脂或其衍生物、十八醇或衍生物、十六醇或其衍生物、二甲基硅氧烷、氨基改性硅油、乳化硅油、阳离子瓜尔胶或聚季铵盐类。
所述的保湿剂选自甘油、丙二醇、凡士林、聚乙二醇或山梨醇。
所述表面活性剂选自脱乙酰壳聚糖、十二烷基二甲氧化胺、十二烷基硫酸钠、月桂酰肌氨酸钠、月桂醇单乙醇胺硫酸盐、月桂酰谷氨酸钠、单硬脂酸甘油酯、甘油单蓖麻油酸酯、椰子酸甘氨酸酯、甲基椰油酰基牛磺酸钠、椰油酰胺基丙酸钠、月桂二乙醇酰胺、十二-十四烷基二甲基甜菜碱、十二烷基醚硫酸钠、十二烷基甜菜碱、N,N-油酰甲基硫磺酸盐、烷醇酰胺、十二烷基二甲基乙酸酯、乙二醇单硬脂酸酯、乙二醇双硬脂酸酯、脂肪醇聚氧乙烯醚硫酸酯、N-N油酰甲基牛磺酸钠。
所述缓冲剂是盐类和/或pH调节剂，例如选自氯化钠、单磷酸钠、偏磷酸钠、磷酸氢二钠、磷酸二氢钠、柠檬酸、甲酸、酒石酸或氢氧化钠。
所述螯合剂选自乙二胺四乙酸二钠、乙二胺四乙酸四钠。
所述防腐剂选自苯甲酸钠、山梨酸钾、脱氢乙酸钠、 羟苯甲酯，羟苯乙酯，羟苯丙酯，羟苯丁酯、甲基异噻唑啉酮，苯氧乙醇丙酸钙、双乙酸钠、乳酸钠。
所述香精可以是食品、药品或日化品领域中常用的香精。
本发明上述所述的稳定的二硫化硒洗剂组合物，其中所含的辅料的用量，没有特别限制，可以按照本领域中药用洗剂或化妆品用洗剂中各种辅料的常规用量。
作为本发明一个优选实施方案，上述所述的组合物，按质量百分比计是由下述原辅料组成的：以二硫化硒计为0.1%~3.0%的二硫化硒超微粉体、保湿剂1.0%~10.0%、表面活性剂1.0%~30.0%、调理剂0~5.0%、螯合剂0~3.0%、防腐剂0~3.0%、香精0~1.0%，以及水余量。缓冲剂的用量是调节组合物合适的pH值，本发明组合物优选pH值在3.0-5.0之间。
作为本发明另一目的，还提供一种制备上述所述的稳定的二硫化硒洗剂组合物的方法，包括如下步骤：（1）制备所述的二硫化硒超微粉体；（2）制备辅料基质；（3）将步骤（1）得到的二硫化硒超微粉体加到步骤（2）得到的辅料基质中混匀。
上述所述的方法，其中步骤（1）中制备所述的二硫化硒超微粉体，将二硫化硒、甘油、皂土、二氧化钛和水混匀后进行碾磨粉碎，得到粒径为(1.0~50.0)μm、D90为(1.0~15.0)μm的二硫化硒超微粉体。优选的，得到D90为(1.0~7.0)μm的二硫化硒超微粉体。
所述碾磨粉碎，可以是本领域的常规碾磨粉碎方式，例如置于碾磨式超微粉碎机内进行碾磨粉碎，或者是置于球磨机进行碾磨粉碎。
上述所述的方法，其中步骤（2）制备辅料基质，可以根据二硫化硒洗剂产品的需要，辅料基质为油包水型（W/O型）基质或者水包油型（O/W）基质，按本领域常规的乳液制备制得辅料基质。
本发明的二硫化硒超微粉体粒度测定，按本领域常规的粒度测定方法进行。例如，采用了百特粒度测定仪或马尔文粒度测定仪测定粒度。
本发明令人意外地获得，二硫化硒、钛白粉、皂土、甘油和水按特定比例混合的研磨料液在常规碾磨粉碎工艺下获得了粒径为(1.0~50.0)μm并且具有D90为(1.0~15.0)μm的粒径分布的二硫化硒超微粉体，所制得的二硫化硒超微粉体，不仅克服现有技术的二硫化硒超微粉体中甘油含量高的缺陷，而且二硫化硒超微粉体微粒范围更小，分布均匀性更好，有利于二硫化硒洗剂产品配制和提高二硫化硒洗剂产品的品质等。
图1：实施例1制得的二硫化硒超微粉体粒度分布测定图
图2：实施例2制得的二硫化硒超微粉体粒度分布测定图
图3：按照CN105456287A方法制得的二硫化硒超微粉体粒度分布测定图
以下实施例仅作为举例以解释或说明本发明内容，其不构成对本发明权利保护范围的限制或约束。
实施例 1 ：二硫化硒超微粉体制备
将二硫化硒干粉、医药级甘油、医药级皂土、医药级钛白粉和去离子水按质量比1：1：1.4：2.0：4.6混合均匀，加入枸橼酸调节pH值在3.5-4.5之间，然后置于碾磨式超微粉碎机内，设定工作功率1500W，转速1500r/min进行碾磨粉碎30min，将碾磨后料液过筛，收集料液，得到二硫化硒超微粉体，用Bettersize2000N激光粒度分布仪进行粒度测定，所制得的二硫化硒微粉体的D90为2.818μm，结果如图1所示。
实施例 2 ：二硫化硒超微粉体制备
球磨机清洗后，确认运转状况完好，按如下组成和比例（重量份）作为球磨料进行投料：二硫化硒干粉1.0份、医药级甘油1.0份、医药级皂土1.4份、医药级钛白粉2.0份和去离子水4.6份，用枸橼酸和磷酸二氢钠调节球磨料pH值在3.0-5.0范围。先开启球磨机慢速，再开启快速搅拌混匀后开启隔膜泵打循环球磨3-5小时，将研磨后料液通过过滤网，并收集料液，得到二硫化硒超微粉体，BT-2003
型激光粒度分布仪进行粒度测定，所制得的二硫化硒微粉体的D90为2.566μm，结果如图2所示。
对比例：按照CN105456287A方法制备二硫化硒超微粉体
将二硫化硒干粉、去离子水、医药级钛白粉和医药级甘油按质量比1：1：2：3混合均匀，加入枸橼酸调节pH值在3.5-4.5之间，然后然后置于碾磨式超微粉碎机内，设定工作功率1500W，转速1500r/min进行碾磨粉碎30min，将碾磨后料液过筛，收集料液，得到二硫化硒超微粉体，BT-2003
型激光粒度分布仪进行粒度测定，所制得的二硫化硒微粉体的D90为37.19μm，结果如图3所示。
分层稳定性考察
取实施例1、实施例2和对比例各自所制得的二硫化硒超微粉体，进行分层稳定性考察。
方法：在恒温48℃培养箱中放置，判定标准为液固分离的为分层的判定标准。进行目测微粉与分散剂（料液）处于状态（混合状态不分层、分层）。结果如表1所示。
表1 二硫化硒超微粉体分层稳定性考察（粉液状态）
实施例 3 ：二硫化硒洗剂
1.0%二硫化硒祛屑护发洗剂，按质量百分比是由下述原料制成：实施例1制得的二硫化硒超微粉体10.0%（以二硫化硒计为1.0%），羊毛脂1.0%，十六醇2.0%，十八醇2.0%，凡士林1.5%，脱乙酰壳聚糖0.3%，10%（质量）甲酸0.7%，十二烷基二甲氧化胺（OB-2）2.0%，水溶性香精0.2%，去离子水余量。
制备：
将羊毛脂、十六醇、十八醇、凡士林混合，加热至90-100℃，保温15-20分钟，冷却至60-70℃，得到油相，备用；
将脱乙酰壳聚糖、10%甲酸、十二烷基二甲氧化胺、香精和去离子水混合，加热至90-100℃，保温15-20分钟，冷却至60-70℃，得到水相，备用；
将水相置于均质反应罐，开启刮板搅拌器，转速设定为10-60r/min，然后将油相缓慢加入水相中，继续搅拌5min后，关闭搅拌器，开启均质开关，设定真空度为负0.09Mpa，转速为2800r/min，进行均质乳化30-40min；然后降温至30-35℃，再开启均质反应罐中的刮板搅拌器，设定搅拌器转速为40-50r/min，加入二硫化硒超微粉体并继续搅拌20-30min，料液隔膜泵输入灌装间灌装（100g/瓶）即得。
实施例 4 ：二硫化硒洗剂
2.5%二硫化硒祛屑护发洗剂，按质量百分比是由下述原料制成：实施例2制得的二硫化硒超微粉体25.0%（以二硫化硒计为2.5%），十八醇2.0%，甘油5.0%，十二烷基醚硫酸钠5.0%，烷醇酰胺4.5%，N－油酰基－N－甲基硫磺酸钠2.3%，十二烷基二甲基甜菜碱2.3%，十二烷基硫酸钠5.5%，单硬脂酸甘油酯1.0%，羊毛脂0.2%，香精0.2%，去离子水余量，用枸橼酸和磷酸二氢钠适量调节pH值3.5-4.5。
制备：
在油相配料桶中，将甘油、十八醇、单硬脂酸甘油酯、羊毛脂分别加入混合，加热使其完全溶解。
在水相配料桶中，加入水、十二烷基硫酸钠、十二烷基醚硫酸钠、十二烷基二甲基甜菜碱、N-油酰基-N-甲基硫磺酸钠、烷醇酰胺混匀，加热搅拌使其完全溶解。
在配制罐中，将溶解的油相全部放入配制罐，再将溶解的水相搅拌下泵入配制罐内与油相混合，水相全部加入后，继续搅拌使其完全乳化混合均匀，关闭搅拌，使其逐渐冷却成基质膏后放置备用。
将上述基质加热，温度稳定在50℃～60℃时，搅拌下快速加入上述制得的二硫化硒超微粉体料液以及香精，开启隔膜泵循环30分钟后，通过取样阀取样测定并控制pH值在3.0～4.5，合格后用料液隔膜泵输入灌装间灌装（100g/瓶）即得。
实施例3和实施例4制得的二硫化硒洗剂，分散性均一，经过6个月的加速稳定性考察试验，结果稳定性良好；在常温放置24个月的考察期内，产品均未见分层，而且微粒分散均匀。
Claims (10)
- 一种二硫化硒超微粉体，所述二硫化硒超微粉体的粒径为(1.0~50.0)μm，其特征在于所述的二硫化硒超微粉体是由二硫化硒、甘油、皂土、二氧化钛和水按1.0: 1.0: 1.4 : 2.0: 4.6的质量比例混合均匀后进行碾磨粉碎制得，并具有D90为(1.0~15.0)μm的粒径分布。
- 根据权利要求1所述的二硫化硒超微粉体，其中所述的二硫化硒超微粉体具有D90为(1.0~7.0)μm的粒径分布。
- 一种稳定的二硫化硒洗剂组合物，其包含作为有效成分的二硫化硒，药用、日化用或食品用的辅料和水，其特征在于所述组合物中二硫化硒质量百分含量为(0.1~3.0)%，并且所述二硫化硒是使用权利要求1-2所述的二硫化硒超微粉体。
- 根据权利要求3所述的稳定的二硫化硒洗剂组合物，其中所述组合物用作药品，其中二硫化硒质量百分含量为(1.0~3.0)%；或者所述组合物用作化妆品，其中二硫化硒质量百分含量为(0.1~1.0)%。
- 根据权利要求3-4所述的稳定的二硫化硒洗剂组合物，其中所述的辅料选自保湿剂、调理剂、表面活性剂、缓冲剂、螯合剂、防腐剂、香精及纯化水中的一种或一种以上。
- 一种制备权利要求3-5所述的稳定的二硫化硒洗剂组合物的方法，包括如下步骤：（1）制备权利要求1-2所述的二硫化硒超微粉体；（2）制备辅料基质；（3）将步骤（1）制得的二硫化硒超微粉体加到步骤（2）制得的辅料基质中混匀。
- 根据权利要求6所述的方法，其中所述步骤（1）中，将二硫化硒、甘油、皂土、二氧化钛和水混匀后进行碾磨粉碎，得到粒径为(1.0~50.0)μm、D90为(1.0~15.0)μm的二硫化硒超微粉体。
- 根据权利要求7所述的方法，其中所述步骤（1）中，是由二硫化硒、甘油、皂土、二氧化钛和水按1.0: 1.0: 1.4 : 2.0: 4.6的质量比例混合均匀后进行碾磨粉碎。
- 根据权利要求6-8所述的方法，其中步骤（1）制得具有D90为(1.0~7.0)μm粒度分布的二硫化硒超微粉体。
- 根据权利要求6-9所述的方法， 其中步骤（2）中，所述辅料基质为油包水型（W/O型）基质或者水包油型（O/W）基质。
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